# Refining Gold from Gold Filled Jewelry



## Oneal58

I have a pound or two or more of 10k, 12k gold filled items with also the same amount of 1/10th/1/20th 10K & 12K, gold filled plated items. Then I also have about 5 pounds of regular gold plated stuff. Can anyone tell me the difference in the gold filled and gold filled plated. I know what the gold plated is but I dont know the difference in the old stuff, the gold filled and gold filled plated? I can feel by weight there is some difference but I don't know for sure. I have been an electrician all my life and can do most of the other skilled trades. I have already built my hood and installed my suction fan out of an old heat pump. I have bought up a good supply of ammonia nitrate fertilizer and want to make my own nitric acid to save money. Will this nitric be strong enough to serve the purpose of melting the gold after I melt it and make shot out of it? I have muratic acid, can't this serve as hydrochloic acid as well. I just need someone who has been there and done that to help me along. I don't want to burn myself, I respect this stuff more than I do the electricity I work with. Just trying to make a few extra dollars during these hard times. Thanks to anyone who can give me some instruction to keep me from hurting myself. I have been reading the books and watching the videos but still have questions. Thanks in advance for any advice you could give me. Oneal58


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## butcher

The way I understand gold fill is think of a thin pipe of gold filled with base metals, thicker than plated materials.

The best advice I can give is read Hokes book, you can get free download from book section, follow her instructions on getting acquainted experiments, and testing of metals in solutions, also search and read the forum most anything you can think of has been discussed in great detail, welcome to the forum, please also read dealing with waste and the safety section, this is just like dealing with electrical work, you need to educate yourself before jumping in understand your risks how to deal with them safely and know what your doing before you begin, just like electrical work you have a lot of studying to do.


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## Oneal58

Hi Butcher, thanks for your reply. I have already read Hokes Book. Several chapters several times. I think I have the basic knowledge of how to go about it. I have all my supplies and protective items. I guess I am just anxious about getting started for some reason. I have a couple rectifiers and plan to use reverse electroylisis on the plated stuff. I seen a video on Youtube that this person laid all his plated things on a copper shelf that he made. He put this copper shelf in a solution and turned on his rectifier. The gold just came right off the plated material. Would you know if he used a stainless steel anode or a gold one? He gave no mention to how many amps he used either. Or the solution he was using. I would like to start with the cheaper electroplated items until I get some experience under my belt. I have looked but cannot find this particular process. I followed his link that he had there on Youtube but he wants to sell the answers that I need. I have spent all the money I need to right now on this project and need to find the answers that doesn't cost me anything right now. Thank you for your advice and answers. Oneal58


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## martyn111

Using the search engine, top right of your screen, search sulphuric cell, anything and everything you want to know about that youtube video is discussed here, free. Welcome to the forum.


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## jimmydolittle

I don’t think ammonia nitrate with muriatic is the right formula for nitric. I’ve always used sodium nitrate. I’ve been out of the game for several years, so best let someone with experience tell you. Edit. Sorry, that's what I used for aqua regia.


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## philddreamer

Sulphuric acid & sodium nitrate, or potassium nitrate for making nitric. Don't use ammonium nitrate, I understand it could cause an explosion.

Oneal, continue reading & learning the do's & don't before you continue.
Some of these chemicals will explode.

Take care & be safe!

Phil


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## Oneal58

Thanks everyone for your help. I have watched 3 videos that Nerdrage has posting in making nitric out of any nitrate based fertilizer. Whether it be sodium nitrate or ammonium nitrate. These 3 videos are on Youtube and look very simple to follow. I have a friend who supplies all the farmers around the county with chemicals for their crops and their farmland difficientcies. He always has a good supply of Urea, Ammonium Nitrate, Ect. Could someone take a quick look at the Nerdrage videos on Youtube and let me know if I am missing something here. From the videos, you can use any nitrate based fertilizer to make nitric. I know I can purchase what I need on Ebay and several other online stores. But if I can make it myself for 30% cost I would much rather go that route. Plus I have already spent a good bit of money in rectifiers, Pyrex Glassware, condensers, Ect;. Could someone verify what I am looking at (Nerdrage Videos) are being understood correctly? It would be appreciated. I have some experience in electroplating and reverse electroplating in an industrial setting. Not the chemical process mind you, but I was the electrician who kept the machinery up and running so I understand the electrical part of the process, but not the chemicals that were used. Thank you so much for your help. Thanks, Oneal58


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## Geo

ive tried all of them and it does make a weak nitric acid but nothing strong enough to refine with.i used the second video from nurdrage,the one that uses sodium nitrate,hcl acid and copper to dissolve some silver and it was too diluted to digest the silver.i finally used it to make AR and it took about 700 ml of this weak acid in hcl to dissolve 18 grams of 10k.


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## Oneal58

Thanks Geo for taking the time and answering my question. 
I can see that using straight Ammonium Nitrate in the first 2 videos would make weak Nitric as you said but why can't I turn the Ammonium Nitrate into a dried powder after taking out all the insouluables and concentrate it. Concentrate the Nitric after turning it into a liquid and then condensing it by distilling it. Is there any danger if I put the ammonium nitrate through these steps? Then use the 3rd method with a condenser to get commercial strength Nitric. From the NerdRage Video what they got was so strong they had to dilute it to get it to go to work on the copper. I know that NerdRage said to use a Nitrate salt and not a fertilizer but if I clean up the Ammonium Nitrate and turn it into a powder wouldn't it make a stronger Nitric. Has anyone tried this before. I wouldn't be adding anything to the Ammonium Nitrate at first. Is this stuff (Ammonium Nitrate) stable in liquid form also? To be honest with you the reason I am harping on this is that the ammonium nitrate I use will cost me nothing. I very much want to be able to use it, if possible. Thank you for any advice in advance.
Oneal58


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## Geo

Oneal58 said:


> Thanks Geo for taking the time and answering my question.
> I can see that using straight Ammonium Nitrate in the first 2 videos would make weak Nitric as you said but why can't I turn the Ammonium Nitrate into a dried powder after taking out all the insouluables and concentrate it. Concentrate the Nitric after turning it into a liquid and then condensing it by distilling it. Is there any danger if I put the ammonium nitrate through these steps? Then use the 3rd method with a condenser to get commercial strength Nitric. From the NerdRage Video what they got was so strong they had to dilute it to get it to go to work on the copper. I know that NerdRage said to use a Nitrate salt and not a fertilizer but if I clean up the Ammonium Nitrate and turn it into a powder wouldn't it make a stronger Nitric. Has anyone tried this before. I wouldn't be adding anything to the Ammonium Nitrate at first. Is this stuff (Ammonium Nitrate) stable in liquid form also? To be honest with you the reason I am harping on this is that the ammonium nitrate I use will cost me nothing. I very much want to be able to use it, if possible. Thank you for any advice in advance.
> Oneal58



ammonium nitrate is the main ingredient of the bomb that blew up the government building in Oklahoma city (it was ground into dust).you should really consider using a different form of nitrate.if your going to distill it anyway just distill 70% nitric using potassium nitrate and concentrated sulfuric acid.BE WARNED!! i ruined my health doing this and will never be well from it.use safety equipment, never breath fumes.even a little bit damages your lungs and it will never heal. if you can afford it just order some online.


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## Oneal58

You know, after some thought I think buying what I need to make AR the first few times will not only keep me safe but will show me what reactions I should expect with industrial/lab quality acids. If I have nothing to compare my results to I do not have a learning curve. 
So, thank you all for talking me out of cutting corners to the finish line. This personality trait has got me in trouble all my life. The shed where I will be working at is close to my house. My Grandkids are always at my house when they get home from school. I would hate to do something stupid and harm anyone innocent, especially my grands. 
I guess my next question I am asking help on is do I need the laboratory grade or would the industrial grade be fine? 
Thanks, Oneal58


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## philddreamer

Industrial grade its what I use. Where abouts are you? 
That way some one here can point you to a supplier.

Indeed, keep the little ones safe! I told my grandkids to NEVER go to my back yard, so they stay away, because " grandpa is making gold" the say. :lol: . 

Phil


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## Oneal58

Hi Phil, thank you for your time to answer my question. So, is there anyone around nearby that I can go to or contact to pick up what chemicals I need? I am in S.C. Thanks Phil, Oneal


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## philddreamer

Kadriver is from S.C..
Try contacting him; he might be able to help you.

Phil


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## Oneal58

Hi Phil, 
I found kadriver and emailed him. Hopefully I will hear back from him. Thank you for helping me, it really is appreciated. 
Oneal


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## philddreamer

No problem, Bro, that's what we are here from. 
I'm just glad I have the opportunity to help others, just like others helped me.

This is a great Forum! 8) 

Phil


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## butcher

Oneal58,
You can also dissolve the gold powders you recover in hydrochloric acid and adding household bleach. 

You could recover the gold using the concentrated sulfuric stripping cell'

Have you visited Laser Steve’s web site? If you have not, look for the link in his posts.

Harold just recently posted some good help for someone working with gold fill.

Copied from Harold’s post:

One does NOT dissolve everything along with the values when there are options. Gold filled is certainly top of the heap where this matter is concerned. Gold filled is generally 95% base metal, all of which is troublesome. Have you given any thought to NOT melting? Think a moment about this idea. First, remove any parts that are magnetic. Avoid including steel in your refining circuit. Also, remove any aluminum should there be any present. The pieces are then heated to dull redness (but NOT melted). That burns off any oils and other substances that can be problematic. You then go after the base metals with dilute nitric acid. The resulting solution will contains traces of silver, along with several other base metals, and will yield thin sheets of the alloyed gold, along with miniscule particles. The material should be subjected to nitric until all base metals have been dissolved. The remaining solids, including the fine sludge that is sure to be a part of the solids, is then gathered in a filter. When dry, it should be incinerated to redness, but, again, do NOT melt. After incineration, screen and go through the material with a magnet. The material should then be given a wash in hot HCl, then rinsed until the rinse water is clear of color. Only then should you dissolve the gold. 

It's all in Hoke (except for the HCl wash after incineration, which is one I developed to aid filtration for such material). 

You can run gold plated items the same way, although, with the cost of nitric acid, you're better served to strip such items with a sulfuric stripping cell, or to use the AP process that is well discussed on this forum. 

Read Hoke! Then read it again. Read until the things I've talked about here make sense to you. 

Harold


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## Oneal58

Hi Butcher, 
Thank you so much for this information. It's the route I am going to take. Harold gave the process to me last night which was appreciated. I also appreciate the information you gave me, I am going to put this to use also. 
Unless I have overlooked it, which is very possible, you didn't mention what I should do with the items that are magnetic. Or gold plated/filled items with ferrous metals in them? Such as the backs of gold filled watch bands covers/necklaces/brooches, Etc;. But about the watch bands, not the entire watch band mind you, just the tops I have taken off the gold filled bands that have some sort of magnetic ferrous metals on/in them. I find these to be slightly magnetic. And also the gold filled items that are a little magnetic, what I mean is that it's just magnetic enough to let you know that there are ferrous metals involved somewhere on it or in it. I have a strong rare earth magnet that I use so it (magnet) will pretty much attract an item if it has any amount of ferrous metal in it? I also found that sometimes some of this material will lose it's magnetism and drop off by it's self if given a little time while other pieces will not lose it's magnetism. I am guessing that the pieces that drop off after a little time have just been influenced by the non-ferrous pieces that it's laid near to in the box. So, I guess my question is what do I do with the items that do not drop off over time. I also have tried grounding some of the pieces before testing with magnet which doesn't help? Thinking that maybe static electricity was playing a part in this reaction somehow? Excuse me if you have already answered this and I just missed it somehow. But I would hate to discard any 14K gold filled items because there just a little magnetic field around them. When I say a little magnetic what I mean is, if I shake the magnet with some of the Jewelry on it, I will usually end up picking it up off the floor. Not so with all of it, but some of it. Some of it has to be pried off the magnet but seems to have a thick coat of gold filled or plated gold on it also. I have tested the gold filled/plated watch band tops that are magnetic and in fact they are gold filled. Before I started on this project I tested all my gold before I sold it on ebay. Probably hundred or so lots with many, many pieces in each lot I sold. I have sold many lots of karat gold over the last 12 or so years now but never gold filled/plated items. I got to where I could tell if an item was gold filled or plated by just watching the reaction when I applied the acid to the gold mark left on the stone. So, the gold is there but just on top of/in/around ferrous metal of some kind. Thanks in advance Butcher for your help and thank all of you (Harold) (Geo) (Phil) and many more who have been helping me. I appreciate all of you and love this site. Hopefully one day I will know enough to return the favor to others like myself. I can't seem to find this answer in Hoke's Book but it is very possible I did overlook the information, or just don't remember reading it? 
Oneal58


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## butcher

Very recently Harold posted a method to process the gold fill, he discussed how to deal with the magnetic portion of the material, I am pretty sure it was in a post with a title about gold fill, I do not remember all details but do remember incineration was a part of the process and running a magnet over powders. 

When Harold suggests something listening to him, and following his advice you can not go wrong (well even if you got stuck he would be there to pull you out).

Look into the other posts about gold fill.
If you are new to this, spend time studying until you understand the process you choose and are fairly confident you can do it, many of us process some high value scrap when we first begin to learn (before we really have a good understanding, then we look back and say if only I had it all to do over again we would do it differently or better with less lose.

If you’re new to this study Hokes book getting doing the getting acquainted
Experiments, and also learning and testing of solutions, you can learn to make stannous chloride here on the forum.

Which process or chemicals you choose you should have some experience with before using them on high value scrap, sometimes it may be better to put your high value scrap up and experiment on lower value scrap.

This is why I normally recommend some one learn with memory fingers.
Read as much as you can, experiment on small lots, till you prove your process,
A magnet inside a plastic bag is what we use when panning for gold, it make separating the magnetic materials from the magnet easier.

Also I would put the magnetic materials the magnet picked up in my stockpot as it may also collect some gold powders or some gold could be mixed with Iron.


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## Oneal58

Hi Butcher, will do as advised. I am doing exactly what you recommended. I am starting with the low end materials that I have accumulated over the years and saving my Karat material now untill I fully understand the process in my mind before I refine it. 
I understand completely what you are saying and it's great advice. I told myself when I got to the point of being able to do this I was not going to take any shortcuts, none. Too dangerous for one thing and can be very wasteful if you don't know what you are doing first. So, I am starting at scratch and am going to climb the ladder, one step at a time. I want to be a very competent refiner hopefully down the road with a lot of studying. Thanks Butcher, Oneal58


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## Harold_V

butcher said:


> Also I would put the magnetic materials the magnet picked up in my stockpot as it may also collect some gold powders or some gold could be mixed with Iron.


Excellent advice. Especially when processing filings from the jeweler's bench, which always contain bits of iron. 

When dealing with items such as watch bands, unless you can strip them with cyanide, you're best served to dismantle them. Items such as the stainless backs and springs should be discarded. 

I would suggest that a conventional (ALNICO) magnet be used when sorting items that have iron within. Many objects that contain gold also contain nickel, which may be attracted to super magnets, at least to some degree. By using a weak magnet, only objects that have the potential to be troublesome should be detected. Those that are strongly attracted to the magnet make great material for the stock pot, where it will be used to cement values. 

Harold


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## Oneal58

Thanks Harold,
I have noticed that (some) of the items that my rare earth magnet will pick up will not be picked up by a large refrigerator magnet my wife keeps her groceries list pinned to the frig. with. So, you have answered that question for me. Also, the pieces that's barely magnetic that I mentioned in my previous post is another question I have no longer thanks to you and Butcher.
I have a couple of other questions.Hoke mentions in her book, when you make a pour and the gold button pour developes a dimple in the top of the drop? Hoke says this is a reliable indicator for telling you whether you have a good quality pour or not? She says this indicates that the button is going to be soft, pliable,easy for the Jeweler to work with. She says this indicates that the button has little or no tin or lead. 
So, how reliable is this dimple forming in helping you determine the purity of the gold button you have? Is this a reliable method of telling if you have a pure or near pure gold button? What are some of the other signs to look for when you pour a button to let you know you have a good high grade button without having to assay or test the button?
Do you use crushed glass on the final melt as Hoke mentioned to do? If so, will you not have to break/crush the button to get the glass coating off to weigh or sell? She also mentioned you can use Saltpeter (KN03) and or soda ash. She also says you need to use Borax each time to coat the crucible before applying heat. I guess what I am asking is, are any of her methods outdated or changed/updated since she wrote her book? Does anyone use these materials in the final melt? I know of course to use Borax coating on your curcible but not sure about the glass, soda ash, or saltpeter?
Hoke also says to use Copperas to drop the gold out of solution. Most everyone on the site here says to use Sodium MetaBisulfate now. That it works much better than Copperas. I looked for a full1/2 day to find a bag of Copperas, finally found some at a Tractor Supply Store, 40 miles away from home. So I was wondering if any of the other information in the book has been outdated/updated and if so what are some of the main things that she says in her book that is no longer used because a new updated process was introduced or a little better refining method was found? 
Does anyone still use Copperas anymore? I bought a 4 pound bag of pure copperas for $22. I haven't used any of them yet so I could take them back if they are not going to be used. I have to carry the Draino I bought back because I checked the MSDS Sheet on Draino and it has other fillers in it besides the Sodium Hydroxide. I found Liquid Fire at Ace Hardware, the MSDS Sheet says it's 99% pure Sodium Hydroxide. So, is this good to use, Am I thinking correctly here, that the Liquid Fire is pure enough to use without cleaning it up or trying to purify something that is 99% pure already? Thanks for your help. Oneal58


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## butcher

Oneal58,

Copperas is an old chemical name for ferrous sulfate (iron sulfate) (FeSO4), it works very well to precipitate gold from solution, many times I even prefer it over SMB, the crystals need to be green, if they are oxidized brown they will not work, I make my own (copperas) ferrous sulfate, using soft iron laminates from old transformers or motors I burn the shellac off them cut them to small pieces and heat them in dilute sulfuric acid about 10%H2SO4 dissolving the iron into a green solution, this green solution is filtered and concentrated down to crystals, kept slightly wet and acidic for storage, I will use the green crystals or the concentrated liquid. 

The ferrous sulfate crystals also are handy for testing purposes in a spot plate to test for gold and also to separate gold in solution in the spot plate to test for other valuable metals, Harold has made several posts explaining how to do this.

Make sure your ferrous sulfate (copperas) is green before using, if it is brown (oxidized) you can use it in the garden and make you some, there are more details about it on the forum.

The Impure sodium hydroxide should be ok for waste treatment, to neutralize the acids.

I thought I have bought liquid fire before and it was concentrated sulfuric acid, are you sure your jug is sodium hydroxide?

If this is liquid fire sulfuric acid it is usually sold with the gallon jug wrapped in plastic and is good for the concentrated sulfuric cell.

Look again at what you have in the liquid fire bottle.

As far as using crushed glass, quartz sand, borax, nitrates, sodium carbonate, flour, charcoal, litharge, and other ingredients, most of these are added as flux when you are melting materials that contain gold to collect or assay the gold or other values, each of these ingredient have specific purpose in the melt, some like glass form slag for oxides of metals to gather into, slag can also shield your melt from environmental oxygen from torch or furnace, nitrates would oxidize base metals in the melt, flour or charcoal remove oxides make CO2 gas, borax also forms a slag and act as flux shield or to help metals from sticking to your dish or crucible, helps to get melt more fluid where powders can melt together better, sodium carbonate also helps with this also and helps remove oxides and can help in conversion of metal salts in the melt to form molten metals (like silver salts when melted)
The use of these and other ingredients in the melt, are chosen by what properties you need them to perform.

Sodium carbonate is hard on melting dish or crucible somewhat attacking it, but can also be used to clean them. I have no proof but it seems to take old slag (glass full of metal oxides) melts them more into metals and glass slag, making them fluid enough with heat to pour them off, it also seems to melt some of the surface coating of the dish and add it to the slag being poured off.

Sometimes people use flux to help improve the looks of their impure gold (or to slightly improve its quality) (in this case re-refining would give higher purity), unless you were just selling it to a refiner as impure, but then why fool with it?

Gold of high purity will melt with only a wet coating of borax to dish so gold will not stick to dish as powders are brought into a molten form, adding too much borax and the gold may be harder to remove from the dish.

The dimple (pipe) and bright color, softness, crystal, and lack of oxide coating does give an indication of purity of the gold.


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## Oneal58

Hi Butcher, you are right, I was thinking one thing and typed another?? I have reallly got to watch this more closely and (proof read), check over what I type. If I can make this type of mistake here, I could also make a mistake under the hood. From what I know now a mistake made with some of the chemicals involved is unforgiving and you will not have a second chance. 
You were right, I am after the sulphuric, but I did buy the Draino. I came home and pulled the MSDS Sheet on it and found it had impurities in it. I didn't buy the Liquid Fire yet, I found it at Ace Hardware then came home and pulled the MSDS Sheet on it. I am going to go back to buy it. I just didn't want to buy something else I could not use. I have done enough of that trying to get the right lab glass I needed off Ebay. Another thing, I thought that all products on the shelves of stores suppose to have the contents labeled on them? I have noticed that some of such items (chemicals) on the shelves don't have what the product contains anymore, just a number and website to check the MSDS Sheet on it? 
But thank you for bringing this to my attention. I really do need to work on this harder, pay closer attention and proof read more. Hoping this practice will follow me to the shed out back. 
So, I will hang onto the Copperas until I open the bag at least. If crystals aren't green and fresh, I just have a good product to use for Iron deficiency in soil. I cannot find a manufacture date on the bag of Copperas I bought anywhere, unless of course I have overlooked it, which is possible. I will look again tomorrow. 
A question on the melt of the high purity gold in the crucible. When you say add a wet coating of Borax to the dish so gold will not stick to dish. Do I add just enough (water?) to Borax to make a paste to coat dish with? If so, about how thick should this paste be? Does the Borax completely burn off during the melt? What if you put too much Borax into the crucible? Do you keep heating the gold until you burn it all off or does it form a slag that can be removed? On new crucibles, should I season the crucibles with a coat of Borax on them or cure them without adding anything in the crucibles before use. 
The more I ask questions, read and study, the more I realize the depth of what I am attempting to do and how little I still know. I thought I would have been melting gold a month ago. I still haven't fired up my torch to melt any gold yet? I honestly don't feel I am any nearer to doing this now than I was a month ago? I have missed only a few days studying during the last couple of months. I will probably average 4 hours of study, reading, a day. It took me a week and a half to read Hoke's Book alone. I took it slow and easy, double and triple reading many chapters. 
I got 1 more question for everyone who reads this post. Was there a lot of anxiety before your first refine/melt or is it just me who feels this way? I just need to get to the place that I feel confident enough to just bite the bullet and get the torch fired up.
Thanks Butcher and everyone else who has helped me so far. I am so thankful I found this site, it's been a life saver, literally. 
Oneal58


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## butcher

Oneal58 
Relax you are getting there faster than you think, patience is a big factor here, my melting dishes I heat them up slowly so I do not crack them to get rid of moisture then just sprinkle some borax powder on the hot dish, just enough to coat it the borax is kind of fluid when hot, and this is what I meant when I stated (wet the dish with borax).

I have heard one member say he painted water wet borax on his dish but I would not do that, as I have had dishes crack just from heating out the moisture of what looked like a dry dish, even though the dishes are not very expensive they are a trouble for me to get and I want to get the most mile's I can out of the ones I have.

The borax becomes a clear fluid when hot (and will change color if it absorbs base metals) if you melt gold even fairly pure you may see a light violet color stain which kind of looks like the diluted stannous test, in the borax coated dish after our done, when borax cools it is like a soft glass clear if not tainted with metals, (this soft glass coating which can be chipped or hammered off a metal if you added a lot of borax to the melt), when we melt our refined gold buttons the gold is not really got a coating of borax, sometimes if you add a little more borax than you needed the button may stick in the bottom of the dish when borax glass cools, these can be moved after gold cools down and before borax cools, or most of the time just popped loose with a pocket knife.

I do not see any reason to fear this, just inform yourself of dangers and take the precautions, a lot of it is common sense, and learning before you jump off the bridge (is there water in the river did you even check) you seem to be doing your homework and I feel you will do just fine.

There is a lot to learning all of this, and it gets easier as you go, but you will never learn everything, you are just starting to see why we give the answers to the question, when a new guy ask us tell me how to refine my gold in the next post. And expects us to tell him in ten lines or less.


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## Geo

Oneal58, i dont think he meant for you to wet the borax.what he meant was,heat the melting dish slowly to a dull red heat and then sprinkle DRY borax on the inside of the dish a little at a time and reapply the heat to melt and push the borax to a smooth coating on the entire surface of the inside of the dish,dont over do it,just enough to coat it evenly.it will look "wet" when you finish and after it cools it will still shine like it is wet.if you actually wet the dish before you try to heat it up the dish will break from trapped moisture exploding out.all my dishes crack a little at first,its caused from heating too fast or cooling too fast but after you have heated it the first time and conditioned it with borax it should hold together through quite a few melts unless you melt something thats dirty.use the dish you will melt pure gold only for melting pure gold and nothing else.after the fkux gets dirty or the crack gets too big you can use it to incinerate in or to do test melts.


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## jimmydolittle

Go to Lazerstes site and watch the video on melting. This will explain the whole concept of preparing the melting dish.http://www.goldrecovery.us/


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## Oneal58

Thanks Butcher and Geo, 
I understand now. 
Another question, I was told by Harold to heat the gold filled watch band tops/cases I have up to a dull red, not melt, just heat them up at 2 seperate times in the process he gave me to burn off all the krud that is on them. I can just imagine what's inside these things after the bands have been worn for years on someone's arm.
Someone has told me to use caustic soda/Lye and boil the gold filled watch band top caps/cases a couple of times on the hot plate. I would prefer to go with Harolds advice on cleaning the watch band top caps and cases than using caustic soda or Lye. Unless of course this alternate method could cause me less trouble down the road. I was looking at these watch band top caps last night. Some of these top caps are nearly 1/4 full of God knows what? The watch cases are not as dirty.
So, I am asking, if the watch band top caps are really dirty will burning them a couple of times as Harold told me to do get all the dirt out/off of them or do I need to boil them up first in some caustic soda/Lye? Do I then burn them like Harold told me to or will they clean up with the Caustic Soda/Lye good enough. I develped a way to get these top caps off quickly but this process that I use squeezes/crushes about 1/3rd of the top cap together, tightly. Maybe tight enough that this Caustic Soda/Lye cannot get to the dirt I traped in there when I squeezed them together. I don't even want to think about having to open each one back up. :shock: It would seem to me to always give them a couple of good burns as Harold has stated anyway to burn this traped krud up. Even if I boil them up first. Also, I wanted to double check to see if this Caustic Soda/Lye does not harm/effect the gold filled band tops and cases. I read this on another site and just wanted to hear what someone thought about this here. I have many days of work taking these top caps off and would not want to destroy the value in them by doing something I am not suppose to. 
I got to go to town and get some of the Liquid Fire from Ace Hardware I need. I need to make up some Stannous Chloride Solution. I read on the site somewhere that I can use lead free plumbers solder and dissolve it in a little nitric acid for my tin. Will this be pure tin, pure enough to make Stannous Chloride? 
Thanks, Oneal


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## butcher

Oneal58,

Always follow Harold's advice, you will not go wrong.
Sometimes there are other way's to do things, but until you understand them stick with known proven procedures,

I cannot say where Harold told you to burn something red hot, we usually refer to that as incineration, it is usually recommended for several reasons, like removing oils and inorganic materials, or carbon-ous materials, incineration is also recommended when we use one acid in a process like nitric acid, and after decanting and rinsing the powders we may incinerate to remove the nitrates formed (removing the previous acid or salts of those acids) because we cannot just rinse out this previously used acid it may effect our next step(like dissolving gold when we do not want it too), so now we can change acids say like washing in HCl (without the previous acid nitric mixing with the HCl and forming a form of aqua regia and dissolve gold) when all we may be trying to do to these powders now is to rid tin and other base metals (see more about tin and incineration)

Another reason we may use incineration, is to oxidize the base metals, this makes them easier to dissolve in acid, one troublesome metal is tin, tin in nitric acid makes a gooey mess, almost impossible to filter, it is also troublesome in chloride solutions, one way to deal with the trouble maker is to incinerate, this oxidizes the tin, which makes it dissolve easier in the HCl (hydrochloric acid) (muriatic acid), this not only helps us to get this trouble making metal washed out of our powders but also improves our ability to filter our solutions. There are other reasons for incineration, but just take Harold's advice he has been there done that, sorry if I new what instruction he gave I may be able to give you more clues as to why he said do it this way, do not miss or skip steps, or change the process unless you understand why and where, even skipping something that seems like why would that matter if I did not do this or that could mean trouble for you later, sometimes these very simple steps are there to eliminate this trouble, and you may not even see why.

Example say I told you to wash some white powders in boiling hot water and then decant, and you figure that heating the water is not important, too much trouble, and you just used cold water, then at the end of the process, you find your gold is full of lead and then you do not understand why, (lead chloride is much more soluble in very hot water, and almost insoluble in cold water), by skipping the part about using hot water (something that would seem unimportant) could mean success or failure, or having to start all over again and possibly making the same mistake again.

Stannous chloride is made with tin (95% tin solder will work) and Hydrochloric acid, also called HCl or muriatic acid.
(Stannous chloride is NOT made with nitric acid, which would give you that gooey stuff I was talking about above, and would not work to test for gold in solution)


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## Oneal58

Hi Butcher, you are right. Harold didn't use heat/burn in the manner I stated. He used incinerate just like you said he would have. I still am working on the technical language, it's slow in comming but I have tunnel vison now and we will get there with your and everyone else's help. All of you have taken your time to answer my questions and that really means a lot to me. I promise to play it back one day down the road with other first timers like me. Only when I become competent to do so. 
I am building my tray/screen for my sulphuric cell now in the den. I am using #10 bare copper grounding wire to build the frame. I am using stripped telephone wire to build the basket by basket weaving the telephone wire to the #10 copper frame . I am doing so in a way not to make any solder joints at all in the sulphuric acid. The only place there will be a solder joint is (1) outside of the cell. Does that sound like it should work to you? I will send you a picture of it when I finish it. I am going to start on the lowest end material I have before I go to Harold's procedure on the gold filled material. I am going to start with some necklaces ( gold plated). Seems to me that the necklaces I chose will have more plating on them than just the run of the mill plated Jewelry. I am going to start with the necklaces that have a lot fine openings (holes) in them. Surface area should be at least twice as much on these than just the flat Herringbone type Necklaces with no openings in them. 
I bought my Liquid Fire (Sulphuric) today from Ace Hardware, I bought a gallon to get started. 
Butcher, another question tonight is, can I use brick cleaner which has I believe 31.45% muratic (hydrochloric) acid when it's time or do I concentrate it? Also, I saw a method of taking a few drops of concentrated peroxide, just a few drops and cleaning up the muratic. Is this step necessary to do? I also found my tin solder, it's 98% tin and 2% silver. Will the 2% silver be a problem? You have already answered this in a previous post about the tin solder for the stannous Chloride but I didn't mention the 2% silver? I am going to start with Industrial grade Nitric Acid. But trying to get ahead of the game I tried to order some Potassium Nitrate and the Farm Supply said they were not going to order anymore untill the spring, when they sell pretty much all their fertilizers. Same story at the other fertilizer dealers I called, can't get the Potassium Nitrate untill next spring. Do you prefer Potassium Nitrate over Sodium Nitrate? I remember you saying you made your Nitric? 
So, can I use the 31.45% muratic to make my Aqua Regia when it's time or do I need to concentrate it? Thank you Butcher, you have really been bending over backwards to help me and it has not gone unnoticed and I am truely greatful. 
By the way I copied Harold's Post, the directions he gave me on the gold filled material when I feel I am ready for that one. It's below.
Thanks Butcher,
Oneal58

ProfilePrivate messageE-mail Harold_V 
Active Member 

Posts: 5951

Joined: February 26th, 2007, 12:58 am

Location: Washington
November 14th, 2011, 6:20 am by Harold_V
Re: modified reverse electroplate theory
Oneal58 wrote:
Hi Everyone, is it best to try and reverse electroplate the gold filled items I have 
Not a good idea. The nature of stripping cells is such that they are very effective on pure gold, but not so good on alloyed gold, which is what you have with gold filled items. 


or just melt the watch cases and make some shot and then drop a small test batch into Aqua Regia just to see is it worth the effort and expense in acids.
Also not a good idea. Have you read Hoke?

If not, why not?


I don't understand how Gold Filled items which are (mostly antique) are put together yet. 
Read Nick's post. He covered it very well, in just a few words. 


Is there enough gold in them to go this route or would it be a waste of good Aqua Regia and time.
If you used that approach, yeah, it's a waste of time. You clearly don't understand how such material should be processed. If you were to approach the project from that perspective, there'd be no end to the problems you'd encounter, all of which can be easily avoided. 

To get good quality return shouldn't I melt everything and then start fresh with AQ and go through all the steps of recovery or is there a simpler route? 
One does NOT dissolve everything along with the values when there are options. Gold filled is certainly top of the heap where this matter is concerned. Gold filled is generally 95% base metal, all of which is troublesome. Have you given any thought to NOT melting? Think a moment about this idea. First, remove any parts that are magnetic. Avoid including steel in your refining circuit. Also, remove any aluminum should there be any present. The pieces are then heated to dull redness (but NOT melted). That burns off any oils and other substances that can be problematic. You then go after the base metals with dilute nitric acid. The resulting solution will contains traces of silver, along with several other base metals, and will yield thin sheets of the alloyed gold, along with miniscule particles. The material should be subjected to nitric until all base metals have been dissolved. The remaining solids, including the fine sludge that is sure to be a part of the solids, is then gathered in a filter. When dry, it should be incinerated to redness, but, again, do NOT melt. After incineration, screen and go through the material with a magnet. The material should then be given a wash in hot HCl, then rinsed until the rinse water is clear of color. Only then should you dissolve the gold. 

It's all in Hoke (except for the HCl wash after incineration, which is one I developed to aid filtration for such material). 

You can run gold plated items the same way, although, with the cost of nitric acid, you're better served to strip such items with a sulfuric stripping cell, or to use the AP process that is well discussed on this forum. 

Read Hoke! Then read it again. Read until the things I've talked about here make sense to you. 

Harold


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## butcher

Oneal58,

The hydrochloric acid you are talking about is what most all of us use, no need to try and clean it up, or do anything to it, as you said.

Some places sell some types that are "green" or something like, that they may have other ingredients, I would not use them.

Just regular muriatic acid is fine, hardware stores or where they sell rock brick or masonry supplies, 

muriatic acid, hydrochloric acid, HCl all are describing the same acid, there are even some old ancient names also.

I have not used the concentrated sulfuric acid stripping cell, and only know what I have read about it, although I have a fair understanding of electrical principles, and played with a few other types of cells, and I have a good understanding of batteries, and other cells, I will try and keep my comments to what I do know, sorry I will not be able to help too much with this project, but many members here will be glad to help.

I would not think the silver in your tin solder would give you any problems, the silver may be an insoluble powder or possibly silver chloride white powder, in the bottom of stannous solution, and the solution could be decanted or filtered off if you wanted too, I do not see where it would cause any problem if you did not separate it out.

I have used both sodium and potassium nitrate, to make nitric acid, they both work well, I like them both for differing reasons, they do have a little different results, the sodium sulfate salts seem much more soluble than potassium salts, potassium salts are better for the environment than the sodium salts, 

I reuse the byproducts from my home made nitric, so I save the potassium or sodium sulfate salts for other uses.

Here in Oregon we have a lot of trees, which mean a lot of stumps, and so some of our feed and grain co-op, hardware stores, (even bi-mart in season) will sell one pound bottles of stump remover, there are two chemicals they use for stump remover
1. Potassium nitrate, 
2. Sodium pyrosulfite (SMB) (sodium metabisulfite),
both of these I use in my recovery or refining.

Hydrochloric acid can be made with rock salt and sulfuric acid, but for now you should just buy yours at the hardware store, just giving you this for information, this I would only use in recovery from ore or low grade material, but also for you remember when you mix sulfuric and salt what you are making.


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## Oneal58

Hi Butcher, thanks. I end up with gaseous hydrogen chloride which I can then bubble through water to get Hydrochloric Acid. I also end up with a soild in the bottom of the reaction vessel that is Sodium Hydrogen Sulfide. I hope I got that right?
Is there a chart offered somewhere that you can use as a guide that tells you how much of each one to use, if you ever need to produce some for any reason. I read a lot of post on the forum but some of them don't give you the quantities involved for some reason?
I have ordered a lot of different sized pyrex beakers and flask, condensers, connector's of different sizes, lids, stpppers, Etc;. My reasoning was if I was going to make a little money at this, which is badly needed to catch up some hospital bills and Dr. bills for me and my wife (both). My wife has had a light stroke on her left side among other issues because of this. Well, we both are almost worn out but we have had a great time the last 40 years. 
But I decided I was going to have to make what I needed after pricing some of the chemicals I was going to need on a regular basis. I have put in a lot of time trying to teach myself some basic chemistry. Chemistry is one class I chose not to take in school because of the horror stories other students would tell me about the classes. But I probably would not have remembered any of it now anyway. I went the electrical route in my career and then Auctioneering, which I miss tremendously. Now you are saying, well I see now, Auctioneering, that's why he rambles so much! :lol: 
But I will probably give you a break for a few days here Butcher. I finished my copper Cathode basket last night and will be running gold plated material over the next couple of days if nothing pops up. So, wish me luck and a blessing could not hurt.
Another question for you today Butcher, then I will let you rest a couple of days. It's getting a little cold outside here but the sulphuric cell suppose to work better when it's cold anyway. 
But, I have a natural gas heater in the shop. It's the open flame unvented type. I wanted to ask you, will the carbon monoxide fumes from the gas heater cause any reactions with any of the acids I will be using? Also this heater puts moisture in the building at times when the temps are right. I know this can't be good the way some acids will suck moisture back into them. Do I need to find myself an electrical heater instead of this gas heater. It's a fairly tight shop but the ceilings are not but about 7 foot. The vent hood does a good job so it may be that I can keep the natural gas heater in place. Just trying to cover all the bases before I begin and get your feelings about it. Thanks Butcher, Oneal


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## butcher

"I end up with gaseous hydrogen chloride which I can then bubble through water to get Hydrochloric Acid. I also end up with a solid in the bottom of the reaction vessel that is Sodium Hydrogen Sulfide. I hope I got that right?"

I am not sure what you are referring to by the above statement?

If you were talking making HCl, forget it just buy it it is very cheap.

If you are talking about making nitric acid then using laser Steve’s method works very well, it uses boiling hot water to dissolve the nitrate fertilizer in then you cool and slowly add the sulfuric acid, let cool again and separate liquid from salts, the liquid is put in freezer and cooled, the salts are again removed (these salts are potassium or sodium sulfate)
100ml H2O
170g-sodium nitrate
Or
200g-potassium nitrate
56ml 98% sulfuric acid

Search for home made nitric acid with Laser Steve

Do not spend much money on materials until you actually need them I use very little lab glass, mostly just jars and kitchenware.

I see no trouble with the heater in your shed, except get the carbon dioxide fumes out of there for your own health, just cover your cell when not in use to prevent it from sucking in moisture, while it is running it generates heat and should discard moisture.

Sorry I lack time to answer more clearly.


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## Oneal58

Hi Harold_V,
Harold, this is Oneal58, you know they guy who has trouble with Etc;. I don't know yet the best way of getting a message to particular members on the site? I have tried not to bother you much but I have a couple of questions about the sulphuric gold stripping cell. Butcher has been kind enough to give me lots of information I am trying to digest now. He has told me that he was not up to date on the Gold Stripping sulphuric cell because he doesn't use that method, at all. He said you would be the man to contact with my questions about the sulphuric cell. You gave me some great information on how to refine my gold filled material and I appreciate it. I plan to use that procedure. You said to use dilute nitric to run the gold filled material. I need to ask you at what % nitric. Would 35% nitric be about right?
I decided to go with the sulphuric stripping cell first to get a little experience and knowledge before I went with the gold filled material I have. Just because the gold filled has a little more gold in it/or on it I should say than the gold electroplated material.
A couple of questions on the gold stripping cell, if you have time to answer them.
Is there a way to tell if you have possibly put a piece of Karat Gold mixed in with the gold plated batch by accident. Will the Karat Gold piece keep it's gold color or will it turn dark just like the gold plated pieces does during the process. 
Also you said to keep the magnetic material out of the gold filled material I will be processing.
My question is with the gold stripping sulphuric cell, can you put the pieces that are magnetic ( ferrous metals under gold plate) in the sulphuric cell. I believe the quantity of material I have is about 60%ferrous and the rest is non-ferrous. Looks to me that the higher end ( well made) non-ferrous necklaces and other pieces has brass under the gold plate. Would you seperate these to run through the cell or do you try and strip the pieces that are ferrous and non ferrous together. Or, are the non-ferrous pieces actually gold filled, just not marked? I could not find a mark on non-ferrous pieces anywhere? The GP or GF or any other type mark are not there. I have tested for 10k and they are not 10K. If I dissolve a piece of this material and test with stannous chloride will I get the same results as if I did the same thing with a gold plated ferrous piece? 
I have a Rheostat in the circuit of my sulphuric cell. I don't know how to figure the load that the material I am running is going to put on the rectifier, thus determining the amperage flow I am going to get. I have a fluke electrical meter in the circuit to determine amperage flow. Is there a formula that can be used to determine the amperage flow I should get by any other method other than trying to come up with surface areas, Etc;. I know the surface area of the anode and cathode would play a part in the load, how you would go about getting that from all the different types of jewelry would be an involved job. It would seem that this would be almost impossible, too time consuming to do, being that there are so many variables that are involved, such as strength of acid, ambient temperature, acid temperature, surface area of material, distance between anode/cathode and the list would go on and on. 
Say for example, I am running 8 ounces of material. The amperage flow is 7 amps through the electrolyte solution. Is this in the ball park of what it should be? I could add more material and bring the amps up. But then as the electrolyte solution gets more saturated with gold with each run the amps would increase. I have read that this increase is due to the increased conductivity of the gold in the electrolyte solution. Where should I try and keep my amperage on 8 ounce runs. I know you would need to know what size cathode, anode, vessel, Etc. But is there a ball park figure when amp flow just gets too high. When the amperage gets to (?) should I let the electrolyte solution settle and decant. 
One more question. I ran across some bars at a flea market that were said to have came from a Jewelry Store closing. These bars was said to be made of lead. The 2 thin bars doesn't look like lead to me. My question is, is there a simple test that can be done to determine if the pieces are lead or zinc? If zinc, can this be used in a sulphuric gold stripping cell?
One last question and I will give you a break. Should I try to clean the material before I strip the material in the sulphuric cell. These necklaces and other Jewelry have everything from sweat salts to oils, dead skin and as you have said another post on the forum, this material has a little of everything in and on them. 
If I do not clean them first will this effect the process when I get to the point of being ready to melt values. I have read that even a little body oil will cause fine gold to float among many other problems caused by dirty material. Or can I just wait until I have rinsed and filtered off the values and incinerate to a red glow, not melt, but do as you said with the gold filled to clean it before putting it in nitric?
I know this is more than just a couple of questions and I apoligize but thank you for your help.
Thank you in advance for anyone who can help.
Oneal58


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## niteliteone

hello oneal58,
Hope your doing well today. I've been following this thread since you started and am glad to see you are still at it.

I'm not able to fully answer the questions you have for Harold but will help a little while you are waiting for an answer to your questions. Study these points and see if you can SEE how these apply.

The current thru your cell will be a result of the voltage applied and the resistance of the cell itself. As the gold removes from the jewellery the amperage will start high and as the gold plating decreases so will the current. When the gold removal is finished the cell amperage should drop close to zero. 

Start with one or two pieces at first and watch what happens to the current flow to the cell. By watching the ammeter as it nears zero you have finished removing gold from the piece. 

The current thru the cell causes the acid to heat up. Heat is your enemy in the cell. Keep an eye on the temperature of the acid. DO NOT let it go over 120 degrees F or it will start attacking the copper in the jewellery fast. 

Also with the dirty jewelery, remember that the acid is a strong solvent and will consume the oils and dirt which will contaminate the acid and you will NOT be able to remove it. Once contaminated the acid will always be contaminated. And this will have an affect on the rest of the process.

Study these points while waiting for Harold to get back to you.

Tom C.


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## jimmydolittle

Also with the dirty jewelery, remember that the acid is a strong solvent and will consume the oils and dirt which will contaminate the acid and you will NOT be able to remove it. Once contaminated the acid will always be contaminated. And this will have an affect on the rest of the process.

This is why you should incinerate the stuff before you place it in your cell, to burn of the dirt, and oils on it. Make sure all the pieces are red hot, then let it cool down. It should help prevent the contamination. I've seen it in some of Harold's posts before.


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## Oneal58

Hi niteliteone and Jimmydolittle, thank you both for posting and answering some important questions I had. I will be around, not going anywhere. I have had this passion all my life. As I said in an earlier post, I just got the time now to follow up on it. 
You have created a couple of more questions for me now that you have the answers to, I am sure. If you don't mind taking the time?
So, what voltage to start with, 6volts, 12volts or other? You said when voltage drops to zero the work is done, stripping of the gold plating has been completed. 
Can you explain why that is?
I know that some of the gold plated items I have are made of what looks like brass through and through. Isn't brass a pretty good conductor on it's own? So, why would the amperage drop to zero when the gold plate is gone and it still has the brass there to use as a conductor? Also, I have filed some of the plating on the pieces and I see a thin copper layer there, though very thin it is, it's a copper layer there. 
Is the answer to this question is that gold is that much of a better conductor than brass or copper and that is the reason the amps drop to zero? 
Are there some gold plated items made of zinc? Also I have many pieces that look like the metal underneath is brass. These pieces are not magnetic, but they look to be made of brass.
Could this be gold filled that isn't marked in any way? 
Will a Stainless Steel thermometer be OK to use to check the heat of the electrolyte, if it reads quickly. Or do I need an all glass thermometer? 
I would not even mention this because Harold has already told me to incinerate the pieces. I believe wholeheartedly that, I do not question it whatsoever. But, I have some watch band tops that are absolutely dirty beyond belief. They are, what looks to be 1/4 full of krud. On the band tops particularly and only, would a wash in Lye hurt them, only the watch band tops? Or will incinerating get all that krud too?
Could I use enclosed ice packs to pack around my vessel to try and keep the electrolyte cool or is this too dangerous (or too stupid) to have the ice packs (water) too close to the sulphuric acid? Or maybe sit the cell on a seperater of some kind so no water could get to the cell? But, If I had one burst for some reason, I know that would be bad even if it was on the floor! So, this is probably a bad idea, right? Or could be just plain stupid, but I needed to ask?
Thank you niteliteone and jimmydolittle in advance for taking your time to answer my questions, it is very much appreciated. 
Oneal58


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## butcher

Oneal58, I sure would like to hear you yoddle an aution. :lol:

maybe if I get something to sell you could help.


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## Oneal58

Hi Butcher, hope you are doing well today. You know, I still do Charity Auctions for the churches around in the area. I can still go for a couple of hours before my breath leaves me. 
I live in a farming community and the churches around here raise a good portion of their donations at auctions once a year. It's a tradition that we have fun at. There is a lot of horseplay and we all have a good time. Farmers usually will give once a year instead of paying their tithes weekly or monthly. They usually have an amount their going to spend and really don't care if they get caught with something. They will run the bid on their friends and that goes back and forth. I have sold a bushel of sweet potatoes for $1000.00 before. Two friends bidding against each other. So, you can see how it can be fun. They, (Church) start up the last of Sept. when the crops are mostly out of the fields and run through Oct. Timed just right, while the farmers still have some money in their pockets. Maybe if you're passing through this area in Sept. or Oct. you could attend one of the auctions. All you have to do is raise your hand and keep it their and I would take care of the rest of it. I promise I wouldn't take your bid more than say, 20 times before you could get your hand back down. :lol: Now, you would be embarressed and pay the price or sneak out  . Which one would you do? Just kidding Butcher :twisted: I have never run the bid on anyone but I have been accused of it a couple of times. First time buyer's don't realize there are others in the room bidding against them at first. But they learn quickly after buying a few things. :shock: But I would always give them a refund if they asked for it. I just wanted to teach them how to bid their first time at auction. It's good to hear from you Butcher. I just wanted to talk to you this time instead of bombarding you with questions. Everyone needs a rest every once in a while. Wasn't kidding about the auction, come on down, we will take care of you. If I remember correctly you are in Oregon, right, Oregon has a lot of stumps? If I am wrong about that please forgive me. That's a long, long way from S.C. isn't it. I am going to let you rest Butcher for a couple of days. But please give me a hand when I get through this Sulphuric Cell trials. Then I will be moving to the hard stuff as they say. 
Good hearing from you Butcher, 
Oneal


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## niteliteone

Oneal58,
I’ll take these one at a time and do what I can.
1. *So, what voltage to start with, 6volts, 12volts or other? You said when voltage drops to zero the work is done, stripping of the gold plating has been completed. *

A standard 12 volt supply should do fine.
Actually I said when the current drops to zero.

*Can you explain why that is?*
It is the reaction of the acid on the gold that allows the current to flow, so when the gold is removed from the jewellery the current will drop to “near” zero. 
If you leave the jewellery in the cell after the current drops it will slowly attack the base metals dissolving them into solution. This is why you need to watch and remove the jewellery when the current drops near zero.

*2. I know that some of the gold plated items I have are made of what looks like brass through and through. Isn't brass a pretty good conductor on its own? So, why would the amperage drop to zero when the gold plate is gone and it still has the brass there to use as a conductor?*

Yes brass is a good conductor in normal circumstances. But remember we are dealing with sulfuric acid as the conductor and as long as we keep base metals out of solution the resistance will be very high preventing most current flow.

*3. Are there some gold plated items made of zinc?*

I’m sure there are some but I can’t say for sure.

*4. I have many pieces that look like the metal underneath is brass. These pieces are not magnetic, but they look to be made of brass.
Could this be gold filled that isn't marked in any way?*

I don’t know the answer to this question.

*5. I would not even mention this because Harold has already told me to incinerate the pieces. I believe wholeheartedly that, I do not question it whatsoever. But, I have some watch band tops that are absolutely dirty beyond belief. They are, what looks to be 1/4 full of krud. On the band tops particularly and only, would a wash in Lye hurt them, only the watch band tops? Or will incinerating get all that krud too?*

If it were me, I would mix a little soap and water and with a toothbrush remove as much excess filth as I could before incineration. But that is just me. Wear gloves.

*6. Could I use enclosed ice packs to pack around my vessel to try and keep the electrolyte cool or is this too dangerous (or too stupid) to have the ice packs (water) too close to the sulphuric acid? Or maybe sit the cell on a separator of some kind so no water could get to the cell? But, if I had one burst for some reason, I know that would be bad even if it was on the floor!* 

Is it safe to smoke a cigarette while putting gas in your car? I know I can throw a lit match into a full can of gas and the match will go out. No boom most of the time.

Get the point? You can do it many times with no problem, just like the match and gas can. It only takes that one time, a mistake or accident happens and you will wish you never had water near sulfuric acid. The out gassing can be very fast and cause a lot of injuries before you even know what happened. 

What happens if your wife would throw some water on a grease fire on the stove?

Why tempt faith? Just DON’T do it. Take a break when it gets warm.

*7. So, this is probably a bad idea, right? Or could be just plain stupid, but I needed to ask?*

Bad idea for sure.
The only stupid questions are when you don’t ask when you don’t know!

I would rather spend hours explaining safety to someone than spend a single minute thinking about them in the hospital because I didn’t have the time to explain safe practices to them.

Tom C.


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## kadriver

Oneal58:

Hello, I received your email and I tried to reply. Was wondering if you got the message I sent back to you?

I live near Charleston - about 2 hours from you.

I would be glad to help you in any way that I can.

kadriver


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## kadriver

Oneal58:

I was reading through the posts and seen where you were looking to get some nitric acid.

I just bought 5 gallons from Terrace Packaging in Kansas City. 67% technical grade. I use it to refine with and it works perfectly.

I would be willing to sell you some of it to help you out.

I paid $207 for 18.92 liters (5 gallons) shipped to my door.

Thats about $11 per liter. I will sell you a 2.5 liter bottle for $30.

We live close enough to each other that it may be possible to drive and meet in the middle - have some coffee, talk shop, and get you some nitric acid to get started.

Send me an email so we can get connected.

kadriver


----------



## Oneal58

Thanks Tom, that has cleared that up for me. I appreciate your help and everyone's help here. I am sure thankful this site is here. 
Tom, I have made a cell and I have used #10 bare copper ground wire as my frame. I then took and stripped telephone wire and made a basket weave pattern to lay my material on. I don't have any sides or front on the frame. My thinking is to keep the Faraday effect to a minimum. When I hook my cathode and anode up can I parallel off of the main voltage supply to say 2 other locations on the anode and cathode? If I remember correctly voltage in a series DC circuit is additive and voltage in a parallel DC circuit stays the same and the amps /current flow is additive. So, if I put the main power supply in the middle and branched off the main supply to each end of the anode and cathode would this help or hurt. But, by doing this may short the circuit out easily? Have you heard of anyone trying this? And the main thing is does it help any to do this? It seems like it would but I am not sure. I will be using lead as my anode and it is solid. I don't know if it would help on the anode, but could it hurt? Just alligator clip over to each end of the anode and cathode from the supply in the middle? After thinking about this, it may give you more current flow say if you have your anode and cathode too far apart. About what distance apart (anode/cathode) do you set your cell up to run?
Have you ever made a mistake and tried stripping a karat piece? If you have what does it look like, does it turn dark or keep it's gold color?
One more question and I will stop bothering you. About how many seconds do you allow your circuit to run. Or how many seconds does it take to strip down a heavy necklace when cell is set up right? Is it best to keep the necklaces hooked together so the current can form a loop on each piece. I can see this helping if the necklace it's touching is only touching another piece in one place that has a good connection with the cathode? Thanks Tom for taking the time.
Oneal58


----------



## Oneal58

kadriver said:


> Oneal58:
> 
> Hello, I received your email and I tried to reply. Was wondering if you got the message I sent back to you?
> 
> I live near Charleston - about 2 hours from you.
> 
> I would be glad to help you in any way that I can.
> 
> kadriver


Hi kadriver, I missed your post untill now. I very much thank you for answering my question about the Niric Acid. If you would do that for me it would be a great help. What is the best way to contact you to get the particulars together to meet. I hate you having to drive half-way for me. That is really doing me a big favor. Should I contact you through email or is there another way that's better. I know with the identify theft the way it is now you have to be careful anymore. I would love to meet with you. My wife always tags along with me, if that's OK. Let me know the best way to set this up. I have been to North Charleston many times. But thats about where my knowledge of Charleston ends. When I was young I would stay with my cousin during the summer a couple of weeks. We would go over to the airport and watch the airplanes land and take off. I see you are a pilot. Many years ago I started on my pilots license and ran out of money and had to stop. I couldn't, in good conscience see putting the money in something that I loved while I had kids that needed things, family to support. I went to ground school at Tech and went on to take the test in Conway, S.C.. It's a little airport right off US378 before you get to Conway. I flew until I was ready to go get tested and that is where I had to stop because of $$. I had dreams of becomming a crop duster but just never made enough money to make that dream happen. This has been 38 years ago and it's getting too late to pick it back up. I don't think I could pass the physical now anyway. The reason I was training in a Cessna 172 and not a trainer was that I was a member of the Civil Air Patrol. We had a member there that was a Flight Instructor. We used the Civil Air Patrol Plane and I would only have to pay the Instructor by the hour and put the fuel into the Cessna 172. So getting the hours in like that was very reasonable. We had several CAP Members doing the same thing that I was doing with the airplane/Instructor at the same time. But then it was noticed by the home office that too many hours was being put on the airplane above the required amount of hours each month. So, that ended the cheap flying lessons and that pretty much put an end to my flying. But let me know what the best way of contacting you on the site is. I very much look forward to meeting with you. I thank you for doing this for me. Not many will go as far out of their way to help someone as you have offered. And especially spend their own money to help someone. So, I would very much like to meet with you. 
Oneal58


----------



## butcher

I also think Kadriver is great for extending his hand in friendship here, that is a fair price, and very nice gesture. 


I love to hear the auctioneer sing, but try to stay away from them, as you say seems like the price can go up before I can put my hand down, or I just do not know when to quit raising my hand.


----------



## Oneal58

Hi Butcher, I realize that a hand has been offered in friendship and it is very much appreciated and humbly accepted. Not too many will extend a helping hand like that anymore when it involves a person's time and really his money. So, I am very greatful and humbled by kadriver's offer. 
As far as your bidding at auction, it very well could be a little of both. Years ago on ebay people would get caught up in bidding wars. This also still happens at regular auctions with buyer's who have little bidding experience. This would usually end up with one or the other bidder paying far too much for an item. Lots of times buyer's remorse would set in and a lot of refunds had to be given during these times. At my Auctions I had a rule, when the hammer went down the bidder owned the item. If the item fell into 1,000 pieces after it was in his/her hand, they owned all 1,000 pieces of it. A new buyer has to pay their due's to become a smart buyer. I felt like it was the buyer's job to bid rationally, not the Auctioneer's job to teach him/her. This doesn't happen too much anymore though. 
Ebay, has educated most potential buyers. On Ebay anymore buyer's wait untill the last few seconds in an auction to bid and know enough now to place all they plan to bid on the item before hand. Anymore, Ebay gives the other bidder a chance to bid again before ending the auction. This has slowed down the amount of snipping as there was before the changes too. You can use a program now to bid for you. Just place the amount you are willing to pay for the item and the program will increase your bid without you being at home or even on the computer. So when someone is trying to snipe the item the program will increase your bid automatically until it reaches your maximum bid amount. That's even if the auction has timed out. I like this about Ebay but I feel that the expenses that ebay charges are getting too high now for the seller. He is having to pass some of this cost on to the buyer. With the last increase recently, you have to pay for your pictures you load if more than 1, even if you host them yourself. They also charge a shipping fee charge which I think is rediculous. Yes,on top of those fees there are listing fees, picture fees, selling out of the country fees, % of shipping fees, final value fees, and then Paypal Fees. I probably have left out a couple that I don't remember. But if you have something that needs to be in front of a lot of people, Ebay is still the way to go. I don't think that Ebay is taking into consideration that the item being sold has to be found, bought, cleaned up, work involved in listing and answering emails, expenses in fuel and time involved finding item. And of course you end up paying too much for an item no matter who you are from time to time. So you do not make money on every item you sell. On Ebay forum, I have talked to people that say their Ebay bill each month is more than they are making. So, I believe Ebay has hit the wall. They have reached a place that anymore increases will shut a lot of sellers down. Really the new charges that Ebay has applied is one of the reasons I decided to start refinning my Karat Gold instead of just selling it on Ebay. I have sold and bought tens of thousands of items during my career as an Auctioneer. But knowledge is a must to make money at anything you do. Just like refinning, you have to have the knowledge to make any money at it, as you are well aware of. You have got to get it right or you will ruin your reputation at the very start. If you can't be trusted or someone questions your competance in refinning you have lost the battle before it begins. That's why I am so very thankful for all of you here on this site. You do not have to answer any of these questions. You take your time and energy to help others who has an interest in refinning. Knowing that, in a sense they will be your competition in one way or the other. But you still do it. So, that makes each and every one of you very special to me. Oh well, wife says she wants me to watch a movie with her. Talk to you later Butcher. 
Oneal


----------



## qst42know

> I love to hear the auctioneer sing, but try to stay away from them, as you say seems like the price can go up before I can put my hand down, or I just do not know when to quit raising my hand.



I know a few hyper speed auctioneers that if they saw 5 hands go up they could call an increment for each before the last in line had a chance to pull their hand down. You have to watch the quick ones very closely. :mrgreen:


----------



## Oneal58

Hi Tom,





I just finished incinerating a crucible of gold plated necklaces to go into the Sulphuric Cell. What I ended up with was what you are looking at in the image I am loading. Do you have any idea what went wrong? The heat turned all of the gold to a grey color. No gold color is there. Maybe on just one necklace there is a little gold color left but that's it. The gold dissapeared? Have any idea? These necklaces are the ones that are magnetic?The URL is below. I don't know if I did this right or not? But you should be able just to post the address in your browser and pull the picture up? Thanks, Oneal58




niteliteone said:


> Oneal58,
> I’ll take these one at a time and do what I can.
> 1. *So, what voltage to start with, 6volts, 12volts or other? You said when voltage drops to zero the work is done, stripping of the gold plating has been completed. *
> 
> A standard 12 volt supply should do fine.
> Actually I said when the current drops to zero.
> 
> *Can you explain why that is?*
> It is the reaction of the acid on the gold that allows the current to flow, so when the gold is removed from the jewellery the current will drop to “near” zero.
> If you leave the jewellery in the cell after the current drops it will slowly attack the base metals dissolving them into solution. This is why you need to watch and remove the jewellery when the current drops near zero.
> 
> *2. I know that some of the gold plated items I have are made of what looks like brass through and through. Isn't brass a pretty good conductor on its own? So, why would the amperage drop to zero when the gold plate is gone and it still has the brass there to use as a conductor?*
> 
> Yes brass is a good conductor in normal circumstances. But remember we are dealing with sulfuric acid as the conductor and as long as we keep base metals out of solution the resistance will be very high preventing most current flow.
> 
> *3. Are there some gold plated items made of zinc?*
> 
> I’m sure there are some but I can’t say for sure.
> 
> *4. I have many pieces that look like the metal underneath is brass. These pieces are not magnetic, but they look to be made of brass.
> Could this be gold filled that isn't marked in any way?*
> 
> I don’t know the answer to this question.
> 
> *5. I would not even mention this because Harold has already told me to incinerate the pieces. I believe wholeheartedly that, I do not question it whatsoever. But, I have some watch band tops that are absolutely dirty beyond belief. They are, what looks to be 1/4 full of krud. On the band tops particularly and only, would a wash in Lye hurt them, only the watch band tops? Or will incinerating get all that krud too?*
> 
> If it were me, I would mix a little soap and water and with a toothbrush remove as much excess filth as I could before incineration. But that is just me. Wear gloves.
> 
> *6. Could I use enclosed ice packs to pack around my vessel to try and keep the electrolyte cool or is this too dangerous (or too stupid) to have the ice packs (water) too close to the sulphuric acid? Or maybe sit the cell on a separator of some kind so no water could get to the cell? But, if I had one burst for some reason, I know that would be bad even if it was on the floor!*
> 
> Is it safe to smoke a cigarette while putting gas in your car? I know I can throw a lit match into a full can of gas and the match will go out. No boom most of the time.
> 
> Get the point? You can do it many times with no problem, just like the match and gas can. It only takes that one time, a mistake or accident happens and you will wish you never had water near sulfuric acid. The out gassing can be very fast and cause a lot of injuries before you even know what happened.
> 
> What happens if your wife would throw some water on a grease fire on the stove?
> 
> Why tempt faith? Just DON’T do it. Take a break when it gets warm.
> 
> *7. So, this is probably a bad idea, right? Or could be just plain stupid, but I needed to ask?*
> 
> Bad idea for sure.
> The only stupid questions are when you don’t ask when you don’t know!
> 
> I would rather spend hours explaining safety to someone than spend a single minute thinking about them in the hospital because I didn’t have the time to explain safe practices to them.
> 
> Tom C.


----------



## kadriver

Oneal58:

If you guide your cursor over my name to the left of this post and hover it there, a drop down menu will appear. From this menu select email kadriver.

In your email to me, please put your email address in the text of the message. I will email you back and we can get connected that way.

I look forward to hearing from you.

By the way, here is a picture of a gold bar that I finished about an hour ago. I like to work late at night into the early morning hours. It is quiet and there are no phone calls or other interuptions.

kadriver


----------



## qst42know

> I just finished incinerating a crucible of gold plated necklaces to go into the Sulphuric Cell. What I ended up with was what you are looking at in the image I am loading. Do you have any idea what went wrong? The heat turned all of the gold to a grey color.



Base metal brass plate will oxidize away, and base metals under the gold may oxidize and the gold may be in the dust produced from the incineration.

I haven't processed the very low grade stuff but assume the incineration needs done from below at a temperature that will destroy any lacquer, organics, and oils but carefully to save any dust produced.

How you incinerated matters. And it does for gold filled as well. Did you use a torch from above for your incineration or heat from below?


----------



## Harold_V

It's entirely possible the heat allowed the gold to migrate to the base metal. It's not lost, just not necessarily visible. Gold migration is a well known phenomenon. It may or may not respond to being stripped if it migrated inward, but it could be recovered by dissolution of the base metal. If they were, indeed, just plated, there will be precious little gold present. If they are gold filled, a stripping cell is the wrong approach, so lose that idea and get on with dissolving the base metal with your choice of solvent. Use nitric if you have it at your disposal. It's fast and efficient. 

Harold


----------



## qst42know

If you incinerated from above in that melt dish, the slight signs of color may be some of your gold.


----------



## Oneal58

Hi qst42know, 
You are exactly right, that's why a smart bidder will wait to see who is bidding and the smart bidder will always follow the Auctioneer to see where he is getting his bids from. Some Auctioneers will just pull the bids out of the air. If you see this happening it's best just to ask the Auctioneer out loud, in front of the crowd, WHERE ARE YOU AT? This will normally slow this type behavior down if he knows someone is following him closely. I have never liked this type behavior by Auctioneers. They give the profession a bad name and leave a bad taste in the buyer's mouth. I don't blame the bidder, I just will never attend that auction again, if I see this happening. But I always will make a remark to the Auctioneer why he will never see me again at his auction. The Auctioneer needs to hear this from a bidder. Need to try and get him to clean his act up if he is going to gain the public"s trust. If I am at an auction and I catch the auctioneer doing this I will do what I suggested above. It will embarrass the auctioneer if he gets caught taking bids from Ghost Bidders. 
But just remember, not all Auctioneers are like this. Most of us have enough integrity to keep the auction clean. But, it still happens far too often. 
Thanks, Oneal58



qst42know said:


> I love to hear the auctioneer sing, but try to stay away from them, as you say seems like the price can go up before I can put my hand down, or I just do not know when to quit raising my hand.
> 
> 
> 
> 
> I know a few hyper speed auctioneers that if they saw 5 hands go up they could call an increment for each before the last in line had a chance to pull their hand down. You have to watch the quick ones very closely. :mrgreen:
Click to expand...


----------



## Oneal58

Thanks qst42know for your reply. It is puzzling that it seems that I burned off all the gold? I guess I need to run the pieces to see if there is any gold there? Can you tell by the amount of powder I should get from the necklaces in the picture?
Thanks, 
Oneal58


qst42know said:


> If you incinerated from above in that melt dish, the slight signs of color may be some of your gold.


----------



## Oneal58

Hi Harold_V, 
It's good to hear from you Harold, I thought you had forgot about me? Did you get the post that I posted for you? I have your name on it and there are several questions there that I have been told that you would be able to answer. Could you please take a look at it, I would very much appreciate it if you would. I am at the point of trying to run my first Sulphuric Cell run. I think I am going to leave the necklaces that are magnetic alone, for right now. This incineration was done on some of the pieces that are magnetic. When I incinerate the non-ferrous jewelry pieces this darkening/greyish coloring, disappearing of the gold color, does not happen? So, I am seeing that if a necklace/jewelry has a lot of ferrous metals in it the darkening/color change occurs. As you posted, gold migrating into the ferrous base metals. And if the necklace is non-ferrous this type darkening/gold color loss did not occur. So, I would have to dissolve all the metal in the necklaces to recover the little bit of goldplate that could be there but just migrated into the ferrous base metals. Which is not worth the acid used or the effort which would be involved. Later on, I may dissolve a few of the magnetic jewelry pieces that turned grey just for the sake of experience gained. 
Harold, if you could take a look at the post I put up for you it would be appreciated. Or I can post again if that's the better route for you? 
Thank you Harold,
Oneal58



Harold_V said:


> It's entirely possible the heat allowed the gold to migrate to the base metal. It's not lost, just not necessarily visible. Gold migration is a well known phenomenon. It may or may not respond to being stripped if it migrated inward, but it could be recovered by dissolution of the base metal. If they were, indeed, just plated, there will be precious little gold present. If they are gold filled, a stripping cell is the wrong approach, so lose that idea and get on with dissolving the base metal with your choice of solvent. Use nitric if you have it at your disposal. It's fast and efficient.
> 
> Harold


----------



## Oneal58

Hi qst42know,
I did incinerate from above down onto the material. I did notice a variation in the color of the plating between the non-ferrous metals and the ferrous metals. I just assumed it had something to do with the karat of the plating? This plating could have very well been brass plating. Then on top of that I incinerated from above?
I also used Borax off the shelf in Wal-Mart. Does anyone know if the Borax off the shelf is good enough to use as a flux? When I was treating/seasoning my crucible I did not get an even thin flow on my crucible as I have seen on Lazersteve's site? You can see in my image that there are little spots that I could not get to melt.
I have 2 different types of torches. I have the acetylene/oxygen and I have a mapp gas torch. I used the mapp gas torch to try to season the crucible with Borax and also to incinerate the ferrous jewelry pieces. Was I getting enough heat from the mapp gas torch? My crucible would have a dull red glow with the lights off? 
As far as the dust produced, I didn't see any gold dust in the bottom of the crucible. 
Thanks qst42know,
Oneal58



qst42know said:


> I just finished incinerating a crucible of gold plated necklaces to go into the Sulphuric Cell. What I ended up with was what you are looking at in the image I am loading. Do you have any idea what went wrong? The heat turned all of the gold to a grey color.
> 
> 
> 
> 
> Base metal brass plate will oxidize away, and base metals under the gold may oxidize and the gold may be in the dust produced from the incineration.
> 
> I haven't processed the very low grade stuff but assume the incineration needs done from below at a temperature that will destroy any lacquer, organics, and oils but carefully to save any dust produced.
> 
> How you incinerated matters. And it does for gold filled as well. Did you use a torch from above for your incineration or heat from below?
Click to expand...


----------



## Oneal58

Absolutely makes your mouth run water kadriver. This is my end goal! Waiting to hear from you.
Thanks, Oneal



kadriver said:


> Oneal58:
> 
> If you guide your cursor over my name to the left of this post and hover it there, a drop down menu will appear. From this menu select email kadriver.
> 
> In your email to me, please put your email address in the text of the message. I will email you back and we can get connected that way.
> 
> I look forward to hearing from you.
> 
> By the way, here is a picture of a gold bar that I finished about an hour ago. I like to work late at night into the early morning hours. It is quiet and there are no phone calls or other interuptions.
> 
> kadriver


----------



## kadriver

Oneal58:

When I first started refining about a year ago, I set up a sulfuric acid stripping cell and ran gold plated items through it for some 20 hours, give or take.

I found a post that described the cell clean out proceedure. Using that process, I recovered a few grams of gold from the stripping cell. It was very satisfying to get those few grams.

It was fun, and a great refining experience. But for the amount of time it took to get those few grams of gold it just seemed impractical - to me.

On the other hand, this is probably the only practical way to remove the gold from gold plated items.

I still have the stripping cell components, but I have never set it up and ran it since that first time.

For some, running a stripping cell may be the only source of gold that can be had.

I would encourage you to proceed with your stripping cell. I can verify that It does produce gold for refining.

Also, here is the post of the first gold bar I refined from karat scrap jewelry that I mentioned to you.

EDIT:

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=37&t=8322

END EDIT

It has many pages and gives a detailed account with lots of photos of the process I used as a first-time refiner attempting to refine my first gold bar. It was done under the guidance of this forum.

During this refining I experienced a mishap that resulted in the loss of some of my gold. I was performing a second treatment of the inquarted gold in concentrated nitric acid after the first treatment with dilute 50/50 nitric.

There are many posts from some of the most experienced refiners on the forum as they helped me through the process.

kadriver


----------



## niteliteone

Oneal58 said:


> November 20th, 2011, 1:01 pm
> Thanks Tom, that has cleared that up for me. I appreciate your help and everyone's help here. I am sure thankful this site is here.
> Tom, I have made a cell and I have used #10 bare copper ground wire as my frame. I then took and stripped telephone wire and made a basket weave pattern to lay my material on. I don't have any sides or front on the frame. My thinking is to keep the Faraday effect to a minimum. ...
> Oneal58



*1) When I hook my cathode and anode up can I parallel off of the main voltage supply to say 2 other locations on the anode and cathode? * 

Yes you can but it’s not necessary. All that is needed it a GOOD connection on each.

*2) If I remember correctly voltage in a series DC circuit is additive and voltage in a parallel DC circuit stays the same and the amps /current flow is additive. So, if I put the main power supply in the middle and branched off the main supply to each end of the anode and cathode would this help or hurt.* 

Not necessary, can only bring more problems than it possibly could solve.

*3) But, by doing this may short the circuit out easily? Have you heard of anyone trying this? And the main thing is does it help any to do this? It seems like it would but I am not sure. I will be using lead as my anode and it is solid. I don't know if it would help on the anode, but could it hurt?* 

Again, Not necessary, possibly can bring more problems than it could solve.

*4) Just alligator clip over to each end of the anode and cathode from the supply in the middle? After thinking about this, it may give you more current flow say if you have your anode and cathode too far apart. About what distance apart (anode/cathode) do you set your cell up to run?*

My cell is 4” wide and I hang the cathode on one side and the anode on the other.

*5) Have you ever made a mistake and tried stripping a karat piece? If you have what does it look like, does it turn dark or keep its gold color?*

Never done this. I don’t know the answer.

*6) One more question and I will stop bothering you. About how many seconds do you allow your circuit to run. Or how many seconds does it take to strip down a heavy necklace when cell is set up right? Is it best to keep the necklaces hooked together so the current can form a loop on each piece. I can see this helping if the necklace its touching is only touching another piece in one place that has a good connection with the cathode? *

I’ve never timed the process, I just watch the process and when the current drops I will stir the pieces with a glass rod, watch the ammeter and remove the pieces when the current drops and stays low.


I haven’t experimented much with this process. My main concern is not to reinvent the wheel, but to understand what is happening IN the process and then adjust my parameters to get the setup that produces the best repeatable results.
But I did start with the basic setup first, *as should you.* That way any questions you ask can easily be answered without trying to troubleshoot the system before the process.

Tom C.


----------



## Oneal58

Hi kadriver, I will be ecstatic when I get to post my picture along with yours and the other members, with a big picture of my first bar. Yes, I believe you are right. Start at the ground level and work my way up, just for the experience. That's my plan, but believe me it's tempting to go for the gold, and skip the cell stripping. kadriver, I just want to say that I just can't express how greatful I am to you for being willing to help me. Heck, you don't know me from Adams House Cat and invited me over to your house to spend the day. You just don't know how badly I would have loved to do that. But I feel it's best to let you get to know me before I impose myself on you and your family for a day. But thank you for the offer, I have questioned myself many times since our conversation today whether I should have taken you up on your offer. Believe me I wanted to badly. But I felt like it would be selfish of me to take you up on the offer. I want to wait until you get to know me. And if it's OK with you then may I take you up on that offer? I would be very greatful to you. I would love to see your setup and ask you a ton of questions. Thank you kadriver and I will see you tomorrow in Monks Corner. 
Oneal58



kadriver said:


> Oneal58:
> 
> When I first started refining about a year ago, I set up a sulfuric acid stripping cell and ran gold plated items through it for some 20 hours, give or take.
> 
> I found a post that described the cell clean out proceedure. Using that process, I recovered a few grams of gold from the stripping cell. It was very satisfying to get those few grams.
> 
> It was fun, and a great refining experience. But for the amount of time it took to get those few grams of gold it just seemed impractical - to me.
> 
> On the other hand, this is probably the only practical way to remove the gold from gold plated items.
> 
> I still have the stripping cell components, but I have never set it up and ran it since that first time.
> 
> For some, running a stripping cell may be the only source of gold that can be had.
> 
> I would encourage you to proceed with your stripping cell. I can verify that It does produce gold for refining.
> 
> Also, here is the post of the first gold bar I refined from karat scrap jewelry that I mentioned to you.
> 
> EDIT:
> 
> http://goldrefiningforum.com/phpBB3/viewtopic.php?f=37&t=8322
> 
> END EDIT
> 
> It has many pages and gives a detailed account with lots of photos of the process I used as a first-time refiner attempting to refine my first gold bar. It was done under the guidance of this forum.
> 
> During this refining I experienced a mishap that resulted in the loss of some of my gold. I was performing a second treatment of the inquarted gold in concentrated nitric acid after the first treatment with dilute 50/50 nitric.
> 
> There are many posts from some of the most experienced refiners on the forum as they helped me through the process.
> 
> kadriver


----------



## Oneal58

Hi Tom, I have posted so many questions I get mixed up on them. If I haven't thanked you for your post I want to do that now. You have cleared up many questions that I had and I appreciate it. I get what you are saying about troubleshooting the system even before my first strip. Ok, I will just get on with it. I have stalled long enough. If everything goes well the next couple of days I will at least have some powder in the bottom of the cell to admire. 
Is there a time limit to how long one can leave the powder in the cell with the sulphuric while the rectifier is off? I have read here on the forum that some just leave the gold in the cell and just let it concentrate until the electrolyte gets so heavy laden with gold that the cell starts to short. Then it is time to decant and start over? They didn't post if they were talking about an hour, day, week or month?
Thanks, Oneal58



niteliteone said:


> Oneal58 said:
> 
> 
> 
> November 20th, 2011, 1:01 pm
> Thanks Tom, that has cleared that up for me. I appreciate your help and everyone's help here. I am sure thankful this site is here.
> Tom, I have made a cell and I have used #10 bare copper ground wire as my frame. I then took and stripped telephone wire and made a basket weave pattern to lay my material on. I don't have any sides or front on the frame. My thinking is to keep the Faraday effect to a minimum. ...
> Oneal58
> 
> 
> 
> 
> *1) When I hook my cathode and anode up can I parallel off of the main voltage supply to say 2 other locations on the anode and cathode? *
> 
> Yes you can but it’s not necessary. All that is needed it a GOOD connection on each.
> 
> *2) If I remember correctly voltage in a series DC circuit is additive and voltage in a parallel DC circuit stays the same and the amps /current flow is additive. So, if I put the main power supply in the middle and branched off the main supply to each end of the anode and cathode would this help or hurt.*
> 
> Not necessary, can only bring more problems than it possibly could solve.
> 
> *3) But, by doing this may short the circuit out easily? Have you heard of anyone trying this? And the main thing is does it help any to do this? It seems like it would but I am not sure. I will be using lead as my anode and it is solid. I don't know if it would help on the anode, but could it hurt?*
> 
> Again, Not necessary, possibly can bring more problems than it could solve.
> 
> *4) Just alligator clip over to each end of the anode and cathode from the supply in the middle? After thinking about this, it may give you more current flow say if you have your anode and cathode too far apart. About what distance apart (anode/cathode) do you set your cell up to run?*
> 
> My cell is 4” wide and I hang the cathode on one side and the anode on the other.
> 
> *5) Have you ever made a mistake and tried stripping a karat piece? If you have what does it look like, does it turn dark or keep its gold color?*
> 
> Never done this. I don’t know the answer.
> 
> *6) One more question and I will stop bothering you. About how many seconds do you allow your circuit to run. Or how many seconds does it take to strip down a heavy necklace when cell is set up right? Is it best to keep the necklaces hooked together so the current can form a loop on each piece. I can see this helping if the necklace its touching is only touching another piece in one place that has a good connection with the cathode? *
> 
> I’ve never timed the process, I just watch the process and when the current drops I will stir the pieces with a glass rod, watch the ammeter and remove the pieces when the current drops and stays low.
> 
> 
> I haven’t experimented much with this process. My main concern is not to reinvent the wheel, but to understand what is happening IN the process and then adjust my parameters to get the setup that produces the best repeatable results.
> But I did start with the basic setup first, *as should you.* That way any questions you ask can easily be answered without trying to troubleshoot the system before the process.
> 
> Tom C.
Click to expand...


----------



## niteliteone

Oneal58
I'm glad I've been able to answer your questions. It helps me learn too. :shock: 
Some of the questions you asked left me with questions too, so I went back to review the forum posts before giving you my answers. 8) Since others will read these posts, I want to be sure the information posted is correct and flows with the teaching of others.

For your question about removing the gold frrom the cell, what I have come up with is, it is a slow process compared to others, so it is OK to hold off until the cell becomes quite full, but before shorting out. 
As long as you are able to keep the cell sealed against moisture getting to the acid, diluting it to a point that it causes adverse conditions for further use.
Remember it is important to have as little H20 in the sulfuric acid as possible since to much moisture will allow the acid to attack the base metals thus causing more problems down the road.

I hope this answers your questions 
Tom C.


----------



## Oneal58

Morning Butcher, just wanted to say Hi. I haven't heard from you in a couple of days so I thought I would check in on you. I am leaving this morning to meet kadriver in Moncks Corner. It's a little town on the way to his place we decided to meet at. He is meeting me to give me some Nitric Acid, I am excited about this. You know Butcher, kadriver even invited me over to his house to spend the day without ever meeting me. I thought this was beyond the call for anyone to go out of their way to help someone else without knowing them first. I felt that taking him up on the offer was just too much to ask of him until he knows me better. I very much wanted to take him up on the offer and wanted to with all my heart but I felt like I just didn't need to impose myself upon him this much at first. But when I meet him today I hope to tell him that once he gets to know me better maybe the offer will still be there to visit him and his family at his place and take a look at his operation. I could spend a couple of hours with him and I would learn a ton!
But I hope you are doing well today Butcher. Butcher do you refine silver as well or just gold? 
Oh well, I need to get a shower to get on the road. I will talk to you later. Thanks Butcher, Oneal




butcher said:


> I also think Kadriver is great for extending his hand in friendship here, that is a fair price, and very nice gesture.
> 
> 
> I love to hear the auctioneer sing, but try to stay away from them, as you say seems like the price can go up before I can put my hand down, or I just do not know when to quit raising my hand.


----------



## butcher

Oneal, 
I think it is great you and Kadriver will get to meet each other hope you both have a good time.

I have recoverd some silver, and have used the nitric treatment to make it a higher grade silver, but have been waiting untill I get enough silver collected before I try refining it in the cell.

I am a small time hobby miner, waste recoverer and refiner, I actually spend more time recovering metals than refining them (small time shade tree refiner).

be careful on the road.


----------



## Oneal58

Hi Butcher, I am glad to see you are still around. I would have thought you would be at an auction somewhere?  Well, I can't call myself a shade tree refiner yet. But I'll bet there is a lot of modesty being displayed here?
Butcher I am just getting in from my meeting with kadriver today. What a guy he is. He took hours going into detail on every single process he used to refine his gold. It's unbelieveable that someone would do that for someone else. Go out of their way that far for others. He brought me the Nitric I needed. He also brought me some other chemicals, copper alligator clips, tin, Etc;. The things he said I would need to get started. I felt so guilty that he took so much time with me I wanted to pay him something for his time. Of course he would not take a penny. I honestly didn't think people like that were still around. I will always be endebted to him, always. I was just overwhelmed by his kindness and unselfish heart, I was blown away, honestly! I would always strive to have such a heart. I truely have been blessed today. It makes you feel good to know that these type people are among us, still. I could only hope to have such a heart. 
Butcher, this Nitric that I got from kadriver will give me a baseline to compare my homemade Nitric to. 
I stopped by a new fertilizer supplier that said he would order a bag of Potassium Nitrate for me so I will have it in the future to make my homemade Nitric. The dealer said he could not get Sodium Nitrate for me? The fertilizer dealer asked me if I wanted soluable or insoluable. Which one do I use, what is the difference? My next question, you probably already know what it is? Do you mind sharing your process with me to make Nitric out of Potassium Nitrate. What strength do you normally end up with, normally? If not, I understand, totally. 
Thanks Butcher,
Oneal58



butcher said:


> Oneal,
> I think it is great you and Kadriver will get to meet each other hope you both have a good time.
> 
> I have recoverd some silver, and have used the nitric treatment to make it a higher grade silver, but have been waiting untill I get enough silver collected before I try refining it in the cell.
> 
> I am a small time hobby miner, waste recoverer and refiner, I actually spend more time recovering metals than refining them (small time shade tree refiner).
> 
> be careful on the road.


----------



## Oneal58

Hi kadriver, my head is still spinning from today. My brain is overloaded just trying to get some notes on paper from what you have taught me today! I don't know why in the world I wasn't taking notes? I didn't expect you to open your entire process up to me, it took me by surprise! I can truely say that I was not prepared for such a course taught over hours. 
I can't believe you took up hours with me, instructing me how you refine your gold, step by step. I did not go prepared to receive the instructions you gave me. You went into detail of your entire process. You just can't put a price on this type information. Being able to ask you the questions I needed to and have you answer them right on the spot. I truely regret not taking notes, I really do. You brought me the Nitric Acid and also other chemicals, copper alligator clips, tin, etc;. Items that you said I needed to get started, and gave them to me! I just don't know how to say this, I am just overwhelmed by your big unselfish heart. It really feels good to know that I live in the same world as such people. Wanting nothing other than to help me? I don't know how I will ever repay you for your help. I honestly hope you need something that I can get or have something that you need in the future. I feel so obligated, endebted to you. I just don't know how other to express what I am trying to say other than I have truely been blessed today to meet such a wonderful person. I still can't believe it? I am so much closer to my goal now than I was this morning it's unbelieveable. You have made a life long lasting impression on me that I dare to attempt to strive for. I have never meet a more unselfish, honest person who really just wanted to help. Expecting or wanting nothing in return. You are few and far between kadriver. I would fly with you anywhere. I felt I needed to post this on the forum so others could see what type of person you really are. 
Thank you kadriver, from the bottom of my heart. 
Oneal58 and wife 


kadriver said:


> Oneal58:
> 
> When I first started refining about a year ago, I set up a sulfuric acid stripping cell and ran gold plated items through it for some 20 hours, give or take.
> 
> I found a post that described the cell clean out proceedure. Using that process, I recovered a few grams of gold from the stripping cell. It was very satisfying to get those few grams.
> 
> It was fun, and a great refining experience. But for the amount of time it took to get those few grams of gold it just seemed impractical - to me.
> 
> On the other hand, this is probably the only practical way to remove the gold from gold plated items.
> 
> I still have the stripping cell components, but I have never set it up and ran it since that first time.
> 
> For some, running a stripping cell may be the only source of gold that can be had.
> 
> I would encourage you to proceed with your stripping cell. I can verify that It does produce gold for refining.
> 
> Also, here is the post of the first gold bar I refined from karat scrap jewelry that I mentioned to you.
> 
> EDIT:
> 
> http://goldrefiningforum.com/phpBB3/viewtopic.php?f=37&t=8322
> 
> END EDIT
> 
> It has many pages and gives a detailed account with lots of photos of the process I used as a first-time refiner attempting to refine my first gold bar. It was done under the guidance of this forum.
> 
> During this refining I experienced a mishap that resulted in the loss of some of my gold. I was performing a second treatment of the inquarted gold in concentrated nitric acid after the first treatment with dilute 50/50 nitric.
> 
> There are many posts from some of the most experienced refiners on the forum as they helped me through the process.
> 
> kadriver


----------



## butcher

Here is the classic method to make nitric acid, worked out early in the forum’s history; (Thanks to Steve and GSP brainstorming), 
I find it one of the best ways to make nitric acid without distilling.

The cold method is not good for use with silver (sulfates salts formed make troubles with silver), for silver you should distill the homemade nitric acid to get nitric without any sulfate salts, or buy the nitric acid.


http://goldrefiningforum.com/phpBB3/viewtopic.php?p=2572#2572 

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=48&t=5825




http://goldrecovery.us/forum_search.asp

Here is one of my favorites, for dissolving copper from gold plated pins and making nitric acid in same reaction:

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=38&t=6199&hilit=killing+two+birds+one+rock


----------



## nickvc

Oneal58 it says it all on the heading of the forum...Hobbyists and professionals helping one another.
For most long term members and regular contributors to the forum that holds true. 
While at times we may seem to be unhelpful to noobies it's for their own good that we point them in the direction of reading Hoke and studying refining in depth,it saves time and avoids misunderstandings if we all talk the same language and have the basics covered. 
The big news for most noobs is that nearly all of us learn something virtually every visit to the forum however long we have been refining, it's that huge a subject that no one knows it all.
I wish you luck in your quest and enjoy the learning and the results that that you achieve, you will have earned them.


----------



## kadriver

Oneal58:

I enjoyed our time together as well. I have been accused of being an instructor of sorts. I like to do it for four reason:

1) because I enjoy it.
2) a sense of duty to the profession.
3) as a tribute to those who took the time to instruct me.
4) it helps reinforce the knowlege base that I have.

I believe that the world is harsh and life can be tough.

It truely is wonderful to be able to make someone's life easier, if only for a short time.

It is the little things that are within our power; opening doors for elderly people, allowing a young mother to go ahead in the grocery line. It's these small things that can make a big difference in the lives of others.

You have my number, feel free to call me any time you have a question. If it is at my skill level, then I will try to answer it the best I can.

If it is beyond my skill level, then I will probably tell you to consult this forum.

By the way, you can find a stannous chloride recipe by simply typing in those words in the search block at the top of this page.

Good luck in your refining!

kadriver


----------



## kadriver

I almost forgot, here is the video I spoke of at our meeting yesterday:

[youtube]http://www.youtube.com/watch?v=gTBBYogskS8[/youtube]

Some of the processes have changed since I made this video.

For example, today I would never drop the gold using sodium metabisulfite dissolved in distilled water - it just creates excess waste. Adding the powder to the container of dissolved gold while stirring vigorously is the best way to go for now.

Also, I would never drop the gold in the large beaker without having it set inside of a cornigware casserole dish (or some other suitable container) to catch the AuCl if it boils over.

I have had AuCl solutions boil over onto my work bench as I was adding sodium metabisulfite due to excess heat and to much nitric acid left in the solution. This caused some of the gold to be lost!

Today, I would add about 5 ice cubes of distilled water and cool the solution before dropping the gold - especially if the solution is highly concentrated - say five ounces or more in less that a liter of liquid.

Hope this is helpful to you.

kadriver


----------



## Oneal58

Hi Butcher, thanks for your reply. I plan on using the homemade nitric down the road to process silver. So the cold methods would not be the way to go, right? I have a distilling condenser so I guess the last method would be the route to go? 
I can get large bags of potassium nitrate fertilizer, so will the same process work with (substitue) potassium nitrate instead of sodium nitrate? Butcher I know there are many post on how to make the nitric but I trust you to give me the best one. Lazersteve said he had an updated process now that he uses. I have trouble with Lazersteve's site with my computer for some reason. I cannot play the videos on his site on my computer? Have you ever watched any of the videos, did you have trouble downloading any of the videos? 
Thanks Butcher for your answer. 
Oneal58



butcher said:


> Here is the classic method to make nitric acid, worked out early in the forum’s history; (Thanks to Steve and GSP brainstorming),
> I find it one of the best ways to make nitric acid without distilling.
> 
> The cold method is not good for use with silver (sulfates salts formed make troubles with silver), for silver you should distill the homemade nitric acid to get nitric without any sulfate salts, or buy the nitric acid.
> 
> 
> http://goldrefiningforum.com/phpBB3/viewtopic.php?p=2572#2572
> 
> http://goldrefiningforum.com/phpBB3/viewtopic.php?f=48&t=5825
> 
> 
> 
> 
> http://goldrecovery.us/forum_search.asp
> 
> Here is one of my favorites, for dissolving copper from gold plated pins and making nitric acid in same reaction:
> 
> http://goldrefiningforum.com/phpBB3/viewtopic.php?f=38&t=6199&hilit=killing+two+birds+one+rock


----------



## Oneal58

Hi kadriver, hope you are doing well today. I will watch the videos in their entirety today. I am in the middle of trying to get some gold plated items stripped today, finally. From what I am seeing so far though, there is very little gold on the gold plating items that I have. But I will keep posting my results. Right now I am letting the sulphuric cool back down to run another batch. I am going to move to another vessel to see if my cathode and anode are too close together causing the acid to heat up too quickly. :?: Thanks kadriver, 
Oneal58

I


kadriver said:


> I almost forgot, here is the video I spoke of at our meeting yesterday:
> 
> [youtube]http://www.youtube.com/watch?v=gTBBYogskS8[/youtube]
> 
> Some of the processes have changed since I made this video.
> 
> For example, today I would never drop the gold using sodium metabisulfite dissolved in distilled water - it just creates excess waste. Adding the powder to the container of dissolved gold while stirring vigorously is the best way to go for now.
> 
> Also, I would never drop the gold in the large beaker without having it set inside of a cornigware casserole dish (or some other suitable container) to catch the AuCl if it boils over.
> 
> I have had AuCl solutions boil over onto my work bench as I was adding sodium metabisulfite due to excess heat and to much nitric acid left in the solution. This caused some of the gold to be lost!
> 
> Today, I would add about 5 ice cubes of distilled water and cool the solution before dropping the gold - especially if the solution is highly concentrated - say five ounces or more in less that a liter of liquid.
> 
> Hope this is helpful to you.
> 
> kadriver


----------



## Oneal58

Hi nickvc, thank you for your post. I understand completely. I can't see how anyone would attempt to get started without first reading Hoke's Book plus other material and reading this forum to be honest. To start something you must first have a starting line defined. Which I didn't have before I read the material and found this forum. As you said, it must be earned. To be honest with you, at my level of intelligence I could not achieve success without the study material and this forum for help. It's still very envolved for me. Thanks nickvc, 
Oneal58



nickvc said:


> Oneal58 it says it all on the heading of the forum...Hobbyists and professionals helping one another.
> For most long term members and regular contributors to the forum that holds true.
> While at times we may seem to be unhelpful to noobies it's for their own good that we point them in the direction of reading Hoke and studying refining in depth,it saves time and avoids misunderstandings if we all talk the same language and have the basics covered.
> The big news for most noobs is that nearly all of us learn something virtually every visit to the forum however long we have been refining, it's that huge a subject that no one knows it all.
> I wish you luck in your quest and enjoy the learning and the results that that you achieve, you will have earned them.


----------



## butcher

Oneal58,
I also have trouble seeing any video's, with a very slow computer and dial up modem connection, that keeps disconnecting every few minutes, virtually impossible to watch a video.

The difference in using potassium nitrate KNO3 and sodium nitrate NaNO3 are ratios used.

They both work very well; potassium salts formed from reaction (K2SO4) seem to me to be more insoluble (cooling too quickly seems to trap some nitric in the K2SO4 salts), (potassium salts are easier on our environment, as sodium forms salts that plants do not like).

The sodium nitrate salts are nice to make nitric from and to me seem hold less nitric acid in the salts (Na2SO4), but these salts seem to be more soluble and even after chilling they still seem to be somewhat soluble in the nitric acid.

Like I said earlier depending on what I am doing determines which one I prefer,

Your distilling unit should be lab glass, or you could use the pickle jar method I gave you a link to, both need precautions to insure safety, and keeping glassware from breaking.

There is much information on the forum of making and using nitric acid, so much that it would be hard for us to retype most all of it, so going back and reading the forum will give you more information than asking a lot of questions will, I have spent a whole lot of time studying nitric acid, making it in all concentrations, concentrating it, and the chemistry of it, some of the main points I have posted about nitric acid over the years, I keep a large note book just on this subject, (I have never had a good memory so I must keep notes of what I learn), so if you come up with a question about nitric acid I may be able to help, if not someone else here on the forum can.

The links I posted earlier are just a couple that I thought would help you get started, there are many many more great posts with information on this subject, the study of nitric acid this in itself can become a very deep subject, a man could probably spend most of his life just learning about nitric acid.

You can make a large batch of nitric acid using the cold method, and distill a portion of this for your silver needs. Or when you and Kadriver need some maybe you guys could go in together and buy what you need.

it is the sulfate salts formed from the sulfuric acid and the sodium or potassium that give problems with silver sulfate is not very soluble.

You asked earlier about soluble or insoluble KNO3 fertilizer, I think you should get soluble, as the insoluble may be prills with some type of coating (waxy?) to make them dissolve more slowly in the soil.


----------



## Oneal58

Hi Butcher,
I called the fertilizer dealer and ordered the 50 lb or 60 lb. bag of Potassium Nitrate Fertilizer. I am to pick it up monday. It's the soluable type that you instructed me to purchase. I guess I will just keep the 2 bags of Ammonia Nitrate I have purchased to put to the Garden and Flowers in the yard next spring. 
I am going to spend the holidays studying the methods of making the Nitric from the Potassium Nitrate since I can get all I want at a good (farmers) price. I plan to strip large/small silver plated items also along with what gold I can scrounge up. But I know I have a good and steady supply of silver plated items that I can get at really good prices. I am in hopes I can get enough silver off of the pieces to make it worth wild (profitable) for me to recover. It will be a slow process to learn the plating thicknesses (returns) on the hundreds of different makers of the silverplated items. Each company, which their are hundreds of, more than likely had different thicknesses of silver they applied to their products. So I will need to keep track of the amounts of silver per square inch of plating or whatever the best method will be for me to use to keep track of the returns of each. I am sure I will go through a lot of Nitric Acid so I would have to make it myself for this venture to be profitable. Hopefully I will find a good source of gold and will not have to refine the silverplate. But everyone is after the gold, as you are well aware of. I have a friend who owns/operates his own computer repair shop. I am in hopes of getting his scraps but he currently sells them on Ebay. I am sure I could match this price at least. My offer would be less than what he could get off Ebay but he would not have all the expenses/work involved by listing on Ebay. But, that route also keeps me processing the plated material. I would much rather be in the refinning of the Karat gold as would everyone else and his brother. So hopefully I will find a source of the Karat Gold later on down the road. The Karat Gold as you know, would be less of a headache from what I have learned so far. It would also be much more profitable time wise (amount of material handled) than the plated material. Thank you Butcher, if I hit a snag on making my Nitric next week I may have to bother you. Thank you for all your help Butcher.
Oneal58



butcher said:


> Oneal58,
> I also have trouble seeing any video's, with a very slow computer and dial up modem connection, that keeps disconnecting every few minutes, virtually impossible to watch a video.
> 
> The difference in using potassium nitrate KNO3 and sodium nitrate NaNO3 are ratios used.
> 
> They both work very well; potassium salts formed from reaction (K2SO4) seem to me to be more insoluble (cooling too quickly seems to trap some nitric in the K2SO4 salts), (potassium salts are easier on our environment, as sodium forms salts that plants do not like).
> 
> The sodium nitrate salts are nice to make nitric from and to me seem hold less nitric acid in the salts (Na2SO4), but these salts seem to be more soluble and even after chilling they still seem to be somewhat soluble in the nitric acid.
> 
> Like I said earlier depending on what I am doing determines which one I prefer,
> 
> Your distilling unit should be lab glass, or you could use the pickle jar method I gave you a link to, both need precautions to insure safety, and keeping glassware from breaking.
> 
> There is much information on the forum of making and using nitric acid, so much that it would be hard for us to retype most all of it, so going back and reading the forum will give you more information than asking a lot of questions will, I have spent a whole lot of time studying nitric acid, making it in all concentrations, concentrating it, and the chemistry of it, some of the main points I have posted about nitric acid over the years, I keep a large note book just on this subject, (I have never had a good memory so I must keep notes of what I learn), so if you come up with a question about nitric acid I may be able to help, if not someone else here on the forum can.
> 
> The links I posted earlier are just a couple that I thought would help you get started, there are many many more great posts with information on this subject, the study of nitric acid this in itself can become a very deep subject, a man could probably spend most of his life just learning about nitric acid.
> 
> You can make a large batch of nitric acid using the cold method, and distill a portion of this for your silver needs. Or when you and Kadriver need some maybe you guys could go in together and buy what you need.
> 
> it is the sulfate salts formed from the sulfuric acid and the sodium or potassium that give problems with silver sulfate is not very soluble.
> 
> You asked earlier about soluble or insoluble KNO3 fertilizer, I think you should get soluble, as the insoluble may be prills with some type of coating (waxy?) to make them dissolve more slowly in the soil.


----------



## Oneal58

Hi Tom, 
I need to ask you a question if you don't mind? I have been running my goldplated items through the sulphuric cell tonight. When I start the cell up I get anywhere from 6-8 amps and then after about 25-45 seconds the current drops to less than 1 amp (about .5 amps). I was worried at first I wasn't getting the gold off but I have inspected the pieces that's comming out of the cell and as far as I can tell it's getting all the gold? I get no reaction when tray is put back into the acid and almost no current flow. 
Is this a normal time (25-45 seconds) to do the stripping of the Jewelry pieces. The reason I ask is I watched the video on youtube of Lazersteve's stripping of the necklaces. He had his rectifier still working on the necklaces after10 minutes if I remember correctly? I wanted to consult with you about this. If I am getting almost no current flow on the amp meter the process is complete, isn't it? Even if it hasn't been but 25-45 seconds. I am trying to put at least 150 grams in at a time because of the size of my home made tray. My tray is not big enough to get anymore in at a time. But Lazersteve's doing 200 grams and going 5-10 minutes. Even at 50 grams more material there shouldn't be that much time difference, should they? 
Just wanting to ask you what is the average time your cell is taking to strip your goldplated items? I am just concerned that I may not be getting all the gold off during this short amount of time? Even if the items look like the gold is gone and the amps have dropped. 
Thanks in advance Tom for any advice. 
Oneal58



Oneal58 said:


> Hi Tom, I have posted so many questions I get mixed up on them. If I haven't thanked you for your post I want to do that now. You have cleared up many questions that I had and I appreciate it. I get what you are saying about troubleshooting the system even before my first strip. Ok, I will just get on with it. I have stalled long enough. If everything goes well the next couple of days I will at least have some powder in the bottom of the cell to admire.
> Is there a time limit to how long one can leave the powder in the cell with the sulphuric while the rectifier is off? I have read here on the forum that some just leave the gold in the cell and just let it concentrate until the electrolyte gets so heavy laden with gold that the cell starts to short. Then it is time to decant and start over? They didn't post if they were talking about an hour, day, week or month?
> Thanks, Oneal58
> 
> 
> 
> niteliteone said:
> 
> 
> 
> 
> 
> Oneal58 said:
> 
> 
> 
> November 20th, 2011, 1:01 pm
> Thanks Tom, that has cleared that up for me. I appreciate your help and everyone's help here. I am sure thankful this site is here.
> Tom, I have made a cell and I have used #10 bare copper ground wire as my frame. I then took and stripped telephone wire and made a basket weave pattern to lay my material on. I don't have any sides or front on the frame. My thinking is to keep the Faraday effect to a minimum. ...
> Oneal58
> 
> 
> 
> 
> *1) When I hook my cathode and anode up can I parallel off of the main voltage supply to say 2 other locations on the anode and cathode? *
> 
> Yes you can but it’s not necessary. All that is needed it a GOOD connection on each.
> 
> *2) If I remember correctly voltage in a series DC circuit is additive and voltage in a parallel DC circuit stays the same and the amps /current flow is additive. So, if I put the main power supply in the middle and branched off the main supply to each end of the anode and cathode would this help or hurt.*
> 
> Not necessary, can only bring more problems than it possibly could solve.
> 
> *3) But, by doing this may short the circuit out easily? Have you heard of anyone trying this? And the main thing is does it help any to do this? It seems like it would but I am not sure. I will be using lead as my anode and it is solid. I don't know if it would help on the anode, but could it hurt?*
> 
> Again, Not necessary, possibly can bring more problems than it could solve.
> 
> *4) Just alligator clip over to each end of the anode and cathode from the supply in the middle? After thinking about this, it may give you more current flow say if you have your anode and cathode too far apart. About what distance apart (anode/cathode) do you set your cell up to run?*
> 
> My cell is 4” wide and I hang the cathode on one side and the anode on the other.
> 
> *5) Have you ever made a mistake and tried stripping a karat piece? If you have what does it look like, does it turn dark or keep its gold color?*
> 
> Never done this. I don’t know the answer.
> 
> *6) One more question and I will stop bothering you. About how many seconds do you allow your circuit to run. Or how many seconds does it take to strip down a heavy necklace when cell is set up right? Is it best to keep the necklaces hooked together so the current can form a loop on each piece. I can see this helping if the necklace its touching is only touching another piece in one place that has a good connection with the cathode? *
> 
> I’ve never timed the process, I just watch the process and when the current drops I will stir the pieces with a glass rod, watch the ammeter and remove the pieces when the current drops and stays low.
> 
> 
> I haven’t experimented much with this process. My main concern is not to reinvent the wheel, but to understand what is happening IN the process and then adjust my parameters to get the setup that produces the best repeatable results.
> But I did start with the basic setup first, *as should you.* That way any questions you ask can easily be answered without trying to troubleshoot the system before the process.
> 
> Tom C.
> 
> Click to expand...
Click to expand...


----------



## butcher

Oneal, I have played with the silver plate, and believe it is a fun learning experience but cost me more than any little silver I get from it, you are correct your goal should be a higher grade scrap, the electronic waste and others are fun and at the same time challenging, but unless you can get large volumes for free, it also does not seem to me to be too profitable (if you take into account money spent (paid my dues to Ebay learning)(chemicals are not that cheap) time involved and dealing with waste).

I do like to mess with low value scrap it keeps my hobby busy, and I try and not let this hobby cost me too much, which when dealing and buying low grade scrap it can easily cost me money and put me in the red, and I like the challenge, but the higher grade scrap is my goal also, I live out in the country, so garage sales I have not been able to do,(have you seen how Kadrivers wife is a master at these?), so I take any spare dime I have and go to my local gold buyer (coin dealer), he is a very honest man, and sells me karat gold and sterling for melt value, now this if I refined and sold the same day I would loose money, but if refined and sold when gold price was higher I will make money, or if our dollar goes down to pennies in value the gold will feed my family.

Also trying to get my skills up to maybe get some jewelers low grade materials, a couple of jewelers I have talked to, do not deal with their sweeps and do not even think about things like rugs and sink traps, but even here I will have to gain trust to get the business, even if they just toss this dust now, if I could prove my skills maybe then I could gain their confidence and get a chance to see if I could do better for them than their present refiner, also talked to the dentist's man who casts dental teeth of these valuable metals they send out the scrap to get it refined and have not much clue as to if they are getting all they could from their scrap, they probably just let the janitor sweep their valuable dust into the trash also (the patient has already paid them for these metals), but first I need some more practice, be able to provide them a profit on their scrap, gain their trust in dealing with me, and get a better place fixed up to refine, (better than this table under the oak tree with a tarp in the rain and snow, that reminds me I need to get my tarp put back up if this rain will slow down), I do not want a big refining business, but just a working hobby that pay's for itself, where I can learn about refining, and maybe get a few chunks of pretty metal for those rainy day's.


----------



## Oneal58

Hi anyone that can help. I am still trying to find my way around on the site. I didn't know if it was best to start a new thread or subject or just post on Butcher's reply to me. Maybe Butcher can tell me what I need to know about the site. 
My question is this, I had a lengthy instructional class given to me by kadriver day before yesterday. I wasn't prepared for that and I didn't take notes. Kadriver and I think a lot alike and I am starting right where he started. We both have similar interest and will be doing similar refinning work with similar materials. He was telling me that the forum took him all the way through the process of getting his scrap gold filled/karat/silver jewelry refined by the members on the site. 
I have been trying to go back and follow all the post that kadriver made with all the responses/questions answered by members on the forum. If I had a way of following him day by day (in the order) of the post I would not have to ask (as many questions) I still haven't found the answers to. I can do a search on kadriver but on each page, which there are 21 pages plus all the replies. When I start trying to follow kadriver and all the forums members answers to his questions, I get lost. I mean I end up not being able to follow him/members on a day by day basis without getting side tracked and lost each time. I have tried this numerous times with the same end result each time? If you understand what I am trying to do, can anyone tell me how the best way to go about it? With doing the search on kadriver I find where he first started asking questions here on the forum. But when I click on the questions I go to another page and I click on an answer there I go to another page and so on. Then I try to navigate my way back to the original page each time I follow a thread all the way through. This is very time consuming and confusing. Is there a way of getting the questions of kadriver and the answers by the forum members in order by date so I don't get lost each time.
Also on LazerSteve's site I can't seem to get my computer to open the videos there. I have broad band and a fairly fast computer running(Windows Vista, Home Premium with Service Pack 2 upgrade) but I get error messages when trying to look at his videos. Has anyone experienced similar problems with the videos there on the site? 
Thanks to anyone who can help,
Oneal58


----------



## kadriver

Oneal58:

I experienced a similar problem while trying to view lazersteve's videos.

When I tried to watch a video, I would get some kind of error.

After several tries, I finally noticed that there was a yellow message bar appearing near the top of the screen each time I clicked on one of the videos I wanted to watch.

It just kind of pops up, and it is easy to miss it.

Once I noticed this yellow bar, I clicked on it and found some instructions that allowed me to run the videos on his site.

next time you try the videos, carefully look near the top of your screen for this yellow bar that appears after you select one of his videos. Click on it and follow the instructions.

I can't remember what it said, and since I have already clicked on the "allow" function in that yellow bar, I can't get it to repeat.

In other words, once enable, the yellow bar no longer appears, It just goes straight to the videos.

Also, you must click on the start button for each video after you select it. The videos do not start automatically after you click on them.

I am going by memory here so i may have left something out.

I have a great memory - it's just short!

Hope this is helpful to you.

kadriver (Kevin)


----------



## butcher

Oneal, 
As far as trying to find and read all of Kadriver’s posts, and following them by date, here is what you might try:
Find one of his posts, click on profile at bottom of his post.
In profile click search users posts,(these should be in order of date) this will bring up his posts (17 pages like this:

http://goldrefiningforum.com/phpBB3/search.php?st=0&sk=t&sd=d&sr=posts&author_id=14587&start=320

Now maybe make notes of the section (he made the posts like help needed section) also the heading (like melting karat gold) and the date, 

You may find a pattern here? Many of these posts may be in same sections.

Now go to forum and board index, go down to the heading like help needed, finding the title subject and read that one, the dates should be in order in the sections

Sorry I am not good on computers maybe some else will know a better way.

edit: changed the word karate to karat


----------



## slickdogg

Oneal58 what web browser are you using to try and view the videos? i had same problem when using internet explorer.... i switched to firefox web browser and all videos play fine now.

Rickey


----------



## Oneal58

Hi kadriver, Love that, Great Memory-Just Short. First time I have ever heard it put that way but it fits perfectly  Thanks for the advice, I will go try that now. 
Kadriver, I have been running the sulphuric cell for several days now. My electrolyte is as black as the ace of spades. I decided to decant the sulphuric. I have been letting the electrolyte settle out. It has been settling now for approx. 35 hours. I expected the electrolyte solution to settle and at least become clearer than it was when I stopped stripping the goldplated material. To my surprise the electrolyte is just as black as it was when I started letting it settle 35 hours ago :?: I am puzzled by this because everything I have read so far says that it should clear up somewhat when the gold settles. 
What am I doing wrong or what has happened to the electrolyte to cause this? Thanks kadriver for your help. 
Oneal58



kadriver said:


> Oneal58:
> 
> I experienced a similar problem while trying to view lazersteve's videos.
> 
> When I tried to watch a video, I would get some kind of error.
> 
> After several tries, I finally noticed that there was a yellow message bar appearing near the top of the screen each time I clicked on one of the videos I wanted to watch.
> 
> It just kind of pops up, and it is easy to miss it.
> 
> Once I noticed this yellow bar, I clicked on it and found some instructions that allowed me to run the videos on his site.
> 
> next time you try the videos, carefully look near the top of your screen for this yellow bar that appears after you select one of his videos. Click on it and follow the instructions.
> 
> I can't remember what it said, and since I have already clicked on the "allow" function in that yellow bar, I can't get it to repeat.
> 
> In other words, once enable, the yellow bar no longer appears, It just goes straight to the videos.
> 
> Also, you must click on the start button for each video after you select it. The videos do not start automatically after you click on them.
> 
> I am going by memory here so i may have left something out.
> 
> I have a great memory - it's just short!
> 
> Hope this is helpful to you.
> 
> kadriver (Kevin)


----------



## Oneal58

Hi Rickey, I tried that also. I switched to Firefox, downloaded it and put it to work but am still experiencing a different, but similar problem? I can get 1 or 2 videos to download now but that's it? Out of all the videos, I can get only 2 to play? That part of it is truely baffling? Thanks Rickey for your help. 
Oneal58



slickdogg said:


> Oneal58 what web browser are you using to try and view the videos? i had same problem when using internet explorer.... i switched to firefox web browser and all videos play fine now.
> 
> Rickey


----------



## Oneal58

Hi Butcher, hope you are doing well today. I will try that Butcher, thanks. Oneal58



butcher said:


> Oneal,
> As far as trying to find and read all of Kadriver’s posts, and following them by date, here is what you might try:
> Find one of his posts, click on profile at bottom of his post.
> In profile click search users posts,(these should be in order of date) this will bring up his posts (17 pages like this:
> 
> http://goldrefiningforum.com/phpBB3/search.php?st=0&sk=t&sd=d&sr=posts&author_id=14587&start=320
> 
> Now maybe make notes of the section (he made the posts like help needed section) also the heading (like melting karate gold) and the date,
> 
> You may find a pattern here? Many of these posts may be in same sections.
> 
> Now go to forum and board index, go down to the heading like help needed, finding the title subject and read that one, the dates should be in order in the sections
> 
> Sorry I am not good on computers maybe some else will know a better way.


----------



## philddreamer

Hi Oneal!

The sulphuric acid is thick, so it'll take a couple of days for the fine gold particles to settle. When I don't want to wait that long, I filter the acid thru a funnel & a fiber glass "plug". It will take several plugs. After I'm done filtering, I rinse the plugs, & run them thru HCL/Cl thus recovering the gold
in them. 

Phil


----------



## Oneal58

Hi Phil, 
Are we talking Pink Panther Type Fiberglass here or other? Do you pack the narrow stem of the funnel with fiberglass or just put the fiberglass in the top of the funnel? If you pack the stem of the funnel, what is the length & diameter of the funnel stem you use or does it matter? I see now "plug" which would mean the stem of the funnel, right? One more quick question Phil, what % mixture and strength of the HCL/CL do you use. I am still working on trying to get the information off the videos at Lazersteve's site but am still unsuccessful with it. I think it's got something to do with the way I have my Media Player Program set up. I will keep trying but it takes time. Thank you Phil for any help. 
Oneal58



philddreamer said:


> Hi Oneal!
> 
> The sulphuric acid is thick, so it'll take a couple of days for the fine gold particles to settle. When I don't want to wait that long, I filter the acid thru a funnel & a fiber glass "plug". It will take several plugs. After I'm done filtering, I rinse the plugs, & run them thru HCL/Cl thus recovering the gold
> in them.
> 
> Phil


----------



## philddreamer

Some other members in the forum like using a "Charmin plug" also known as toilet paper, but the sulphuric will eat it up & makes a mess. I don't like using the charmin; use & re-use the fiber glass, & when it gets clogged, I use a bit of HCl/Cl & it dissolves the gold sediment & the plug is clean.

So, yes, the pink or yellow or white, as long as it's fiber glass. I also found that kaowool will work, but its expensive. (I had some left over from when I installed my woodstove.) Yes, you pack the stem of the funnel. 
I use 4:1 HCl/Cl, I add the clorox in small increments until all the dark sediment is dissolved. 

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=39&t=7034&p=65081&hilit=fiber+glass+filters#p65836

Phil


----------



## kadriver

Oneal58:

I recall having to allow the acid in my stripping cell to settle for several days like Phil pointed out.

Eventually you could see through the acid and the black material had collected on the bottom of the cell.

The acid was not crystal clear, it was still dark, but transparent.

I have saved a bunch of gold plated jewelry that has been accumulating. I may have to get the sufuric acid stripping cell set up and get it running again.

I think December 2010 was the last time that I ran it.

Back then I was too green and anxious to have to wait for the black gold powder to build up in the cell - let alone the idea of having to wait for it to settle.

Since I have gained a little more experience, hopefully I have gained some patience.

thanks - kadriver


----------



## qst42know

Oneil58

If you want to see all of a members posts. Use the "advanced search" from the top of the page, insert the name in the author box and you will get a full list of each post.

http://goldrefiningforum.com/phpBB3/search.php?keywords=&terms=all&author=kadriver+&sv=0&sc=1&sf=all&sr=posts&sk=t&sd=d&st=0&ch=300&t=0&submit=Search


----------



## Oneal58

Hi qst42know, 
Thanks, I will try that now. Thanks, Oneal58



qst42know said:


> Oneil58
> 
> If you want to see all of a members posts. Use the "advanced search" from the top of the page, insert the name in the author box and you will get a full list of each post.
> 
> http://goldrefiningforum.com/phpBB3/search.php?keywords=&terms=all&author=kadriver+&sv=0&sc=1&sf=all&sr=posts&sk=t&sd=d&st=0&ch=300&t=0&submit=Search


----------



## Harold_V

qst42know said:


> Oneil58
> 
> If you want to see all of a members posts. Use the "advanced search" from the top of the page, insert the name in the author box and you will get a full list of each post.
> 
> http://goldrefiningforum.com/phpBB3/search.php?keywords=&terms=all&author=kadriver+&sv=0&sc=1&sf=all&sr=posts&sk=t&sd=d&st=0&ch=300&t=0&submit=Search


Alternately, click on the individual's Profile button, bottom left of the screen. That takes you to his private page, where you can then click on a button to see all of his posts. 

Harold


----------



## Oneal58

Hi Harold
That worked for me, thanks a million. Harold I ran the sulphuric cell for several days/nights. I decided to decant and I have been letting the sulphuric cell settle out the gold bearing black powder. The Cell has been really slow to settle. I don't know if this is a good sign or a bad sign? From what I can gather from others, 48 hours should have been long enough for the gold powder to settle and the electrolyte should be showing signs of clearing? I have ran about 2.5 lbs. of gold plated through and found a few pieces of karat gold that got by me, I started stripping them before I realized the pieces were karat gold. My amps on the rectifier would never pull back and the fizzing would not stop and I realized the pieces were karat gold. 
So, I guess my question is if the electrolyte is heavy laden with gold powder is this the reason the cell has not settled in 4 days? Which would be a pleasant surprise! Or could there be another reason for the electrolyte not to clear up. Such as cell getting too hot, darkening the acid like you get when you overheat oil, or is that even possible? Contamination from a piece of gold plated plastic jewelry that got by me or other? I have checked the cell this morning and it's still black? Unless there has been earthquakes while I was sleeping the cell has not been moved in nearly 4 days. There should be signs of the electrolyte clearing but there isn't? I really cannot tell any difference in the acid solution now compared to when I quit stripping. I am going to decant tomorrow no matter what. I have been told by another member to use glass fiber insulation packed into a glass funnel to filter. I guess that will be the way I go. 
I am moving on to the gold filled jewelry with the instructions you gave me next week. Thanks Harold, 
Oneal58



Harold_V said:


> qst42know said:
> 
> 
> 
> Oneil58
> 
> If you want to see all of a members posts. Use the "advanced search" from the top of the page, insert the name in the author box and you will get a full list of each post.
> 
> http://goldrefiningforum.com/phpBB3/search.php?keywords=&terms=all&author=kadriver+&sv=0&sc=1&sf=all&sr=posts&sk=t&sd=d&st=0&ch=300&t=0&submit=Search
> 
> 
> 
> Alternately, click on the individual's Profile button, bottom left of the screen. That takes you to his private page, where you can then click on a button to see all of his posts.
> 
> Harold
Click to expand...


----------



## Oneal58

Hi kadriver, just wanted to say high. Hope you are doing well. My cell still hasn't settled kadriver, nearly 4 days. I don't know what is going on? I have asked Harold about this and am waiting on his reply. I could have got the cell too hot kadriver or contaminated it with gold plated plastic jewelry. 
Kadriver, did you use the HCL/CL process to recover your gold out of your cell? You and I never got into the sulphuric cell process the other day. I think I have the process in my head and notes from what I have been able to piece together here and there. But, I just want to be sure and not make any mistakes. Do you mind me asking what process you used and what to look out for? I am still having trouble with LazerSteve's Site with the videos. I have read your post where you looked at the videos and followed them step by step. I am able now, with Harold's help to follow through your post and replies from members in order. Just like you when you were learning, I will be following you step by step. I love the way you put your steps in order and numbered them. Step by step, this helps someone like me more than you will ever know kadriver. But either I have not gotten to the place you ran your cell or my search has left the sulphuric cell out for some reason? I have someone more up on computers than I that's going to take a look at my computer tomorrow. Hopefully I will be able to watch the videos, from everything I have heard from the forum they helped tremendously. Thanks kadriver,
Thanks, Oneal58



kadriver said:


> Oneal58:
> 
> I recall having to allow the acid in my stripping cell to settle for several days like Phil pointed out.
> 
> Eventually you could see through the acid and the black material had collected on the bottom of the cell.
> 
> The acid was not crystal clear, it was still dark, but transparent.
> 
> I have saved a bunch of gold plated jewelry that has been accumulating. I may have to get the sufuric acid stripping cell set up and get it running again.
> 
> I think December 2010 was the last time that I ran it.
> 
> Back then I was too green and anxious to have to wait for the black gold powder to build up in the cell - let alone the idea of having to wait for it to settle.
> 
> Since I have gained a little more experience, hopefully I have gained some patience.
> 
> thanks - kadriver


----------



## qst42know

Your acid may never be transparent clear again more like coffee colored, at least not while still concentrated. I have encountered quite a bit of gold filled on silver both marked and not marked. This may be why your acid is still dark, and that would explain why your pieces kept fizzing.

Have you been to the bottom to see what has settled? The color of the acid is less important than what has dropped, at least for now. As long as it hasn't absorbed too much water from the air it can be used again.


----------



## Oneal58

Hi qst42know, thank you. 
I have taken a little look at the bottom of the casserole and there is powder there. That is why I decided to decant. I have went to extra pains keeping the water out of the sulphuric. I forgot one night and left the cover off the cell and had an open window near by, but it did not rain that night and the humidity was low, thank goodness. (Question-1) Is there a way to tell if the electrolyte has absorbed water into it? I dried off even the alligator clips before re-inserting them back over the solution and would only let the very tip of the clip touch the sulphuric. I was using a basket I made out of #10 bare copper wire but found out I was not getting the reaction I thought I was getting at first. I would get good amperage flow at first and then the amps would drop back to around .5 amps and the fizzing would stop. The amperage would stay at .5 amps, so I assumed the deplating was complete and the .5 amps was because of the resistance of my hand made basket in the circuit. When I started taking a closer look at the items I had stripped, I could still see gold under the oxidized black coating. When I would hook the pieces up individually I would get good amperage flow again and more fizzing. Of course not as much as before but enough to let me know that gold was still there, I was leaving some gold on the pieces. So I changed my setup and went to hooking each piece up individually and then making up some pigtails, (jumpers) so I could run more pieces at one time. I went back through all the pieces I had previously stripped. That kept me busy changing out pieces but I would rather do that right now than just sit there and wait. Also, I have confidence that I am getting all the gold plate off. 
I got one more question if you don't mind. (Question-2) When you say that you had ran into goldplated silver? I have ran into the same thing. So, if I left the gold on silver in the cell after the gold was gone this will cause the the electrolyte to be really black also? So, I will have some silver in the electrolyte solution in amounts I wasn't expecting?
Thank you qst42know for your responses, thank goodness for this site! I can't say this often enough, I don't know what I would have done if I hadn't of found this site with all the willing members to guide me!
Oneal58




qst42know said:


> Your acid may never be transparent clear again more like coffee colored, at least not while still concentrated. I have encountered quite a bit of gold filled on silver both marked and not marked. This may be why your acid is still dark, and that would explain why your pieces kept fizzing.
> Have you been to the bottom to see what has settled? The color of the acid is less important than what has dropped, at least for now. As long as it hasn't absorbed too much water from the air it can be used again.


----------



## philddreamer

"(Question-1) Is there a way to tell if the electrolyte has absorbed water into it?"
I only left it incovered for a few days in the garage when I first started learning the process last year, & noticed the level of the liquid went up. Since, I've been covering the container & I've made the habit of putting a mark, that way I know how much acid I begin with in the container. 
If I notice the volume goes up, well its time to heat & evaporate some of the water. I do this after I have recovered the values & filtered. 

Take care!

Phil


----------



## qst42know

1. I am certain there is a way to tell if the electrolyte has absorbed to much water but I'm not familiar with the method. Perhaps someone who is, will chime in.

2. The cell will strip silver plate or attack solid silver and the solution does go black and may change the conductivity of the electrolyte. But no one can agree on a method to get the silver out. 

Dilute by slowly pouring the acid into 3 volumes of water. Be careful and slow this will get hot. Some material should settle and this should be the last of the gold. The dilute acid can be recycled by evaporating but this is very dangerous and may not be cost effective if you don't pay much for new acid.

There are a couple of methods that may work to recover the silver when the acid won't function any more. *I have not fully investigated these methods so keep that in mind.*

And now the questionable, at best experimental steps you may want to skip altogether.

A. Cement the dilute acid with iron, iron should push the silver out of solution along with other base metals. I recall from the memory of a very old text (early 1800s I think) this was used by the Philadelphia mint for recovering silver from Dore gold. 

B. From memory another member a very long time ago reported that adding HCL to the dilute acid produced silver chloride that then settled to the bottom. I have tried this very small scale and it seemed to work, but produced the strong odor of chlorine gas, very dangerous stuff.

[spelling edit]


----------



## butcher

Hoke I believe talked about getting the silver out of concentrated sulfuric acid, by pouring the acid into volumes of water to make it real dilute, (never pour water into acid), then adding table salt to form silver chloride. 
(this was in C.M. Hoke in alternative method of using concentrated sulfuric acid rather than nitric acid to part the gold and silver (karat gold), if my memory is not failing).

So from what she says, and what we know: 
(Two moles) table salt (NaCl) and sulfuric acid (H2SO4) together form --> hydrochloric acid (two moles) (HCl) and sodium sulfate (Na2SO4).

2NaCl + H2SO4 --> 2HCl + Na2SO4

Silver chloride would form, and precipitate, my only concern would be keeping the sodium sulfate soluble (dilution may solve that?).

Note above this would no longer be sulfuric acid and could not be reused in your cell, and I also do not know about the chlorine gas fumes qst42know has mentioned.

A downside is not being able to reuse the H2SO4 as sulfuric acid.

I am still under the opinion (no proof) that the concentrated H2SO4 could only hold so much silver (or any other metal), before it was loaded (saturated) and any more dissolved (through electrolysis) would precipitate as sludge, who knows.


----------



## qst42know

> I am still under the opinion (no proof) that the concentrated H2SO4 could only hold so much silver (or any other metal), before it was loaded (saturated) and any more dissolved (through electrolysis) would precipitate as sludge, who knows.



My small experiments on silver plate indicate the solution becomes less and less effective at stripping, to the point of stopping altogether. There may have been some on the bottom at that point but I don't recall, and the acid was quite dark. Any silver plated iron introduced to the mix somehow prevented the stripping action as well.


----------



## Oneal58

Hi Phil, thank you for your answers. I too watch the level of the cell. I am losing some quantity each time I strip. I have lost approx 10-15% of the quantity I started with. I think a lot of this is due to me dragging the pieces out of the solution that is wet with acid and I am losing acid in this manner each time. Plus my electrolyte gets quiet warm sometimes and I think I am losing some acid through evaporation. Thanks Phil, 
Oneal58



philddreamer said:


> "(Question-1) Is there a way to tell if the electrolyte has absorbed water into it?"
> I only left it incovered for a few days in the garage when I first started learning the process last year, & noticed the level of the liquid went up. Since, I've been covering the container & I've made the habit of putting a mark, that way I know how much acid I begin with in the container.
> If I notice the volume goes up, well its time to heat & evaporate some of the water. I do this after I have recovered the values & filtered.
> 
> Take care!
> 
> Phil


----------



## butcher

Hot concentrated sulfuric will dissolve silver.

Silver plate can be de-plated as anode in a cell with heated concentrated sulfuric acid.

Silver as an anode will lose electrons (oxidation basically dissolves into solution) in dilute room temperature sulfuric solution.

I do not see why silver would not dissolve as anode in the concentrated sulfuric cell at room temperature (I am puzzled here), although I see where it would be held in acid as silver ions if it was oxidized by the electicity.
It seems to me that heat would be the only difference, normally heat just speeds the reaction that may take a long period of time to accomplish (still puzzled).


----------



## Oneal58

Hi Butcher, this question on the sliver came up when I was stripping the gold plated material I have. I found that a few of the pieces was gold plated over sterling silver. Someone mentioned that the silver will effect the process of the sulphuric cell by turning it black and the electrolyte not wanting to settle, which I am experiencing. I sure hope not, I am not after the silver, I am after the gold powder on the bottom of the dish. To recover this gold, (I hope) powder, with very little silver I hope, I would decant filter a couple of times. Then treat with HCL/Cl. To get the gold in suspension then drop the gold. Now if there is a lot of sliver in there, more than anticipated is that going to cause me trouble in trying to recover (droping) the gold? Just focus on the gold and participate the silver out after dropping the gold? NOTE!, there were only maybe 4 pieces that was sterling under goldplated and I stopped the reaction when the gold was stripped and I seen the piece was still fizzing. I Kept looking at the items that I was deplating. When they turned silver and didn't stop fizzing I would take them out immediately and test them to verify they were sterling. So, I am sure this isn't the first time someone has ran into this problem. I am just trying to find a solution before I have a problem with the silver being in the Sulphuric Solution if in fact some did get in there? Just add the HCL/CL drop the gold and save the solution to recover the silver out of when I have enough to mess with. Or drop the gold, then run the gold through a AR process. Butcher, I am tired and everything is running together tonight. I got to call it quits for today. Thank you Butcher for your help, as always. A good nights sleep will make every thing clearer tomorrow. I hope this post makes sense tomorrow. Thanks Butcher, Oneal58



butcher said:


> Hot concentrated sulfuric will dissolve silver.
> 
> Silver plate can be de-plated as anode in a cell with heated concentrated sulfuric acid.
> 
> Silver as an anode will lose electrons (oxidation basically dissolves into solution) in dilute room temperature sulfuric solution.
> 
> I do not see why silver would not dissolve as anode in the concentrated sulfuric cell at room temperature (I am puzzled here), although I see where it would be held in acid as silver ions if it was oxidized by the electicity.
> It seems to me that heat would be the only difference, normally heat just speeds the reaction that may take a long period of time to accomplish (still puzzled).


----------



## Geo

when you dissolve the powder in hcl/cl gold will stay in the solution and any silver dissolved will precipitate back out as silver chloride.after you dissolve all the powder filter through a couple coffee filters.the silver shouldnt be a problem.remember that gold and silver will not stay in the same solution except for trace amounts and i think cyanide,unsure about that though.


----------



## Oneal58

Hi Geo, thanks. When I filter a couple of times I save the filters in a seperate container to process the silver after I have accumulated enough to mess with? I have some sterling silver that I am going to refine by way of Nitric. If I wash these filters good and distill can I add this to my silver refine or will I be contaminating my silver batch? I am sure there is probably a little copper, solder, maybe some nickel and tin that will be in there. What to do with it? Thanks, Oneal



Geo said:


> when you dissolve the powder in hcl/cl gold will stay in the solution and any silver dissolved will precipitate back out as silver chloride.after you dissolve all the powder filter through a couple coffee filters.the silver shouldnt be a problem.remember that gold and silver will not stay in the same solution except for trace amounts and i think cyanide,unsure about that though.


----------



## Geo

actually the base metals isnt the problem with adding this to your sterling, its the fact that silver chloride isnt elemental silver (silver metal) it needs to be reduced to obtain the silver metal.check out lazersteves videos on his website concerning silver chloride to begin with at www.goldrecovery.us follow the login instructions and watch the free videos.after you have reduced the AgCl to elemental form you can add that to your sterling if you want to but if done properly it should be pure enough for a silver cell.


----------



## Oneal58

Hi everyone, 
Well, I decanted today out of the gold stripping sulphuric cell I had been stripping into for 5 days with about that same amount of settling. I could not find any fiberglass so I used toilet tissue to plug the glass funnel. I had been warned by Phil not to do this. 
I plugged the filter funnel and started pouring. The filter filled up quickly and I stoped. Eventually I saw that it was starting to filter and then all the contents in the filter broke through the toilet paper as I had been warned by phil. Then the toilet paper followed the black sulphuric down into the beaker. I put another plug in and tried again. Thinking I did not pack the toilet paper tight enough. The same thing happened again. Talk about hard headed, but I was determined to see the bottom of that cell. So I continued to pour untill I could see that I did have powder in the bottom of the bowl. I tried to pour off as much sulphuric as I could and then the powdered mud slipped and fell into the funnel and went into the cell. Out of a knee jerk reflex I made the situation even worse. Most of the black powder went into the filter and down into the 1000ml beaker. 
Now I have stirred up everything again and now I have toilet paper mixed in with the sulphuric. 
I looked at the cell, very little black powder was left. I took a deep breath and washed the rest into the beaker. So now I am right back where I started and have toilet paper in the mix. 

Question-1- I did not put Glycerine into the sulphuric, I finally got my computer to show Lazersteve's videos and seen he put glycerine in his sulphuric. Was this the mistake I made and can it be corrected?
Question-2-If I do not plan to revisit the stripping cell again is there a way I can recover the gold out of the sulphuric without worring about saving the sulhuric? Thus saving time, or just wait again.
Question-3- Can I carefully dilute the sulphuric with water so the gold will settle quicker by changing the viscosity? 
Question-4-What am I going to do about two funnels full of toilet paper in my electrolyte? 

Thanks to anyone for their help. I feel beaten tonight but I still have my eyes on the prize.
Depressed but not beaten. 
Thanks, Oneal58


----------



## nickvc

1 you don't need the glycerine in the cell it serves no purpose.
2 And 3 yes you can dilute the sulphuric BUT you must add the sulphuric to water not the other way round, the dilute solution can be used to remove lead from later processing.
4 When you have recovered your powders and toilet paper dry and then incinerate before further treatments.


----------



## Oz

If you used concentrated sulfuric acid the toilet paper will be magically gone in the morning. Concentrated sulfuric will digest organics, this is why Phil told you not to use it.


----------



## Geo

(1).glycerin is not needed.the video is 7 years old and steve hasn't updated it.

(2).leave everything in the beaker undisturbed for a few days.the liquid will become transparent,not clear but you can see light through it.decant slowly or syphon down close to the powder and stop.

(3).you can carefully dilute the sulfuric with 1 part sulfuric to 3 parts tap water.remember,"first the water and then the acid,otherwise it wont be placid".this will speed it up a fraction but unnecessary.

(4).after you have given it a few days the fibers of the toilet paper will be no more.sulfuric acid reacts to organics in a very aggressive manner.thats why it is so dangerous to you and me.


----------



## kadriver

Oneal58:

Hello, I was trying to think back when I did my sulfuric acid cell clean out.

I bought a package of fiberglass body filler material from advance auto and used it to try to filter the gold powder from the sulfuric acid in the deplating cell.

I packed it into a buchner type funnel (big mistake) and poured the electrolyte in.

The experiment failed miserably, all the gold and acid went right on through with no filtering effect at all.

Defeated, I took a 2 liter pyrex beaker and filled it with 1000 ml distilled water (tap water would have probably worked).

Then I carefully poured the concentrated sulfuric acid electrolyte from the failed filtering experiment into the 2 liter beaker half full of distilled water - being careful not to over-heat.

I even used a plastic kitchen spatula to scrape all the black from the bottom of the cell into the 2 liter beaker half full of distilled water.

Once most of the acid was removed from the cell with the spatula, I actually was able to rinse it with distilled water into the 2 liter beaker.

There was some heat generated but I can't remember how much. I would not use a non-heat risistant glass container for doing this.

I vaguely recall using a second 1000 ml beaker half full of distilled water because I ran out of capacity with the first 2000 ml beaker.

Once I had the acid diluted, I allowed it to settle.

Once settled, I poured off the clear liquid from both beakers, ensuring none of the black power escaped during the pour.

Then I refilled each with distilled water and settled again. I repeated this several times

I think I kept rinsing until I could not smell the sulfuric acid in the black powder any longer.

I remeber thinking that this was too much time & effort for such a small amount of gold. This is probably why I have not used the cell since then. 

Once I had the black powder as clean as I could get it, I made some aqua regia and dissloved the black powder, added a few drops of sulfuric to precipitate any lead, filtered as usual and dropped the gold.

I think I got about 2 grams of gold after using the cell for about 20 hours. It was not a very pretty piece as there was still some contamination that was left in the black powder. Today I would use more care in processing the black powder.

As I stated before, I believed that the amount of gold retrieved was not worth the effort to me, especially since I had already produced a bar or two of fine gold from karat scrap.

But this line of thinking has now changed. I am going to get the sulfuric acid deplating cell set up again and start using it - this post has reinvigorated my desire for processing this type of scrap!

Also - Oneal58, you said you had some copperas. Where did you say that you found it? 

Hope this is helpful - kadriver


----------



## Geo

Kadriver

you can make your own copperas by digesting some soft steel in warm-hot sulfuric acid.i guess theres no need to tell you to be careful but, be careful when working with hot sulhuric acid. your copperas will be as pure as the material that you started with.make sure the steel is clean with no other metal on it and make sure to use new diluted sulfuric acid(new battery acid should work ok,do not concentrate).if you start with 400 ml of acid digest all the steel that the acid will hold.then evaporate the acid down and when you reach a quarter of the volume you started will bright blue crystals will start forming,this will be your copperas.continue evaporating till the solution is nearly dry, then remove from the heat and allow to cool.removed whats left of the solution and rinse your crystals in cold water through a few rinses and filter.allow the crystals to dry and store in new concentrated sulfuric acid (just enough to keep the crystals wet).


----------



## Oneal58

Thank Geo, I appreciate your post. I will get there yet. Will post a picture of my returns. Thank you for answering my post. 
Oneal58



Geo said:


> (1).glycerin is not needed.the video is 7 years old and steve hasn't updated it.
> 
> (2).leave everything in the beaker undisturbed for a few days.the liquid will become transparent,not clear but you can see light through it.decant slowly or syphon down close to the powder and stop.
> 
> (3).you can carefully dilute the sulfuric with 1 part sulfuric to 3 parts tap water.remember,"first the water and then the acid,otherwise it wont be placid".this will speed it up a fraction but unnecessary.
> 
> (4).after you have given it a few days the fibers of the toilet paper will be no more.sulfuric acid reacts to organics in a very aggressive manner.thats why it is so dangerous to you and me.


----------



## Oneal58

Thanks Oz, that's good news. Thank you for posting. 
Oneal58


Oz said:


> If you used concentrated sulfuric acid the toilet paper will be magically gone in the morning. Concentrated sulfuric will digest organics, this is why Phil told you not to use it.


----------



## Oneal58

Thank you nickvc for your post. I appreciate your help. It's good to find out that the toilet paper problem will just be a bad dream. Appreciate your help. 
Oneal58



nickvc said:


> 1 you don't need the glycerine in the cell it serves no purpose.
> 2 And 3 yes you can dilute the sulphuric BUT you must add the sulphuric to water not the other way round, the dilute solution can be used to remove lead from later processing.
> 4 When you have recovered your powders and toilet paper dry and then incinerate before further treatments.


----------



## Oneal58

Thanks Kadriver, when you asked where I found the copperas at in your earlier post I thought you may need or want some. I didn't see this later post. But if you want any just let me know. If I find the copperas are old when I open the bag, I will use this method below you gave me. I am starting on the gold filled items today. I am going to dilute my electrolyte from the cell first and let it be settling. I am going to use Harolds instructions he gave me. Use diluted Nitric to seperate the foils of gold off the gold filled items. 
1-Kadriver when he says diluted will it be 50/50 Nitric/Water with the strength of the Nitric I got from you? 
2-Kadriver you also mentioned in an old post you found Stump Out at HD. That the Stump Out was Metabisulfite, did I read that wrong? I went to HD the other day and the product they had called (stump out) had Potassium Nitrate in it?
Thanks Kadriver,
Oneal58



Geo said:


> Kadriver
> 
> you can make your own copperas by digesting some soft steel in warm-hot sulfuric acid.i guess theres no need to tell you to be careful but, be careful when working with hot sulhuric acid. your copperas will be as pure as the material that you started with.make sure the steel is clean with no other metal on it and make sure to use new diluted sulfuric acid(new battery acid should work ok,do not concentrate).if you start with 400 ml of acid digest all the steel that the acid will hold.then evaporate the acid down and when you reach a quarter of the volume you started will bright blue crystals will start forming,this will be your copperas.continue evaporating till the solution is nearly dry, then remove from the heat and allow to cool.removed whats left of the solution and rinse your crystals in cold water through a few rinses and filter.allow the crystals to dry and store in new concentrated sulfuric acid (just enough to keep the crystals wet).


----------



## qst42know

Oneal58 said:


> Hi qst42know,
> I did incinerate from above down onto the material. I did notice a variation in the color of the plating between the non-ferrous metals and the ferrous metals. I just assumed it had something to do with the karat of the plating? This plating could have very well been brass plating. Then on top of that I incinerated from above?



I don't want to contradict anything you have been told and I am quite a bit behind in this conversation. The point I was attempting to make is this, thin gold plate is often applied over a shiny coat of nickel and then coated in just enough gold to give it the right color, to this perhaps a dip in lacquer to make the soft gold last a while. 

Migration of gold is well known and I don't dispute the possibility that some of your missing gold disappeared in that way. 

While incinerating thinly plated material from above it is also possible that you oxidized the nickel undercoat and shed some of what little gold that was there as a dust blown away by your torch. 

In my monitor the photo of your melting dish interior has a slight pink color to it. That is why I suspect some losses due to it being blown away. 

[Is that how the dish appears in real life, pink on the inside?]

The point I was trying to make is this, heat from below, and not in a refractory melting dish may be less prone to losses than a windy torch from above.

When I incinerate even gold filled items there is always some dusty shed material that I am careful to include in the digestion.


----------



## Oneal58

Hi qst42know, yes there is a slight pink hue to the melting dish in places. I believe locked into the Borax as well. I have since started heating from below to heat the gold plated items as per your first post. I see now that with high heat directly onto the gold plated items will cause the items to lose their plating. 
Unless the gold has migrated into the metal as Harold said could be happening. Which could be very possible because I put a lot of heat to it. But I don't plan on trying to get at this gold by melting all that heavy metal in the necklaces to get the little bit of plating that could be locked within the metal. Just isn't worth the trouble/gas/acid, Etc;. I heat from the bottom now just enough to burn off the dirt, laquer, Etc;. I then stop, I got really heavy handed the first couple of burns with the torch which could also have played a part. 
Thanks qust42know,
Oneal58


qst42know said:


> Oneal58 said:
> 
> 
> 
> Hi qst42know,
> I did incinerate from above down onto the material. I did notice a variation in the color of the plating between the non-ferrous metals and the ferrous metals. I just assumed it had something to do with the karat of the plating? This plating could have very well been brass plating. Then on top of that I incinerated from above?
> 
> 
> 
> 
> I don't want to contradict anything you have been told and I am quite a bit behind in this conversation. The point I was attempting to make is this, thin gold plate is often applied over a shiny coat of nickel and then coated in just enough gold to give it the right color, to this perhaps a dip in lacquer to make the soft gold last a while.
> 
> Migration of gold is well known and I don't dispute the possibility that some of your missing gold disappeared in that way.
> 
> While incinerating thinly plated material from above it is also possible that you oxidized the nickel undercoat and shed some of what little gold that was there as a dust blown away by your torch.
> 
> In my monitor the photo of your melting dish interior has a slight pink color to it. That is why I suspect some losses due to it being blown away.
> 
> [Is that how the dish appears in real life, pink on the inside?]
> 
> The point I was trying to make is this, heat from below, and not in a refractory melting dish may be less prone to losses than a windy torch from above.
> 
> When I incinerate even gold filled items there is always some dusty shed material that I am careful to include in the digestion.
Click to expand...


----------



## butcher

Making ferrous sulfate (FeSO4), also called copperas or iron sulfate.

Copperas is green in solution or in crystal form. 

Ferrous sulfate is good to use to precipitate gold from acidic solutions.
2AuCl3 + 6FeSO4 à 2Au (s) + 2Fe2(SO4)3 +Fe2Cl4

Iron sulfate will also precipitate platinum from boiling hot solution if pH 7.

FeSo4 crystal can be used to detect dissolved gold in solutions in the spot plate,
This is useful also if the gold is in solution with another precious metal, we can use the copperas crystal to test for gold in one dish of spot plate (brown ring) this precipitates the gold and remaining solution moved to another dish in spot plate and tested for other precious metal.

Copperas crystals (green) these crystals will oxidize easily if not stored properly, dry (acid low) and exposed to air (turning brown) the brown crystals will not precipitate gold, most all copperas I have found in garden centers has oxidized and is useless for our needs here.

The green copperas crystals, when made should be kept fresh in storing, I will keep them wet, few drops of sulfuric acid to keep them acidic, store in air tight plastic container (screw on plastic lid with seal an old stump remover bottle is what I use), they have a very long shelf life this way.

It is as easy to make a large batch of ferrous sulfate, as it is to make a small batch of copperas.

You need as pure iron as you can get (not steel), soft Iron laminates from old transformers, or electric motors, is what I use.

An old transformer cut iron laminate welds (hacksaw or angle grinder Etcetera), remove copper winding an save (to rewind another transformer, old motor, use as wire, or throw in your copper scrap metal pile), separate the iron laminates, cut into small pieces (with tin snip’s), use torch to burn off shellac and oils, add this Iron to dilute sulfuric acid (10% H2SO4), (the dilute acid is best as iron can passivate (not dissolve) in strong sulfuric acid), you can dilute battery acid (one part 32% battery acid to two parts water), or dilute the drain cleaner in water.

:shock: Always add the concentrated sulfuric acid to water slowly watching the temperature rise from reaction).
Never add water to concentrated sulfuric acid it will boil out and splash all over you burning you severely or blinding you}  

The iron will dissolve slowly in cold solution, heating will speed the reaction, you can boil this solution of iron metal and dilute sulfuric acid because the sulfuric acid has such a high boiling point so gases evolved are mainly just water in fumes.
I use a Pyrex Mr. coffee pot, or white corning ware casserole dish on solid iron metal burner electric hot plate.

After as much iron as will dissolve (dissolves into the concentrating acid) lower temperature and pour this green solution into another jar, letting un-dissolved iron metal and carbon settle well.

Filter solution back into evaporating dish and boil down to crystals, when you get a few inches of crystals cool solution somewhat then pour into a clean jar let cool more and crystals settle, decant liquid back into boiling vessel and make more crystals, this concentrated solution can be used also.

For storing crystals see information above.


Oneal, you should not use flux or borax when you incenerate the materials, that and what Quest for to know has stated can be reason for loss of thin plating.


----------



## Geo

butcher said:


> Making ferrous sulfate (FeSO4), also called copperas or iron sulfate.
> 
> Copperas is green in solution or in crystal form.
> 
> Ferrous sulfate is good to use to precipitate gold from acidic solutions.
> 2AuCl3 + 6FeSO4 à 2Au (s) + 2Fe2(SO4)3 +Fe2Cl4
> 
> Iron sulfate will also precipitate platinum from boiling hot solution if pH 7.
> 
> FeSo4 crystal can be used to detect dissolved gold in solutions in the spot plate,
> This is useful also if the gold is in solution with another precious metal, we can use the copperas crystal to test for gold in one dish of spot plate (brown ring) this precipitates the gold and remaining solution moved to another dish in spot plate and tested for other precious metal.
> 
> Copperas crystals (green) these crystals will oxidize easily if not stored properly, dry (acid low) and exposed to air (turning brown) the brown crystals will not precipitate gold, most all copperas I have found in garden centers has oxidized and is useless for our needs here.
> 
> The green copperas crystals, when made should be kept fresh in storing, I will keep them wet, few drops of sulfuric acid to keep them acidic, store in air tight plastic container (screw on plastic lid with seal an old stump remover bottle is what I use), they have a very long shelf life this way.
> 
> It is as easy to make a large batch of ferrous sulfate, as it is to make a small batch of copperas.
> 
> You need as pure iron as you can get (not steel), soft Iron laminates from old transformers, or electric motors, is what I use.
> 
> An old transformer cut iron laminate welds (hacksaw or angle grinder Etcetera), remove copper winding an save (to rewind another transformer, old motor, use as wire, or throw in your copper scrap metal pile), separate the iron laminates, cut into small pieces (with tin snip’s), use torch to burn off shellac and oils, add this Iron to dilute sulfuric acid (10% H2SO4), (the dilute acid is best as iron can passivate (not dissolve) in strong sulfuric acid), you can dilute battery acid (one part 32% battery acid to two parts water), or dilute the drain cleaner in water.
> 
> :shock: Always add the concentrated sulfuric acid to water slowly watching the temperature rise from reaction).
> Never add water to concentrated sulfuric acid it will boil out and splash all over you burning you severely or blinding you}
> 
> The iron will dissolve slowly in cold solution, heating will speed the reaction, you can boil this solution of iron metal and dilute sulfuric acid because the sulfuric acid has such a high boiling point so gases evolved are mainly just water in fumes.
> I use a Pyrex Mr. coffee pot, or white corning ware casserole dish on solid iron metal burner electric hot plate.
> 
> After as much iron as will dissolve (dissolves into the concentrating acid) lower temperature and pour this green solution into another jar, letting un-dissolved iron metal and carbon settle well.
> 
> Filter solution back into evaporating dish and boil down to crystals, when you get a few inches of crystals cool solution somewhat then pour into a clean jar let cool more and crystals settle, decant liquid back into boiling vessel and make more crystals, this concentrated solution can be used also.



i dont mind being corrected and really appreciate someone taking the time to point out any errors i may make in my comments as im still learning.the laminates your referring to can not be pure iron or even close to it.pure iron is a crystal and does not bend easily without breaking such as castiron.the soft laminates from transformers is an alloy that can be searched on the web.(i did) so i wouldnt look foolish saying this but can contain as little as 85% iron with Ni or Co these can be bent double and be flexed many times before breaking,iron will not stand up to these stresses.

the crystals i spoke of look more like aqua-marine but according to wiki copperas crystals are green if pure.


----------



## Oneal58

Thanks Butcher, this information will come in good. I appreciate your answer. I have a couple of questions, again.
Following Harolds advice I put my gold filled items into a 500ml flask and covered with 150 ml of water. I poured out 150ml of Nitric into a beaker. I then slowly started adding my Nitric I got from Kadriver. I put a small amount of Nitric into the beaker and reaction started. The Nitric and water turned a green color at first. When the reaction seemed to be slowing I added approx. another 75 ml of Nitric. The reaction was liken to a volcano, it spewed for what seemed like a couple of minutes. It finally calmed down enough I could approach the flask again. The flask was very hot and venting the mustard colored gas. I left it alone for a while. I went back to it after 5 minutes or so. It had calmed down. I then added the remaining 50 ml of Nitric Acid. I back away, a good distance and watched. It did not boil over again.
Question-1- Is it better to use a beaker or a flask when doing this type work? 
Question 2- Is it better to cover the beaker or flask after adding the Nitric?
Question 3- I know Harold says to keep adding Nitric untill all base metals have been dissolved. DO I dilute the Nitric to keep it 50/50 or just keep adding concentrated Nitric to the Flask. This of course will be increasing the strength of the Nitric in the Flask. 
Question 4-What did I do wrong to get the boil over, I thought I was being careful to avoid a boil over? Is this something you have to develope a feel for?
Question 5- Can I leave everything just the way it is overnight and do I cover it?
Question 6- Can I take the Nitric inside a building and it be OK to go into that building the next moring?
Question 7- Am I missing something so far?


----------



## Oneal58

Thanks Geo,
I will put this to use, I really appreciate your response. I am printing all my replies and making a notebook of the replies for references. Thanks,
Oneal58



Geo said:


> butcher said:
> 
> 
> 
> Making ferrous sulfate (FeSO4), also called copperas or iron sulfate.
> 
> Copperas is green in solution or in crystal form.
> 
> Ferrous sulfate is good to use to precipitate gold from acidic solutions.
> 2AuCl3 + 6FeSO4 à 2Au (s) + 2Fe2(SO4)3 +Fe2Cl4
> 
> Iron sulfate will also precipitate platinum from boiling hot solution if pH 7.
> 
> FeSo4 crystal can be used to detect dissolved gold in solutions in the spot plate,
> This is useful also if the gold is in solution with another precious metal, we can use the copperas crystal to test for gold in one dish of spot plate (brown ring) this precipitates the gold and remaining solution moved to another dish in spot plate and tested for other precious metal.
> 
> Copperas crystals (green) these crystals will oxidize easily if not stored properly, dry (acid low) and exposed to air (turning brown) the brown crystals will not precipitate gold, most all copperas I have found in garden centers has oxidized and is useless for our needs here.
> 
> The green copperas crystals, when made should be kept fresh in storing, I will keep them wet, few drops of sulfuric acid to keep them acidic, store in air tight plastic container (screw on plastic lid with seal an old stump remover bottle is what I use), they have a very long shelf life this way.
> 
> It is as easy to make a large batch of ferrous sulfate, as it is to make a small batch of copperas.
> 
> You need as pure iron as you can get (not steel), soft Iron laminates from old transformers, or electric motors, is what I use.
> 
> An old transformer cut iron laminate welds (hacksaw or angle grinder Etcetera), remove copper winding an save (to rewind another transformer, old motor, use as wire, or throw in your copper scrap metal pile), separate the iron laminates, cut into small pieces (with tin snip’s), use torch to burn off shellac and oils, add this Iron to dilute sulfuric acid (10% H2SO4), (the dilute acid is best as iron can passivate (not dissolve) in strong sulfuric acid), you can dilute battery acid (one part 32% battery acid to two parts water), or dilute the drain cleaner in water.
> 
> :shock: Always add the concentrated sulfuric acid to water slowly watching the temperature rise from reaction).
> Never add water to concentrated sulfuric acid it will boil out and splash all over you burning you severely or blinding you}
> 
> The iron will dissolve slowly in cold solution, heating will speed the reaction, you can boil this solution of iron metal and dilute sulfuric acid because the sulfuric acid has such a high boiling point so gases evolved are mainly just water in fumes.
> I use a Pyrex Mr. coffee pot, or white corning ware casserole dish on solid iron metal burner electric hot plate.
> 
> After as much iron as will dissolve (dissolves into the concentrating acid) lower temperature and pour this green solution into another jar, letting un-dissolved iron metal and carbon settle well.
> 
> Filter solution back into evaporating dish and boil down to crystals, when you get a few inches of crystals cool solution somewhat then pour into a clean jar let cool more and crystals settle, decant liquid back into boiling vessel and make more crystals, this concentrated solution can be used also.
> 
> 
> 
> 
> i dont mind being corrected and really appreciate someone taking the time to point out any errors i may make in my comments as im still learning.the laminates your referring to can not be pure iron or even close to it.pure iron is a crystal and does not bend easily without breaking such as castiron.the soft laminates from transformers is an alloy that can be searched on the web.(i did) so i wouldnt look foolish saying this but can contain as little as 85% iron with Ni or Co these can be bent double and be flexed many times before breaking,iron will not stand up to these stresses.
> 
> the crystals i spoke of look more like aqua-marine but according to wiki copperas crystals are green if pure.
Click to expand...


----------



## qst42know

> I put my gold filled items into a 500ml flask and covered with 150 ml of water. I poured out 150ml of Nitric into a beaker.



In a 500ml flask, 300ml of solution pretty much guarantees a fountain. It doesn't leave much room for expansion.

A beaker or coffee pot filled no more than perhaps 1/3 full is much safer. A watch glass or other glass cover condenses some of the fumes.

Cover and leave outside. Put the whole thing inside a bucket or plastic storage container with lid if there is a chance someone or something might spill it in the night.


----------



## Oneal58

Thanks qst42know for your respones. 
Question 1- Do I dilute the nitric down to 50/50 and add to the beaker or do I just keep adding full strength to the beaker now. I have since changed over to a large 1800ml beaker. But do I gradually keep increasing the strength of the Nitric in the beaker if I still have base metals that are not dissolved. Or just keep adding the 50/50 nitric? Thanks, 
Oneal


----------



## qst42know

> i dont mind being corrected and really appreciate someone taking the time to point out any errors i may make in my comments as im still learning.the laminates your referring to can not be pure iron or even close to it.pure iron is a crystal and does not bend easily without breaking such as castiron.the soft laminates from transformers is an alloy that can be searched on the web.(i did) so i wouldnt look foolish saying this but can contain as little as 85% iron with Ni or Co these can be bent double and be flexed many times before breaking,iron will not stand up to these stresses.




Geo

I did look these alloys up, and some discussions on their use. I see they are many times more expensive and used for more critical applications than the low alloy 1020 steel which would be common in small transformers and fractional HP motors.

I was previously unaware of these special alloys. Thanks for finding this it could have been a mysterious contamination in a gold precipitation.


----------



## qst42know

Oneal58 said:


> Thanks qst42know for your respones.
> Question 1- Do I dilute the nitric down to 50/50 and add to the beaker or do I just keep adding full strength to the beaker now. I have since changed over to a large 1800ml beaker. But do I gradually keep increasing the strength of the Nitric in the beaker if I still have base metals that are not dissolved. Or just keep adding the 50/50 nitric? Thanks,
> Oneal



I have only used poormans nitric which is 50%.

Anyone else?


----------



## butcher

Geo,
I am also still learning, 
And as you, I also want to be corrected or shown the best way to do this if there are better ways, I would also like to learn as much as possible about the Iron alloy's and their use.
As far as I know the laminates is fairly pure iron,

I have not seen where cobalt or nickel was used in this type of laminates in transformers; there are many different types of metals used in electro magnetic core metals(electical metals), used in electronics and electrical industry, and may be many different types used for this or other purpose depending on the magnetic reaction needed in their use.

I have heard of small amounts of silicon and other metals in laminate, but this has not given me any problems in the copperas that I know of. 

The ferrous sulfate from your garden supply I would say has more metal contaminates, but if green will work well for use.

Most all iron or steel will have contaminates.

I have not seen where cobalt or nickel was used in this type of laminates; I would like to see the composition (the document you spoke of reading), just out of curiosity.

The transformer laminates are the best Iron I have found to make ferrous sulfate with, I thought they were fairly high purity soft easy to work with thin and makes great ferrous sulfate. (Without using my blacksmithing stockpile).

Real iron is hard to come by since we do not use blacksmith shops any more, I do have some railroad iron or horseshoe iron that may be fairly close.

Iron can be very soft and flexible, or made to be hard brittle and crystallized and break like glass. This is usually done with heat treatment or can also be from other materials like carbon, silica and so on in the metal or added to it. 
Cast Iron I thought has much more contaminates, I do not know if these would affect the copperas if it were made from cast Iron, I do not think they would but I do not know.

http://www.aksteel.com/pdf/markets_products/electrical/Mag_Cores_Data_Bulletin.pdf

http://en.wikipedia.org/wiki/Cast_iron

I also make ferrous sulfate using sodium bisulfate (the byproduct white crystal salts saved from making nitric acid) the sodium bisulfate act very similar to the dilute sulfuric acid in water with heat.


----------



## Geo

this is a company that makes laminates with special alloys.my point being unless you have the specs for each individual transformer or motor stator your playing Russian roulette with your processes. www.magmet.com/lamination/materials.php wiki states that the electrical steel is an alloy but only list Si as the other component but there are others.would you use something your not sure about that may contain a contaminant or something you know for sure whether it does or not and if it does whats in it and what you can expect.


----------



## Oneal58

Hi Everyone and Anyone, 
I have just got back in from adding more nitric acid to the lot of gold filled material (jewelry) I am dissolving the base metals from. 
I have added nitric and each time I get a reaction telling me there is more metal to be dissolved. 
I add more nitric, full 70% nitric now in 100ml increments since I moved the batch to large 1800ml beaker. 
I have added nitric now for the fourth time and am still getting a reaction and the flask heats up each time.
From what I have read I keep adding the nitric untill the reaction ceases. Telling me I have dissolved all base metals. 
In total, I have put 450ml of nitric into the batch of gold plated material. 
I started with 3/4 pound of gold filled items, rings, necklaces, Etc;.
I am still getting reaction and heating of the vessel.
I am going to stick with this routine untill I can add the nitric and not get the reaction and heat.
I am into this process now about 2-1/2 hours. 
Am I following procedure or have I left something out? 
Thanks, Oneal58


----------



## Geo

Oneal58

it takes 1 gallon of 70% nitric to digest 2 pounds of copper.you have 3/4 pound of material and not all of that is copper.you should use 1404 ml 70% nitric acid for this process. cover with a watch glass or any glass cover and add a little heat.


----------



## Oneal58

Thanks Geo, I appreciate that. So, I have a long way to go yet to get all the base metals dissolved. I will bring the heat plate outside tomorrow and start adding a little heat to get more work out of the nitric? I just didn't know how close or how far I was away from the goal of getting the base metals out. Thank you for answering that question. Live and learn. I should have looked that up before I got started, saved me a lot of worry. 
Can you overshoot with the nitric and cause yourself problems? What I mean is can you overwork the material with nitric? 
Thanks, Oneal59


----------



## butcher

Oneal,
Your 70% nitric should be diluted with water, for each gram of copper it would take about 4.2ml of 70% HNO3 and 4.2ml of water.
It takes about 130ml HNO3 70% and 130ml of water to dissolve an ounce of copper.
It takes about ½ gallon 70% Hno3 and ½ gallon water to dissolve a pound of copper.
(Thanks GSP, I hope I did not screw up the numbers here).

If your using 70% nitric and heating without water, much of your nitric is being lost to fumes, as the nitric is already at its azeotropic mix, adding water will help to keep nitric in your pot dissolving the copper. I find adding some 3% H202 hydrogen peroxide is also beneficial in solution.



Geo,
Thank you for that document, I have not found 80% nickel transformer laminates or inductor cores but I will search for them now, I would like a source of that white metal for other purposes.

Most all of the transformers and motors I have run into have soft iron laminates.

As I stated earlier there are many alloys and metals used, "electrical steels” used for their magnetic properties in the industry.
Some very exotic mixtures also inductors and choke’s also can have a wide variety of compounds.

I do not believe you would be playing Russian roulette using the iron transformer laminate or old motor laminates, My crystals of ferrous sulfate seem really pure, I have had no trouble using them (I could be washing the trouble (if any) out when I wash the gold powders I really cannot say), but as long as I achieve good results with the process I will continue to use it.

I would sure hate to post a process to make your own chemical if it would cause other's problems in there processes, and if that is the case I will not post it, and-or remove it.

Iron can be softer than aluminum and cut with a knife, although you will not run into much soft pure iron nowadays, blacksmithing a lost art they used a lot of it long ago, but modern steel has replaced its use, even our modern Iron is actually steel.


----------



## Oneal58

Hi Butcher, hope you are doing well today. Thank you for your post, this is good information to know. I realize I do not have the knowledge and understanding of the process yet. But to be competent it will take many, many, years, not months. You have to start somewhere and be hungry to learn, which I am. Just like understanding electrical properties, how it's made, what makes it do what it does, what characteristics it displays when certain loads are applied and componets are placed into a circuit. It has taken me a lifetime and many years of study and I still only scratch the surface on the subject of what I know. Just as some my think that wiring a house, calculating the loads, Etc;. May seem complicated, but honestly it's the most simplest thing to do in the electrical field. It is #1 on a scale to infinity! I say this because I am sort of like in that stage with refinning right now, it seems complicated. But I know down the road somehwere everything will click and the light will go off in my head. I will then build upon that base. I am full of questions but I have to learn how to ask them first, if you are following me. But I am a person that has to get his hands on something, try it, learn from my mistakes. But also try and prepare myself enough that I don't do damage or harm myself or others in the process. The electrical field can be dangerous, it killed my brother. You have to respect it, just as I respect this field. Carelessness can kill you! I feel confident that I can make a decent refinner. I realize I will be weak in the technical areas of the field just as I am weak in areas of the electrical field. But I made a decent electrician even though there is tons of things I didn't know and still don't know. 
So, when I ask all these questions that may sound dumb, consider where I am right now and please be forgiving and understanding. I am at #1 on a scale to infinity. 
Thanks Butcher
Oneal58


----------



## Oneal58

I left my Nitric Acid covered last night with a larger container on top of the nitric. I added a fresh batch of Nitric before I went to bed around 2:00 A.M.. I walked out the house this morning to where I had the batch of Nitric dissolving base metals on Gold Filled Jewelry. Thinking that any reaction would have been long stopped I lifted the lid before checking the direction of the wind or wearing my air cartridge face mask. I lifted the lid and before I knew it I got a whiff of strong Nitric. The Nitric was still fumming brown smoke. I stopped breathing and backed off from the Nitric container. My question is, how much of this stuff will do damage of some kind?
Thanks Oneal,


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## publius

1. *NO* respirator cartridge will filter out or neutralize Nitric Acid fumes and the associated vapors.
2. Any amount of exposure to Nitric acid and associated vapors will do damage to lung and eye tissue that may or may not heal.
3. Nitric acid reactions should be done under a fume hood or outside where the air can easily dilute the fume/vapors produced.

Play it safe.

Robert


----------



## Geo

this is a story i have told on the forum awhile back.i started dealing with nitric acid about twenty years ago making it for my father and others in the mining community.i had no chemistry knowledge and only knew the process as published in chemistry books.i made nitric for almost nine months forever sick and coughing up blood.i didn't know that i was slowly killing myself.even though i actually breathed the fumes a few times that strike my memory it seemed i was smelling the familiar smell of nitric all the time.now im disabled with COPD and cant walk through Lowe's or Walmart without oxygen.i have never smoked a cigarette in my life.you cant be too safe.nitric acid was called "the red death" by miners for a reason.respirators do not work for nitric acid.you really need to devise a way to vent these fumes away from you or build a fume hood.if your exposed to nitric acid fumes for only a short period of time it can at the least give you pneumonia and at the most it causes pulmonary edema that CAN kill you days after exposure.

please be careful.

Jeff


----------



## Oneal58

I have a fume hood installed. I didn't trust it to keep the fumes out of my enclosed area. I was warned many, many times to do this outside. Which I followed directions. I hope I didn't get enough into my lungs to cause any damage. I did the wrong thing when I held my breath, I should have turned and exhaled instead of holding the fumes in? I just didn't think quick enough. Oh well, I have been knocked silly by electrical jolts, through no fault of my own. Maybe this will get my attention to be even more diligent to stay on guard and stay safe. Thank you fellows for your input, time will tell. 
Thanks, Oneal58


----------



## Oneal58

Hi Everyone, just giving an update on my progress with the sulphuric cell. 
I diluted sulphuric by 1/3rd and then 5 hours later 1/3rd again. I ended up with what you see in the images I loaded. I will let this settle more and then pour off and wash again and decant.
Question 1- I am considering a Nitric treatment to the black powder or is this necessary Or the right thing to do? 
I will then add HCL/CL at 4 to 1 ratio. 
Question 2-Am I on base with the process so far, let me know if I have forgotten something? 

I have my 3/4 lb. gold filled items I am dissolving base metals by Nitric in it's final stage, I hope. I am warming solution to see if I can get any more reaction but I believe the process is about finished. To dissolve the base metals in this 3/4 lb. lot has taken about 1600ml of Nitric. That's on base with the fromula that Butcher gave me to use to dissolve copper. I am finding that this is an expensive route to take but I don't want to make that call yet, untill I see the returns. I know I will be making my own Nitric from now on. I picked up a couple more bags of Potassium Nitrate yesterday from farm supply. When I transfered the Nitric to the Coffee Pot the gold looked like it was metal free. 
Question 3-What are the signs of spent Nitric/how do I tell if it is spent. I have a large crock I will be putting the Nitric in for later processing. I have some Litmus Paper, can I use this to tell? I have loaded a picture of where I am with the gold filled. 
Last Question 4-Why can't I save the powder from my sulphuric cell and just put it in with the gold I will be getting from the Nitric Treatment of the gold filled material. 
Thank anyone for their response.


----------



## Geo

after you have diluted your sulfuric and reclaimed your powder you can reclaim the sulfuric acid by evaporating the water back out of the solution.


----------



## Oneal58

Thanks, Geo, every little bit of information is a big help. Oneal58


----------



## Oneal58

Could someone tell me why It's a bad idea to run my gold powder that I got from the sulhuric cell through with the values recovered from the nitric treatment of the gold filled jewelry? I know that HCL/Cl of the powdered gold has been recommended. I am fine with that, I just would like to know (why is it best) to use HCL/CL on the sulphuric cell powder and the AR on the values from the nitric process. This is just so I can understand why? Thanks to anyone who will answer. Oneal58


----------



## Geo

i dont see a problem with dissolving those at the same time in the same solution.the problem arises when you go from a hcl solution to a nitric solution without first incinerating the material.or from nitric solution to hcl solution for that matter.you cant rinse acid from your material,for instance,if you used AP to process gold plated items and you wanted to insure the base metal was gone it wouldnt be wise to go straight to a nitric acid wash because as you know nitric acid and hcl acid make AR.your expecting to wash your foils to remove any base metal left and instead you dissolve a portion of your gold.if you didnt know that in advance you may neutralize and discard the solution containing your gold.and if you had dried and weighed your foils after rinsing with water thinking you removed the hcl and then washed in nitric you would be wondering where your gold went.


----------



## philddreamer

"Could someone tell me why It's a bad idea to run my gold powder that I got from the sulhuric cell through with the values recovered from the nitric treatment of the gold filled jewelry?"

I don't think its a bad idea, if I'm recovering the gold, not refining it. I've done it, & noticed no problem. Someone please correct me if I'm wrong.

"I know that HC/Cl of the powdered gold has been recommended. I am fine with that, I just would like to know (why is it best) to use HC/CL on the sulphuric cell powder and the AR on the values from the nitric process. This is just so I can understand why? Thanks to anyone who will answer. Oneal58"

HCl/Cl is mostly recommended because is cheaper than AR & the chlorine is easier to get rid of before trying to precipitate. It's a process the noobs can learn to "handle" quicker. Also, some folks can't afford the nitric or can't find it; HCl & bleach are very easy to find, so its the easiest alternative to AR. Keep in mind that HCl/Cl takes longer to digest the gold.
We all have a preferred process for dissolvong gold, mine is AR. HCl/Cl when I'm cleaning filters, or dissolving gold from chinaware...

Take care!

Phil


----------



## butcher

Oneal, 
You could do these separate for less trouble, or combine them.

Here are some things to consider helping you to make the decision.

Much of what I chose next would be decided on how much base metals I may have in these powders from the two different processes I used earlier.

I would most likely wash both recovery’s of gold well and mix them together, but realizing that there could be traces of nitrates in the mix,(this could be dealt with), after a good wash of the powders you could incinerate the powders and avoid that trouble of nitrate's.

Now do I have tin that may give me trouble? If so a boil in HCl, then dilute and settle and decant then hot water wash settle decant repeat till clear, and re-incinerate (if going back to nitric wash later). 

Think about this is if using HCl/bleach you do not want to evaporate too much or you will have salts to deal with (not that big of deal).

Which process I chose next would have several factors to think about, how much base metals are left? HCl/bleach is easier but I would not be able to do another wash with nitric acid to remove these base metals, (unless I wanted to deal with traces in this solution later, not that big of deal, but do I want to go there?).

I could go to another nitric wash and then aqua regia, but here I will have to eliminate the nitric acid by slow evaporations, and this is harder for beginners to deal with and precipitation is also harder for beginners (as they may still have nitric in solution) which way or process do I choose?

After incineration you could use HCl with small additions of bleach used to put gold into solution this is much easier to deal with (than aqua regia), but if you still had some base metals that your washes may have missed, they would also report to this solution, as long as there was not that much base metals the process will work fine and I can do another refining for purity.

Or after incineration you could heat in HNO3 70% and water 50:50mix, then go to aqua process (more difficult) which way do I choose?

I think HCl/bleach would be my choice.


----------



## Oneal58

Hi kadriver, 
I have the black powder now out of the sulphuric cell. I also have the foils from my first nitric acid treatment of the gold filled jewelry. I can't seem to get any answers on some of my questions on the forum. I hope you can help me. 
I have the black powder from the sulphuric cell and the foils from the nitric bath of the gold filled jewelry. 
Do I use 2 different type processes here, 1 for the black powder, (HCL/CL) and 1 for the foils, (AR). Then decant and drop the gold>
Is the answer to the question is that the gold black powder from the cell is too pure (high karat) for the AR to attack?
Will a nitric bath for the black powder help any, I might have dropped some silver and other metals along with the gold when stripping with the cell?
Am I missing any steps in the process?
Is this the best route to take with each. Could you tell me why the 2 different processes is recommended? I need to know this , just for me, for the sake of knowing it?
Thanks Kadriver,
Thanks, Oneal58


kadriver said:


> Oneal58:
> 
> I recall having to allow the acid in my stripping cell to settle for several days like Phil pointed out.
> 
> Eventually you could see through the acid and the black material had collected on the bottom of the cell.
> 
> The acid was not crystal clear, it was still dark, but transparent.
> 
> I have saved a bunch of gold plated jewelry that has been accumulating. I may have to get the sufuric acid stripping cell set up and get it running again.
> 
> I think December 2010 was the last time that I ran it.
> 
> Back then I was too green and anxious to have to wait for the black gold powder to build up in the cell - let alone the idea of having to wait for it to settle.
> 
> Since I have gained a little more experience, hopefully I have gained some patience.
> 
> thanks - kadriver


----------



## Oz

I am going to skip any answers to your questions and ask instead why I see so much of your processing (in your first picture) that looks like your primary work space is occupying indoor living space. None of this is worth your health or that of your family’s.


----------



## Geo

Oneal58

i wish you the best of luck.i hope you figure all of this out and look forward to seeing your first gold button.i will not clutter your thread with my useless post anymore.

for all the other members, if there are any that can and are willing to help Oneal58 please try and help him figure out this puzzle.


----------



## Oneal58

Hi Geo,
Please forgive me if I have offended you in any way. If I did I didn't mean to. I very much appreciate your post and look forward to each and every one of them. I check my computer many times a day for post on the questions that I ask. I am still learning how to use the site. After taking another look at previous post on this thread I see where you have answered this question that I had been trying to get an answer to. I am very sorry, honestly. Please don't stop posting and helping me. You have been in there for me for many, many post and I apppreciate you trying to help me. But I have had a couple of heart attacks and they have changed me. I have a tendency to get tunnel vision and overlook things, such as your post to answer the question I asked. It wasn't because I didn't seek your advice or want your advice, it was just that I didn't see it. Please don't leave me hanging here. I need everyone here on this forum and the last thing I want to do is offend anyone. If I offended you, I am sorry. Will you accept my apology, it is heart felt. 
I need to say when I asked kadriver the question, it was because I didn't know where else to turn. It seemed as though nobody was reading my post and some of the questions I asked I could not get answers to. I drove to meet with Kadriver and know him. He is the person who gave me a lot of material to get me started. When I thought no one was looking at my post I had no where else to turn but to someone who I thought would help me and I knew. 
But thank each and every one of you. If I have not thanked all of you in every post it was just an oversight and I am sorry. 
Oneal58
As far as my working space it is an old house that my mother lived in. It is on my porperty and I started to tear it down last year. The termites have done a number on it but I still use it for storage. I would not dare bring this operation inside around my grand's or my wife. 
Member's on this site, please do not take me wrong, I really don't know how I sound to others reading what I post. I may sound arrogant, selfish, dumb, I just don't know? But I know one thing for sure, I need each and every one of you. Your help is not taken for granted or unappreciated, no matter how it may sound on these post. Thank each and every one of you for your help and your post. Please don't take me wrong, I am not that way.
Thank You, Oneal58
A


Geo said:


> Oneal58
> 
> i wish you the best of luck.i hope you figure all of this out and look forward to seeing your first gold button.i will not clutter your thread with my useless post anymore.
> 
> for all the other members, if there are any that can and are willing to help Oneal58 please try and help him figure out this puzzle.


----------



## Oneal58

Hi Butcher and everyone who has been helping me. I truely appreciate it. 
After close inspection of the material that came out of the nitric bath I can see that there are still pieces of grey metal on a good bit of the gold. I went ahead with the advice to combine the 2 and give both the sulphuric cell values and also the values that needed a little longer in Nitric. I have got the material in the nitric bath now. It's cold here today and I have had to heat the nitric to get a reaction.
Question 1- The color of the first bath in Nitric was a dark bluish geenish color. The color of this batch is almost a black color? Is it becasue most of the copper has been dissolved in the first nitric treatment?
Question 2-Butcher you said that I would have to evaporate the nitric by slow evaporations. Can I evaporate in the same flask as I am giving the material the nitric bath in?
Question 3-Do I dilute in some way by adding the nitic with values to water and then evaporate many times this way? After several evaporations do I evaporate down dry? That is once I am sure all the nitric has been evaporated?
Question 4- Then go with the AR or do I need to recover, incinerate and then go to the AR treatment
P.S.
Question 5- I did not do the HCL Boil for tin before the nitric treatment. Somehow I overlooked this. Can I do the HCL Boil for tin when I get all the Nitric out, then incinerate and do the HCL Boil for tin? 
I know Butcher you said this was the hard route for beginners. But I am in this for the long haul with everyone's help. I want to tackle the process that I will be using on a regular basis from here on out.
Am I in line here or am I leaving out something?
If anyone wants to reply to this post I welcome it. 
Thank you butcher, and everyone! 
Oneal58
P.S., I left out the HCL boil for tin. Can I do the HCL boil for tin after I get all the nitric out before the AR??

I very much appreciate your post. I can't figure out why these post was not on my page untill this morning.
Butcher I just want to say I very much appreciate your help. I am seeing things more clearly now. Without you and the members of this forum I could not go on, on my own. Thank you Butcher for all your help. You have been there for me from the beginning and I appreciate you. I will follow your advice, Thank You,
Oneal58



butcher said:


> Oneal,
> You could do these separate for less trouble, or combine them.
> 
> Here are some things to consider helping you to make the decision.
> 
> Much of what I chose next would be decided on how much base metals I may have in these powders from the two different processes I used earlier.
> 
> I would most likely wash both recovery’s of gold well and mix them together, but realizing that there could be traces of nitrates in the mix,(this could be dealt with), after a good wash of the powders you could incinerate the powders and avoid that trouble of nitrate's.
> 
> Now do I have tin that may give me trouble? If so a boil in HCl, then dilute and settle and decant then hot water wash settle decant repeat till clear, and re-incinerate (if going back to nitric wash later).
> 
> Think about this is if using HCl/bleach you do not want to evaporate too much or you will have salts to deal with (not that big of deal).
> 
> Which process I chose next would have several factors to think about, how much base metals are left? HCl/bleach is easier but I would not be able to do another wash with nitric acid to remove these base metals, (unless I wanted to deal with traces in this solution later, not that big of deal, but do I want to go there?).
> 
> I could go to another nitric wash and then aqua regia, but here I will have to eliminate the nitric acid by slow evaporations, and this is harder for beginners to deal with and precipitation is also harder for beginners (as they may still have nitric in solution) which way or process do I choose?
> 
> After incineration you could use HCl with small additions of bleach used to put gold into solution this is much easier to deal with (than aqua regia), but if you still had some base metals that your washes may have missed, they would also report to this solution, as long as there was not that much base metals the process will work fine and I can do another refining for purity.
> 
> Or after incineration you could heat in HNO3 70% and water 50:50mix, then go to aqua process (more difficult) which way do I choose?
> 
> I think HCl/bleach would be my choice.


----------



## Oneal58

Hi Oz, 
I am working out of a old house that I was going to tear down. It was where my mother lived and most the house has been damaged by termites. I appreciate your concern but I would not dare bring this type process into my home around my grands and my wife. I have even told my grands when they see Pops in the old house to not even come close to it. That it is really dangerous and could kill or hurt you or me. They are 9 years and 4 years old. I have instilled a fear of them going near the old house, which was my purpose. I wouldn't trade 1 of my grands, wife for all the gold in the world. You see, I have already lost my son due to a farm accident and a brother that got electrocuted. So, I realize what family means, it is my job to keep them safe. So, don't worry, protecting my family is priority #1. 
Thank you Oz for your concern and thank you Oz for your many post. I really appreciate you and all your post. I appreciate and am thankful for everyone on this site. I can't say this often enough. Thanks to everyone. 
Oneal58


Oz said:


> I am going to skip any answers to your questions and ask instead why I see so much of your processing (in your first picture) that looks like your primary work space is occupying indoor living space. None of this is worth your health or that of your family’s.


----------



## Oneal58

Hi Phil, thank you so much for your postings. You are very much appreciated, I can't say this often enough. All of you on this site is very much needed and appreciated. Not taken for granted but really appreciated. I am very thankful for each and every one of you. 
Thank you Phil for your many post!
Oneal 58




philddreamer said:


> "Could someone tell me why It's a bad idea to run my gold powder that I got from the sulhuric cell through with the values recovered from the nitric treatment of the gold filled jewelry?"
> 
> I don't think its a bad idea, if I'm recovering the gold, not refining it. I've done it, & noticed no problem. Someone please correct me if I'm wrong.
> 
> "I know that HC/Cl of the powdered gold has been recommended. I am fine with that, I just would like to know (why is it best) to use HC/CL on the sulphuric cell powder and the AR on the values from the nitric process. This is just so I can understand why? Thanks to anyone who will answer. Oneal58"
> 
> HCl/Cl is mostly recommended because is cheaper than AR & the chlorine is easier to get rid of before trying to precipitate. It's a process the noobs can learn to "handle" quicker. Also, some folks can't afford the nitric or can't find it; HCl & bleach are very easy to find, so its the easiest alternative to AR. Keep in mind that HCl/Cl takes longer to digest the gold.
> We all have a preferred process for dissolvong gold, mine is AR. HCl/Cl when I'm cleaning filters, or dissolving gold from chinaware...
> 
> Take care!
> 
> Phil


----------



## Oneal58

Hi Everyone, I just want to say that I don't know what happened to my postings. It seemed I was asking the same question trying to get an answer to and I had no responses? I don't know if my computer was updating correctly or what had happened? I just did not see the many post that all of you had put up for me. I still can't figure out why I didn't see the many answers I had gotten. Was the site updating correctly yesterday? I truely can't see how I overlooked them, but it happened. And I am sorry if I made any of you feel that I wasn't taking your advice. 
When I wrote kadriver last night to ask him before I went to bed I honestly did not see the many post that I had received on the question. I thought everyone had either stopped reading my post or abandoned me, honestly!
I want to thank each and every one of you from the bottom of my heart. I don't know what I would do if you weren't here to help me. You take your time and energy to answer these post. Not because you have to or in some cases even want to. You do it to just help. That's a quality that few have and it does not go unrecognized. You are not taken for granted and you are appreciated, each and every one of you.
Thank You from the bottom of my heart for your help. 
Oneal59


----------



## Oneal58

Hi Everyone,
I am right in the middle of a Nitric Evaporation and know that I cannot bring the solution to a boil, (Hoke's) I can no longer see brown fumes comming from the solution. 
Question 1- Does this mean all the nitric has worked off. I have the amount of water left in the beaker. This has taken all afternoon. I have kept the container covered the whole time. Venting through a wet cloth. 
Question 2-I need to treat the solution for tin, can I add HCL now while the solution is warm? There is about 300ml of solution in the container, how much HCL to add if this is the right thing to do? Or do I wait to treat with sulphuric during the AR process?
Question 3- Once treated do I decant, filter, wash, incinerate and then go with AR? 
Am I on base? 
Thanks to anyone who has the time to answer.
Oneal58


----------



## Geo

i have a question.when you say evaporating nitric are you talking about from an AR solution?

is this the process you were doing of removing base metal with nitric acid?

If so there is no need to evaporate the nitric as that is only needed in an AR solution. If you add hcl acid now you will create AR and dissolve your gold. IF this is a process to remove base metal with nitric acid and all the base metal is dissolved and your left with gold and perhaps some salts now is the time to turn off the heat and let the solution cool. Test with stannous chloride to make sure theres no gold in your solution. Dilute your solution with tap water 50/50 and reheat to a slow boil to dissolve the salt. Turn off the heat and let everything settle. Decant as much solution as you can without pouring out any foils or solids. Add water and return to the heat and bring to a slow boil. Repeat this until the rinse water is clear,do not add hcl acid. You should be left with clean gold foils and powder. Now proceed to the refining stage.


----------



## goldenchild

Since it sounds like you've done your homework I will offer my help.

1. No brown fumes usually mean no more nitric but then again there could be some left in solution. You're supposed to periodically add HCL to an evaporating solution to drive off nitric. More specifically when the solution becomes more viscous. HCL is actually exhausted letting no more nitric evaporate out of solution, hence the additions of fresh HCL. This is even more evident when an AR digestion comes to a halt but there is plenty of nitric still in solution. An addition of fresh HCL will start it right back up. Don't go overboard with evaporation. The HCL doesn’t have to be like maple syrup before fresh HCL additions. This is one of those things you will learn from experience.

2. Its highly advised to get rid of the tin before you digest with AR or you will end up with a big mess. Remember tin reacts with gold chloride to get that nice purple color. No imagine digesting tin and gold at the same time. An excess of HCL doesn't hurt so in an evaporating solution of say 300ml I would say to add 25 to 50ml of fresh HCL at a time. And yes you can and should add HCL while solution is warm. BE CAREFUL! Hoke states that a small amount of H2SO4 is added to the AR solution to hasten the expulsion of nitric and to drop any lead that may be in solution.

3. Once you are finished with steps 1 and 2 let the solution completely cool and settle. Some will chill the solution and others dilute with water. Decant and filter your solution. Precipitate and wash thoroughly. Follow steps 1-3 again if necessary.

P.S.
Learning to use just enough nitric to complete a digestion will make step 1 a breeze.

Edit
After reading Geo's post I have to now point out that 1-3 is AFTER you have recovered your gold.


----------



## kadriver

Oneal58:

I just finished a 2.4 troy ounce pure gold bar and shipped it out to the refiner today. i worked late last night and got back to it early this morning - self inflicted pressure. I called and got a price lock on the gold bar before it was refined and ready to go! So I was under pressure to ship it out by the end of the day today so the refiner would get the gold by tomorrow (Friday).

Anyway, I have briefly read through your posts here and this is my experience:

I have processed gold filled scrap only one time using HCl/CL. It was when I first ordered the DVD from lazersteve. I did it for the experience and I have not done it since. I have plenty of nitric acid and the AR treatment is something I am familiar with. AR=aqua regia

You can use AR to dissolve the gold filled foils. You can also use AR for the black powder from your sulfuric cell. I don't see any reason why you can't use HCl/Cl for either type of these materials also. I don't think it makes a difference.

I am currently in the middle of a gold filled recovery and refinement myself. I started with 260 grams of gold filled watch covers and jewelry.

I started by incinerating the gold filled scrap to redness. Then I added distilled water and then nitric acid (about 850 ml each).

I put it all in a coffee pot with a lid and "cooked it" for several hours.

I then let it sit for a day or so. Once settled and cool, I filtered off the liquid, allowing the "purple mud" the go into the filter at the very end. I took the clear filtered liquid which was dark blue, and neutrailzed it with Urea.

I put the filtered liquid in a large beaker and added a coil of copper wire to cemented the silver from the solution - there was about 1 ounce or so (estimate) of cemented silver in the liquid - it is still cementing as I write this.

I rinsed all the fine material from the coffee pot into the filter, but kept the foils and shells of gold in the coffee pot. There was a pale purple mud about 1/8 inch thick in the filter. I saved the filter, just left it in the buchner funnel.

I then re-treated the gold foils with some more (about 200ml total) dilute (50/50) nitric as some of the base metals had not dissolved completely.

Also, I found a chain I had saved from a previous batch from some months ago. The chain was saved because it still had base metal that was not dissolved. I added this chain to the foils in the coffee pot with the second 50/50 nitric treatment.

More red fumes came from this reaction confirming that base metals were present.

I cooked the batch this time for about 2 hours until no more red fumes were present and the solution was boiling vigorously. the solution was black this time - I think because of the chain, it may have had iron - I don't know.

Oneal58, I am pretty sure there is lead and tin are in my batch of gold filled scrap. I say this because of what I found in the filter paper from the first filtering of the liquid from the coffee pot - a pale purple paste that looks like lite purple silver chloride. I am thinking that this is tin and lead mixed with some colloidal gold and gold powder. The gold can be recovered from this mud according to Harold.

I would guess that there is a good chance that your gold filled batch also has these contaminates. Therefore, it is probably not a good idea to mix your two batches together - although I read where you have already done so.

A while back, Harold had written a post where he recommended that gold filled foils, mud, and everything should be sent to the filter - this is one of the only times that it makes sense to put all the material into the filter.

Once in the filter, Harold stated, that the whole batch should then be incinerated, filter and all - to get the gold mud - then the incinerated material should be treated (boiled) with full strength HCl.

Boiling in full strength HCl will get rid of the tin and lead that are sure to be present from gold filled scrap.

Once the treatment with HCl is complete, wash with water several times, then treat with aqua regia and proceed as usual with filtering and precipitation of the gold.

I hope I have not mis-quoted Harold on this. I have this process printed out and in a notebook at my shop and just happened upon it as I was reviewing.

The foils from the second cook are still sitting in the coffee pot in that black liquid. Tomorrow I plan to pour eveything into the filter as Harold recommended. Foils, gold mud, and anything else from the reaction vessel. Then I will let it dry and incinerate the whole mass - filter and all. Then treat by boiling it in HCl. Once complete I will wash with distilled H2O (Tap is probably OK here) and then dissolve in aqua regia.

I will let you know how this batch turns out. I am curious to know how it will turn out myself as this will be the first time I use Harold's process on this gold filled batch. i am hoping for good results.

I have done gold filled batches in the past were I rinsed out all the purple mud into the filter, then saved the filter. The foils were not allowed to go into the filter. I rinsed the foils in the coffee pot with plenty of hot water, then dissolved the foils only (no mud and no incineration).

The resulting gold bead came out OK, but it was not very pure and had a silvery coating on top, but it tested at least 22k. I think it weighed about 3 or 4 grams. i sold it on Ebay as 22k Gold and got about 80% of spot price for it with a positive feedback from the buyer. 

I hope this is helpful to you. Aslo, I hope I did not mis-quote Harold on the process I wrote about above in this post!

kadriver


----------



## butcher

Oneal,
Everybody here wants to help< and all are giving good advice.
I see several problems, one you’re just learning and may not grasp the whole picture,
Some are giving advise based on the long wording in your questions, and then we may get mixed up on where you are or where your planning to go, so it seems with so many of us giving you directions (in this confusion) you will start getting pointed into many directions.

This way of helping you is confusing you and us.
Normally it is better to follow one person’s advice that know exactly what you’ve done and can just tell you what to do next.

You get a broad view with many members helping but it can also get confusing.

So lets get all on the same page or maybe let one person help here.

First we either need to make the questions and answers simpler.
Know exactly where you’re at and which way you wish to go.
Understand each step that has been taken.
And the direction we plan to go.
And we need to get all our answers pointing the same direction.

Please explain where you are please making it simple.
Explain your plan on process you intend to take.

The members helping can give better steps to take,

Oneal then you still may get a couple of different advice, so members need to know which plan your going with and the next steps, some of us may choose a different route so some answers may differ.

Hope this helps
This is a good thread for many to learn from, but can also become one to confuse them.


----------



## Oneal58

Thanks Geo, I need to let you know right where I am, how I got there and where I was trying to get to. I want to get on the same page with everyone. I might have mislead you and others on where I was and what I was trying to do plus which route I have taken and why. I will post tonight and try to explain what I have done to the best of my ability. Then you will know where I am. And would appreciate any advise on where I need to go from here. I feel that some may think I am going the HCL/CL route. I didn't go that route for the reasons I will post. 
Thanks Geo, a new post will follow. I am sorry for the confusion I have caused. 
Oneal58



Geo said:


> i have a question.when you say evaporating nitric are you talking about from an AR solution?
> 
> is this the process you were doing of removing base metal with nitric acid?
> 
> If so there is no need to evaporate the nitric as that is only needed in an AR solution. If you add hcl acid now you will create AR and dissolve your gold. IF this is a process to remove base metal with nitric acid and all the base metal is dissolved and your left with gold and perhaps some salts now is the time to turn off the heat and let the solution cool. Test with stannous chloride to make sure theres no gold in your solution. Dilute your solution with tap water 50/50 and reheat to a slow boil to dissolve the salt. Turn off the heat and let everything settle. Decant as much solution as you can without pouring out any foils or solids. Add water and return to the heat and bring to a slow boil. Repeat this until the rinse water is clear,do not add hcl acid. You should be left with clean gold foils and powder. Now proceed to the refining stage.


----------



## Oneal58

Hi Butcher, I think I have not been clear on what I have done, how I got there and where I am trying to get to. I will be making another post tonight just to let everyone know where I am and try to find out where I need to go next. I will be posting to the best of my abilities where I am. Post will follow.
Thanks Butcher,
Oneal58



butcher said:


> Oneal,
> Everybody here wants to help< and all are giving good advice.
> I see several problems, one you’re just learning and may not grasp the whole picture,
> Some are giving advise based on the long wording in your questions, and then we may get mixed up on where you are or where your planning to go, so it seems with so many of us giving you directions (in this confusion) you will start getting pointed into many directions.
> 
> This way of helping you is confusing you and us.
> Normally it is better to follow one person’s advice that know exactly what you’ve done and can just tell you what to do next.
> 
> You get a broad view with many members helping but it can also get confusing.
> 
> So lets get all on the same page or maybe let one person help here.
> 
> First we either need to make the questions and answers simpler.
> Know exactly where you’re at and which way you wish to go.
> Understand each step that has been taken.
> And the direction we plan to go.
> And we need to get all our answers pointing the same direction.
> 
> Please explain where you are please making it simple.
> Explain your plan on process you intend to take.
> 
> The members helping can give better steps to take,
> 
> Oneal then you still may get a couple of different advice, so members need to know which plan your going with and the next steps, some of us may choose a different route so some answers may differ.
> 
> Hope this helps
> This is a good thread for many to learn from, but can also become one to confuse them.


----------



## Oneal58

Thanks Kadriver, I need to let everyone know where I am, how I got there and where I was trying to get to. I want to get on the same page with everyone. I might have mislead you and others on where I was and what I was trying to do plus which route I have taken and why. I will post tonight and try to explain what I have done to the best of my ability. Then you will know where I am. And would appreciate any advise on where I need to go from here. I feel that some may think I am going the HCL/CL route. I didn't go that route for the reasons I will post. 
Thanks Kadriver, a new post will follow. I am sorry for the confusion I have caused. Look for another post to explain where I am. 
Oneal58


kadriver said:


> Oneal58:
> 
> I just finished a 2.4 troy ounce pure gold bar and shipped it out to the refiner today. i worked late last night and got back to it early this morning - self inflicted pressure. I called and got a price lock on the gold bar before it was refined and ready to go! So I was under pressure to ship it out by the end of the day today so the refiner would get the gold by tomorrow (Friday).
> 
> Anyway, I have briefly read through your posts here and this is my experience:
> 
> I have processed gold filled scrap only one time using HCl/CL. It was when I first ordered the DVD from lazersteve. I did it for the experience and I have not done it since. I have plenty of nitric acid and the AR treatment is something I am familiar with. AR=aqua regia
> 
> You can use AR to dissolve the gold filled foils. You can also use AR for the black powder from your sulfuric cell. I don't see any reason why you can't use HCl/Cl for either type of these materials also. I don't think it makes a difference.
> 
> I am currently in the middle of a gold filled recovery and refinement myself. I started with 260 grams of gold filled watch covers and jewelry.
> 
> I started by incinerating the gold filled scrap to redness. Then I added distilled water and then nitric acid (about 850 ml each).
> 
> I put it all in a coffee pot with a lid and "cooked it" for several hours.
> 
> I then let it sit for a day or so. Once settled and cool, I filtered off the liquid, allowing the "purple mud" the go into the filter at the very end. I took the clear filtered liquid which was dark blue, and neutrailzed it with Urea.
> 
> I put the filtered liquid in a large beaker and added a coil of copper wire to cemented the silver from the solution - there was about 1 ounce or so (estimate) of cemented silver in the liquid - it is still cementing as I write this.
> 
> I rinsed all the fine material from the coffee pot into the filter, but kept the foils and shells of gold in the coffee pot. There was a pale purple mud about 1/8 inch thick in the filter. I saved the filter, just left it in the buchner funnel.
> 
> I then re-treated the gold foils with some more (about 200ml total) dilute (50/50) nitric as some of the base metals had not dissolved completely.
> 
> Also, I found a chain I had saved from a previous batch from some months ago. The chain was saved because it still had base metal that was not dissolved. I added this chain to the foils in the coffee pot with the second 50/50 nitric treatment.
> 
> More red fumes came from this reaction confirming that base metals were present.
> 
> I cooked the batch this time for about 2 hours until no more red fumes were present and the solution was boiling vigorously. the solution was black this time - I think because of the chain, it may have had iron - I don't know.
> 
> Oneal58, I am pretty sure there is lead and tin are in my batch of gold filled scrap. I say this because of what I found in the filter paper from the first filtering of the liquid from the coffee pot - a pale purple paste that looks like lite purple silver chloride. I am thinking that this is tin and lead mixed with some colloidal gold and gold powder. The gold can be recovered from this mud according to Harold.
> 
> I would guess that there is a good chance that your gold filled batch also has these contaminates. Therefore, it is probably not a good idea to mix your two batches together - although I read where you have already done so.
> 
> A while back, Harold had written a post where he recommended that gold filled foils, mud, and everything should be sent to the filter - this is one of the only times that it makes sense to put all the material into the filter.
> 
> Once in the filter, Harold stated, that the whole batch should then be incinerated, filter and all - to get the gold mud - then the incinerated material should be treated (boiled) with full strength HCl.
> 
> Boiling in full strength HCl will get rid of the tin and lead that are sure to be present from gold filled scrap.
> 
> Once the treatment with HCl is complete, wash with water several times, then treat with aqua regia and proceed as usual with filtering and precipitation of the gold.
> 
> I hope I have not mis-quoted Harold on this. I have this process printed out and in a notebook at my shop and just happened upon it as I was reviewing.
> 
> The foils from the second cook are still sitting in the coffee pot in that black liquid. Tomorrow I plan to pour eveything into the filter as Harold recommended. Foils, gold mud, and anything else from the reaction vessel. Then I will let it dry and incinerate the whole mass - filter and all. Then treat by boiling it in HCl. Once complete I will wash with distilled H2O (Tap is probably OK here) and then dissolve in aqua regia.
> 
> I will let you know how this batch turns out. I am curious to know how it will turn out myself as this will be the first time I use Harold's process on this gold filled batch. i am hoping for good results.
> 
> I have done gold filled batches in the past were I rinsed out all the purple mud into the filter, then saved the filter. The foils were not allowed to go into the filter. I rinsed the foils in the coffee pot with plenty of hot water, then dissolved the foils only (no mud and no incineration).
> 
> The resulting gold bead came out OK, but it was not very pure and had a silvery coating on top, but it tested at least 22k. I think it weighed about 3 or 4 grams. i sold it on Ebay as 22k Gold and got about 80% of spot price for it with a positive feedback from the buyer.
> 
> I hope this is helpful to you. Aslo, I hope I did not mis-quote Harold on the process I wrote about above in this post!
> 
> kadriver


----------



## Oneal58

Hi Everyone, this is Oneal58. 
I am going to try and tell everyone exactly where I am right now. I think I have not conveyed to everyone exactly where I am at, how I got there and where I would like to try to go. I am sorry for this confusion. It is totally my fault. 
I will first explain how I got here. As all of you who have been helping me know I worked about 5 days on the sulphuric cell stripping gold plated Jewelry. I ended up with a small amount of black powder from the cell. I diluted the sulphuric down in steps and washed the black powder several times in distilled water. 
Where the confusion is coming in at is that I had gold filled jewelry I was working on during the same time. I spent 1600ml of Nitric on 3/4 lb of gold filled jewelry dissolving the base metals from. I decanted/filtered and saved the dark blue greenish solution and put it in a big crock for later processing.
After taking a closer look at the material out of the Nitric Bath that held the (gold filled items) Jewelry, I saw that the material still had some grey metal in and on the gold filled items. 
Step1- Here is what I did, I put the black powder from the sulphuric cell in with the partially dissolved gold filled material from the nitric bath into the same beaker. 
Step 2- I added 200ml of water and 200ml of Nitric to the gold black powder from the sulphuric cell (plus) the material (foils attached to metal) into the same flask, (all material in 1 flask)
Step 3-I started warming the Nitric to get a reaction started. Once the reaction started I covered the container and let the solution sit on low heat while covered. The solution vented dark brown vapors for 45-1 hr. and then stopped fuming. I continued heating the solution on low heat to make sure that I drove off as much nitric as possible. 
Step 4-I stopped right there, took the flask off the heat, covered it and put it up to cool. 
*This is where I am at right now. *
I believe I have all the base metals dissolved and am waiting for the solution to cool. 
I know I probably have tin and maybe lead still in solution due to the purple color I got from the wash water when I washed it before I put the 2 together. 
*I want to go with the AR recovery method*, I know it's harder on a beginner but this is the method of choice I hope to use in all my recoveries in the future. 
I hope this will let everyone know where I am in the process and where I would like to go with your help. 
I apologize to everyone for not being clear where I was at and where I was headed. I must pay better attention trying to inform you of where I am in a process and where I want to go to. I have got to be able to know where I am before I can relate to you for you to be able to help me. 
Thank all of you for your help, this would be impossible for me if it wasn't for you. I am sorry for the confusion. 
Oneal58
Oneal58


----------



## Geo

In that case follow the directions i listed above with rinsing the foils and powder till the rinse water is clear. If you feel there is more tin in the powder and want to try and remove it before AR process you will need to incinerate your material first,but personally in my opinion i wouldnt think theres enough tin to effect the outcome of your AR process and besides, you will wash the final product with hot hcl acid before you melt anyway. Theres no real need to dry the material as long as all the base metal is removed,decant as close as you can get without pouring off the foils or powder and proceed with AR in the same flask. Dr Poe has posted on colloidal gold and may be able to tell you more about that subject. What i do know is you can save the purple wash water and evaporate all the water till it dries completely,im not sure how much gold could be in the purple water or even if its worth trying to reclaim. My guess would be somewhere in the millionths of a gram category but after the water dries it can be redissolved or maybe even condensed down and stored until when/if you get more it can be added to make it worth processing.


----------



## butcher

Oneal, 
Here are my thoughts:

Junk jewelry, gold plated jewelry, and gold fill, can have many undesirable metals involved depending on what they were from. Copper base metals common (pewter, lead tin and so on would not be uncommon).

Your color of the wash water is an indication of some metals that are going to give you headache, it sounds like colloids, probably carbon-ous trash in solution with tin and other undesirable metals.

(The colloids can be broken with heating and strong acidic solutions (we will not discuss now in detail) 

(The rinse water from nitric rinse add it to the spent nitric solution (after filtering) we will boil this down later concentrating the acid and recovering any traces from it).

You had sulfate salts with the lead salts so lead would very possibly be in powders (nitric may not have remove lead here).

This process can be done in one dish keeping powders in the pot removing liquids as needed,
I use a white corning type casserole dish, on electric hot plate with solid metal cast iron burner.

You may see some other details in this post to another member: http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=12165




Powders separated from nitric solution these I would wash rinse and dry.

Incinerate powders to red hot, (to oxidize base metals like tin, burn off any trash, remove sulfates, nitrates and so on)

Let cool spray dry powders with mist from water bottle to wet, then add HCl.

Boil in HCl, (then the add water to dilute) keep HCl-water hot but below a boil, let powders settle well in this hot solution, and then decant hot solution, (this will help to remove tin, lead, trash, any copper you may have and other things you do not want in solution later (some gold colloids may follow these rinses).

Add water to powders and repeat these very hot water rinses until water solutions we decant are clear.

(Keep these chloride washes together in jar separate from other waste let them settle we will also concentrate and filter them later to retrieve values they may hold later).

Now heat to dry powders.

Re-incinerate the powders red hot, (This will help to remove chlorides that can give us trouble with our next nitric step), Cool.

Again spray down with mist water bottle, wash sides of pot down (this helps keep fine powder from bubbling and floating away when you pour in acids).



Add dilute nitric acid (70% HNO3 + H20 50:50 solution), bring to boil, then cool, letting powders settle well, decant solution and then, several hot water washes (decanting only from well settled powders).

Now add HCl to cover the powders (with little bit of excess), add nitric in very small amount (drops) with med heat (let reaction complete), if all gold has not dissolved, then add a few more drops (let reaction complete) repeat till all gold in solution.

Now we will eliminate any excess nitric you may have:

Let solution heat (not too hot but fumes evaporating off), (watch for boil over), (keep eye on solution but your nose out of it), (have wash bottle handy if foaming occurs you can spray it down with mist from water bottle).

Add a few drops of sulfuric acid, (this will help to remove lead in later steps, and keep from forming salts on evaporations).

Concentrating solution we want it thick like syrup but do not make crystals or salts, add some HCl to wet again, heat until syrup again, repeat HCL to wet, one more time evaporate to syrup, add water till solution is four times volume, turn off heat cover pot let sit overnight.

Now silver if any will be in powders with lead if any, (it should be cold enough outside to crystallize these out of solution.
(We could test for more dissolved silver with a little non-iodine table salt, but since we will be refining this again, I would not mess with that now).

Decant this gold solution, filtering into a clean vessel; let this settle to see if clear.

Now you can use precipitant of choice to precipitate gold, let gold settle.

(Make up stannous chloride solution) test a portion of solution to see if gold still in solution, if barren, then decant solution (put solution in your container to treat for waste disposal),

Wash the gold powders using Harold’s method for pure gold.(see post on getting gold pure).

Re-refine your gold or save these powders for another re-refining as you accumulate more of these powders later.

Read this through before beginning you and other members can ask questions and check this over as I may have missed some step or forgot some thing.

This is just my suggestion you do not have to follow it, but we must decide on one process and not mix several processes.

Members may have other (better methods) suggestions, you may wish to follow them instead.

Members may give suggestions to improve this then we may need to tweak this process.


----------



## qst42know

What happened to numbering your questions so those that wish to help can? 

It was making it easier to help.

Quoting full posts of other members just makes maters worse. Trying to find where you are stuck among that many more paragraphs takes a great deal more time and effort.

I know you are anxious to get your gold and want to forge ahead as fast as you can but please be patient. 

This is a spare time thing for many of us, at times there is precious little to go around.

While waiting you could use the search function, "Lazersteve" covers "black powder from the cell" better than any of us.

If you use those terms in quotes above in your search you will find the entire process stepwise covered several times.


----------



## Oneal58

Thanks Geo for your post. I now have a clear understanding of the direction I need to go in and the steps I need to take. I am going to get started in a few minutes. I will keep posting just to let everyone know how it's going. Thank you so much for your post, it is appreciated. 
Thanks, Oneal



Geo said:


> In that case follow the directions i listed above with rinsing the foils and powder till the rinse water is clear. If you feel there is more tin in the powder and want to try and remove it before AR process you will need to incinerate your material first,but personally in my opinion i wouldnt think theres enough tin to effect the outcome of your AR process and besides, you will wash the final product with hot hcl acid before you melt anyway. Theres no real need to dry the material as long as all the base metal is removed,decant as close as you can get without pouring off the foils or powder and proceed with AR in the same flask. Dr Poe has posted on colloidal gold and may be able to tell you more about that subject. What i do know is you can save the purple wash water and evaporate all the water till it dries completely,im not sure how much gold could be in the purple water or even if its worth trying to reclaim. My guess would be somewhere in the millionths of a gram category but after the water dries it can be redissolved or maybe even condensed down and stored until when/if you get more it can be added to make it worth processing.


----------



## kadriver

Butcher:

Excellent post. I am going to print it out and use it to process the gold foils and purple mud at my shop.

I will let you know how it turned out.

I am going to make photos and post them here later on. 

Thank you!

kadriver


----------



## Oneal58

Hi qst42know, thank you for your post. I don't understand? 
*Question 1*-Doesn't the site put the post of the previous member's post up automatically when I reply back to them? 
*Question 2*- Is there a way to reply to each individual person that helps me but does not bring their post along with my post again? 
*Question 3*-Do I just click on (POST A REPLY) instead of "Quote" at the bottom right of the window? Will this save bringing the previous person's post forward with mine?
*Question 4*-If none of these questions will do the job, can you tell me the best way to reply to each person who helps me?
I thought I was numbering my questions but when I look back I see that sometimes I did and sometimes I didn't? Sorry about that, I promise to do a better job with that. I realize everone isn't old like I am and has a full time job. That's why I want to not waste anyone's time here. I cannot ramble on and on when the potential helper has a job to go to early next morning. I realize the sacrifice you guys are putting forward just for the sake of helping people like me. As I said before, it does not go unappreciated and recognized. I surely want to make it as easy as possible for you to help me and not complicate things with the way that I post.
Believe me when I say that I have been where you are and realize what you are saying.
I can remember getting behind an elderly driver when I was a young man. How upset I would get when I would have to slow down for him/her when I was trying to make it to work on time. I said then that the state should pass a law that takes the license of old people when they start driving that slow on the road, there a danger to themselves and everyone around them. 
Just let me say, I have had to eat those words.
Qst42know, I will study the site and see how I can more accomodate the very ones who are trying to help and without them, I would be lost. I will try to do a better job in my postings.
Oneal58 




qst42know said:


> What happened to numbering your questions so those that wish to help can?
> 
> It was making it easier to help.
> 
> Quoting full posts of other members just makes maters worse. Trying to find where you are stuck among that many more paragraphs takes a great deal more time and effort.
> 
> I know you are anxious to get your gold and want to forge ahead as fast as you can but please be patient.
> 
> This is a spare time thing for many of us, at times there is precious little to go around.
> 
> While waiting you could use the search function, "Lazersteve" covers "black powder from the cell" better than any of us.
> 
> If you use those terms in quotes above in your search you will find the entire process stepwise covered several times.


----------



## Oneal58

Butcher thank you for your post, I am going to get busy. I will keep everyone posted on my progress, going to be a busy day. 
Thanks, Oneal58



butcher said:


> Oneal,
> Here are my thoughts:
> 
> Junk jewelry, gold plated jewelry, and gold fill, can have many undesirable metals involved depending on what they were from. Copper base metals common (pewter, lead tin and so on would not be uncommon).
> 
> Your color of the wash water is an indication of some metals that are going to give you headache, it sounds like colloids, probably carbon-ous trash in solution with tin and other undesirable metals.
> 
> (The colloids can be broken with heating and strong acidic solutions (we will not discuss now in detail)
> 
> (The rinse water from nitric rinse add it to the spent nitric solution (after filtering) we will boil this down later concentrating the acid and recovering any traces from it).
> 
> You had sulfate salts with the lead salts so lead would very possibly be in powders (nitric may not have remove lead here).
> 
> This process can be done in one dish keeping powders in the pot removing liquids as needed,
> I use a white corning type casserole dish, on electric hot plate with solid metal cast iron burner.
> 
> You may see some other details in this post to another member: http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=12165
> 
> 
> 
> 
> Powders separated from nitric solution these I would wash rinse and dry.
> 
> Incinerate powders to red hot, (to oxidize base metals like tin, burn off any trash, remove sulfates, nitrates and so on)
> 
> Let cool spray dry powders with mist from water bottle to wet, then add HCl.
> 
> Boil in HCl, (then the add water to dilute) keep HCl-water hot but below a boil, let powders settle well in this hot solution, and then decant hot solution, (this will help to remove tin, lead, trash, any copper you may have and other things you do not want in solution later (some gold colloids may follow these rinses).
> 
> Add water to powders and repeat these very hot water rinses until water solutions we decant are clear.
> 
> (Keep these chloride washes together in jar separate from other waste let them settle we will also concentrate and filter them later to retrieve values they may hold later).
> 
> Now heat to dry powders.
> 
> Re-incinerate the powders red hot, (This will help to remove chlorides that can give us trouble with our next nitric step), Cool.
> 
> Again spray down with mist water bottle, wash sides of pot down (this helps keep fine powder from bubbling and floating away when you pour in acids).
> 
> 
> 
> Add dilute nitric acid (70% HNO3 + H20 50:50 solution), bring to boil, then cool, letting powders settle well, decant solution and then, several hot water washes (decanting only from well settled powders).
> 
> Now add HCl to cover the powders (with little bit of excess), add nitric in very small amount (drops) with med heat (let reaction complete), if all gold has not dissolved, then add a few more drops (let reaction complete) repeat till all gold in solution.
> 
> Now we will eliminate any excess nitric you may have:
> 
> Let solution heat (not too hot but fumes evaporating off), (watch for boil over), (keep eye on solution but your nose out of it), (have wash bottle handy if foaming occurs you can spray it down with mist from water bottle).
> 
> Add a few drops of sulfuric acid, (this will help to remove lead in later steps, and keep from forming salts on evaporations).
> 
> Concentrating solution we want it thick like syrup but do not make crystals or salts, add some HCl to wet again, heat until syrup again, repeat HCL to wet, one more time evaporate to syrup, add water till solution is four times volume, turn off heat cover pot let sit overnight.
> 
> Now silver if any will be in powders with lead if any, (it should be cold enough outside to crystallize these out of solution.
> (We could test for more dissolved silver with a little non-iodine table salt, but since we will be refining this again, I would not mess with that now).
> 
> Decant this gold solution, filtering into a clean vessel; let this settle to see if clear.
> 
> Now you can use precipitant of choice to precipitate gold, let gold settle.
> 
> (Make up stannous chloride solution) test a portion of solution to see if gold still in solution, if barren, then decant solution (put solution in your container to treat for waste disposal),
> 
> Wash the gold powders using Harold’s method for pure gold.(see post on getting gold pure).
> 
> Re-refine your gold or save these powders for another re-refining as you accumulate more of these powders later.
> 
> Read this through before beginning you and other members can ask questions and check this over as I may have missed some step or forgot some thing.
> 
> This is just my suggestion you do not have to follow it, but we must decide on one process and not mix several processes.
> 
> Members may have other (better methods) suggestions, you may wish to follow them instead.
> 
> Members may give suggestions to improve this then we may need to tweak this process.


----------



## qst42know

See Oneal, you just found your own answer. Post Reply and Quote button.

And of course you can answer several members in a single post.

Just give it a break in between, hit enter twice and start a new paragraph.


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## kadriver

Oneal58:

Here is what the filter looked like after drying for 24 hours. I filtered it yesterday pouring all the powders into the filter and leaving the foils in the coffee pot.

When it was wet it was about 1/8 inch thick - light purple mud.

I put the filtered liquid in a large beaker and cemented out the silver, got about 1 to 1.5 troy ounces!

I removed this dry filter and set it in the corningware casserole dish for incineration.

The second picture is the liquid from the second dilute nitric acid treatment. It looked black, but the photos make it look brown.

Notice the difference in color of the brown liquid going into the filter and the blue/green liquid at the bottom of the filter flask (filtrate).


----------



## kadriver

Here is a good shot of the contract in color between the liquid being filtered and the filtered liquid in the bottom of the flask.

I added this clear liquid to the cementation beaker and more silver began to form on the coil of copper wire.


----------



## kadriver

I put all the gold foils and mud into the filter and rinsed good with distilled water.

Then I took the filter out of the funnel and placed it into the corningware casserole dish for incineration.

I put the burner on high and waited for the whole batch to glow red.


----------



## kadriver

Unfortunately, it would not get hot enough so I squirted some lighter fluid on the papers and foils.

The flames completely consumed the papers, and the foils all turned red hot.


----------



## kadriver

I then dumped the incinerated papers and foils into a beaker for a HCl bath.


----------



## kadriver

I then added hydrochloric acid to the incinerated foils and papers. This is where I am with the process right now.

After the bath with HCl, I will settle and decant, then wash with lots of distilled water (tap water probably ok here).

Once thouroughly rinsed, I will add about 150 ml or so hydrochloric acid and heat slowly.

Then I will begin to add nitric acid to the container to form AR. I will add the nitric a little at a time until all the foils and material appears to have been dissolved.

Then I will add some sulfuric acid to precipitate any lead that has made it this far into my AuCl. Then neutralize with urea.

Once nutralized, I will filter and then precipitate the gold and proceed from there as usual.

Thanks - as alway, critical input from the forum is welcomed and appreciated.

kadriver


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## Oneal58

Hi Kadriver, you are a man of many talents, keep doing what you are doing! I got stuck this afternoon, had to go see what was wrong with the lights on a float that's going to be in a parade tomorrow. I didn't get anything done today after I called you. I had to stop everything. I plan to try to start back up on my powders and foils tomorrow. Thanks Kadriver, great post! Show and tell does it every single time. Please keep it up. I learn a ton from these type post you are doing. When you first was getting started you posted like this, I keep going back to them from time to time. I plan to try and do the same thing. I don't know about anyone else but if I can see something done, I pretty much can grasp it. So, again, please keep it up! 
Oneal58


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## goldenchild

Kad,

How is the double burner working out for ya?


----------



## goldsilverpro

kadriver,

In Loewen's book, he uses charcoal starter for incinerating papers. Would be cheaper than using lighter fluid and maybe safer.

Good to see you using a CW Pyroceram dish. They certainly will take a lot of abuse.

Chris


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## Oneal58

Hi Everyone, I haven't had a chance to do anything much for the last couple of days. 
Yesterday before I was called I did go ahead and neutralize my Nitric with Urea, I worked the copper coil until I was called to give a hand to someone. I left the copper coil in the neutralized Nitric overnight, I just got back in the house from checking it?

Question 1- Why has a thick froth formed on top of the neutralized Nitric? 
Question 2- What is this thick froth and what caused it? I have cemented silver nitrate in the bottom of the beaker but have a thick foamy froth on top, several inches thick in a 2000ml beaker. 
Question 3- What do I do with this froth, as far as the correct way to dispose of it?
Question 4- I see that some of it settled back down on top of the cemented silver in the bottom of the beaker? 
Question 5- Did I add too much Urea, I wanted to make sure that I had the Nitric Acid neutralized but I might have put too much? 
Question 5- It has a greenish silver color to it, has it got silver in it?
Question 6-I did have the solution warming when I put the copper coils into the Nitric after neutralizing. Did a hot solution cause this?
I will go get a picture of this and load it, give me a few minutes. 
Thanks for helping,
Oneal


----------



## kadriver

Oneal58:

Looks like too much urea! I had the same problem. 

Dilute the whole batch with distilled water.

Pour half into another 2 liter beaker, then add distilled water to each while stirring.

You only need abot 2 or 3 spoons of urea to do the trick.

It looks like you saturated the solution with it.


----------



## kadriver

goldenchild:

I got that double burner at the thrift store for 8 bucks.

My jaw dropped when I seen it sitting there on the shelf, and I snatched it up. I think it gets hotter than the single burner I was using.

Chris: 

Those corningware dishes seem indestructable. I find those at yardsales and thrift stores and get them for 2 or 3 dollars apiece. Some even come with covers.

They are essential for the home refiner if you ask me!

thanks - kadriver


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## Oneal58

Hi Kadriver,
Question 1- What to do with the silver in the bottom of the beaker? Do I mix it all back up together before dilute?
Question 2- When I do this, if this is the case, will silver settle back to bottom of beaker on it's own?
Question 3- Will Urea stay in solution in cold temps? 
Question 4- Is it best to warm solution again, both of the solutions?
Answer 1- I can finally give an answer here, yes I soaked the Urea to it!



kadriver said:


> Oneal58:
> 
> Looks like too much urea! I had the same problem.
> 
> Dilute the whole batch with distilled water.
> 
> Pour half into another 2 liter beaker, then add distilled water to each while stirring.
> 
> You only need abot 2 or 3 spoons of urea to do the trick.
> 
> It looks like you saturated the solution with it.


----------



## kadriver

kadriver said:


> Question 1- What to do with the silver in the bottom of the beaker? Do I mix it all back up together before dilute?



No, just pour the liquid from the 2 liter that has the froth of urea into another 2 liter container until you have equal amounts of liquid in both. Don't worry about getting all the silver into one container, just concentrate on getting that excess urea dissolved.



Oneal58 said:


> Question 2- When I do this, if this is the case, will silver settle back to bottom of beaker on it's own?



Yes, the silver should settle back to the bottom. However, I have seen it float to the top from time to time so don't be alarmed if this happens (floats). Floating silver usually means too much nitric acid causing gas as the cemented silver redissolves. But I don't think you will have a problem with too much nitric acid with all that urea in there!

Also, please consider that some nitric acid is required to cement the silver. With this much urea, you may have to add a couple (2 or 3) drops of nitric acid to make the silver cement out. 

You will have to experiment with this, maybe put some of the blue solution in a small 100 ml container and put a piece of copper in it and watch it for a while. Add a drop or two of nitric acid to see if there is any change to cementation action. Then adjust the big batch according to the results you get on the 100 ml sample. Maybe none will be needed as all the silver is already cemented out!



Oneal58 said:


> Question 3- Will Urea stay in solution in cold temps?



Yes, but I have seen it precipitate out of solution if it is highly saturated. But this observation was on a batch of gold I was doing, I have not seen it do this with silver processing.

I am not sure, but I think the urea will wash out when you rinse the silver with hot water. I put all my silver into a buchner filter with vac assist. I then pour boiling distilled water through it until it runs clear. Then I take a sample of the hot water out of the filter flask and add a few drops of HCl. If it stays clear, then I know the silver is clean. But if it clouds up due to silver chloride, then I know more washing is needed.

If the urea decides to show back up in your solution, then just add some hot distilled water and it will quickly re-dissolve.



Oneal58 said:


> Question 4- Is it best to warm solution again, both of the solutions?



In my experience, warm solutions tend to keep chemicals dissolved more readily than a cold solution.

I did the same exact thing that you did with this batch. I over did it with the urea trying to kill the nitric acid. I solved the problem by adding warm distilled water - all the urea dissolved.

Here is a picture of the silver that I cemented out of the gold filled scrap batch. I was surprised to see this much silver, probably about 3/4 to 1 troy ounce (estimated).

Hope this helps - kadriver


----------



## kadriver

Now back to the process of the gold filled scrap:

Here is what the foils and mud looked like after taking a bath in hot Hydrochloric acid, and then settling over night.


----------



## kadriver

Next, I poured off the green liquid being careful not to let any foils or mud pour off into the receiving beaker.


----------



## kadriver

I then prepared some boiling distilled water and added it to the foils, htere was still a little hydrochloric acid in the with the foils as I could not pour it all out with out losing some of the black powder.


----------



## kadriver

I let the whole thing settle for a couple hours, then poured off the cloudy liquid and added more boiling distilled water. I did this over and over all day and into this evening.


----------



## kadriver

Oh yes, I did test both solutions with stannous chloride with negative results.


----------



## kadriver

Finally, on the about the sixth washing with hot distilled water, the batch settled quickly and relatively clear.


----------



## kadriver

there was some settling of powder of some sort in the receiving container. I will process this later on to see if it is of value.


----------



## kadriver

Now that I concluded that the foils and mud were somewhat clean, I added about 100 ml full strength hydrochloric acid.


----------



## kadriver

I then placed the beaker with the foils and mud inside a casserole dish with the heat off. Then I added small amounts (about 2 ml) of nitric acid to form aqua regia. It took about 4 droppers of 2 ml each to completely dissolve the gold foils and mud.


----------



## kadriver

Here is the reaction in progress - the solution is green in color, but yellow around the edges. It took about 8 ml of nitric acid to dissolve all the gold foils and mud. 

 EDIT  I added low heat to aid the reaction.  EDIT


----------



## kadriver

I then added a few drops of concentrated sulfuric acid (about 4 or 5) to precipitate out any lead that remained in the solution.


----------



## kadriver

Here is a view of the dissolved gold from the bottom of the beaker.


----------



## kadriver

Here I am using urea to destroy nitric acid so the solution will no longer dissolve gold.

I have never used the treatment recommended by Hoke to get the nitrc acid out. She has a process where sulfurcic acid is added to prevent spattering and crystal formation. The solution is heated to a syrup, then re-wetted with hydrochloric to drive off the unused nitric in the solution. The sulfuric also removes lead.

Using urea seems much simpler and easier than going through the evaporation process - especially considering that the solution could start to spatter!

If someone can explain the reason and or advantage for evaporation, then I would be interested in hearing about it.


----------



## kadriver

I will let this settle over night. I sit it sideways in a bowl. This will cause the solids to settle and allow me to pour it off without having the settled solids bloom into the settled liquid as I pour it into the filter.

I cover the opening to the beaker with dampened paper towel to prevent foreign material from getting into my gold solution.


----------



## kadriver

Tomorrow I will filter the solution and use stump out to drop the gold.

I expect to get about 4 grams of pure gold from this batch - we will see.

kadriver


----------



## Geo

Kadriver

do you complete the refining of these small batches at the end of this process or do you stockpile your AuCl for a bigger drop at one time?


----------



## kadriver

Geo:

I usually go ahead and drop the gold and make a button.

Something about having that piece of gold in my hand.

Plus, When I started, I estimate the yield in terms of pure gold from the amount of gold filled scrap I am processing.

I like to weigh the finished button to see how close I can got to the estimate.

I use this ratio (from lazersteve's DVD) .025g pure gold per every 100g gold filled scrap.

With this batch I started with 230g gold filled scrap. So I should expect to get
2.5g + 2.5g + (.3 X 2.5g) = 5.75 grams pure gold.

I am somewhat sloppy and inexperienced with my refining of gold filled scrap. Plus I tend to be impatient. With these variables factored in I am expecting a buttom of gold that weighs about 4 grams.

Processing gold filled scrap is a rare treat for me. I think it took three months or so to accumulate the 230 grams for this batch.

kadriver


----------



## butcher

I have never added urea to a silver nitrate solution.
I do not under stand why you guys would do that?
The silver would precipitate just fine without it.
If you had excess nitric it would just dissolve a little more copper to replace the silver.
Or you could add more silver to use up the nitric.

Even better to use only the nitric you need to dissolve silver with heat (leaving some silver for the next batch, or after you have just a tiny amount of silver decant the silver nitrate solution and finish the small amount of silver with fresh dilute HNO3, that way if you use excess on it a little heat can drive it off.

Oneal, it looks to me your blue foam is copper carbonate, from the CO2 gas the urea makes, the copper carbonate and it will not be very soluble, the nitric Kadriver suggests adding may help dissolve it, but to me that is a waste of nitric and urea fertilizer,
I would use the urea on the grass and keep it out of your lab, actually there are some dangerous chemistry compounds that can form when you mix urea and nitric acid, they can also form ammonia in the solution, now you can have another dangerous compound’s with than ammonia and silver mixed with urea nitrate, (I do not know all of the chemistry, as from reading about it can get really complex)(but from what I have read I sure would not want to make up something that would blow my face off or worse) my suggestion get rid of the urea there is no need for it.

Kadriver I notice you keep moving you metals around from one container to another (pouring to decant solutions),

I run almost a whole process in one container like the casserole dish on the hotplate almost from beginning to end, it stays on the hotplate almost the whole process, 

Here is example of some type of process I may run:
I may incinerate, wash, decant, dissolve metals in acid like nitric, decant, rinse, decant, dry, incinerate, wash, add another acid like HCL to dissolve metals, decant, rinse, neutralize, decant, rinse, dry, incinerate, rinse,

(Now they may come off the hotplate and out of dish this is the only time the dish came off the hotplate or powder removed from the dish) I may remove powders, and screen them through funnel with Nylon type screen into a jar (large material in funnel may go into a jar to be processed later, or discarded depending what it was),

And then fine metal powder goes back into casserole dish) to finish the process on the hot plate, then I may add an acid to dissolve values, decant solution, rinse, and may still have other values to process in the dish.

Point is it stays in the pot the most of process.

I normally do not pour solutions to decant them, I use a suction bulb (it looks like a large plastic syringe with a green bulb attached (think turkey baster suction bulb) they are very chemical resistant and hold up well to all the acids I use, it takes a little while but I can decant a five gallon bucket with this tool when I want to, (it is also a good tool to start suction on a cipher hoses with), another tool I use to decant with is the plastic pipette, you can get down to the last drop without picking up powders,(a trick I use is cut the bulb off a pipette and stick its tube onto my larger suction bulb, now I can reach further down a jar, and have a small opening on the end to control how fast the liquid suck out (so as not to move liquid in jar to disturb things, or get larger volume than pipette could alone or reach the last drop way down in the bottom of jar.

Some other handy tools in my lab, fiberglass stirring rod, glass stir rod, long handle plastic spoon, large long handle, and small plastic tweezers, a piece old Pyrex boiler sight glass (to crush powder like mortar and pestle about 1 inch thick and 2inch wide 8 inches long, stainless steel crusher bar, well most any other thing you can find in the kitchen, or at a second hand store, Pyrex coffee pots, crock pots, blender, coffee mug warmers, wine separator funnels, battery jars, stainless steel pans, pickle jars, canning jars, well I could go on and on.

Another thing to consider my hot plate has a solid cast iron burner with wire heating coil inside, so my dish heats evenly, and holds up well with hot plate on high and propane torch incinerating powders from above.
I would be a little worried about putting the dish directly on the coil type burner like your using, I would probably put a flat steel metal plate between coil and dish. I really do not know if this would give you trouble.

The best way to eliminate nitric from Aqua Regia, is not to add it in excess to begin with using only the exact amount needed to oxidize the gold with no excess.


Evaporation of nitric from Aqua Regia is easy, but it is one process you should also learn when you have to keep an eye on it and when you can relax and let the process work while your not watching it.
Dilute solutions will mostly vapor of water.
Lets look at nitric and water alone for a second, a dilute nitric solution will vapor off mostly water, the nitric acid in solution will concentrate (up to a point) up till its azeotropic point, for nitric acid that is 68% in solution (the highest concentration you could achieve for nitric acid by this method), then the acid will come off as vapors (68% acidic vapor fumes) until the nitric was gone from the vessel.
Ok now lets look at just HCl and water, very similar a very dilute HCl will vapor off mostly water, the acid will concentrate to its azeotropic point, at this point around 20 something percent (bad memory) at this concentration the acid will not get any higher and now the fumes will vapor off 20 sum percent HCl.
Also the boiling points of these acids change with concentration, (similar to how pure water and salt water have very different boiling points)
Now Aqua Regia, evaporating a dilute solution, water would be the first to vapor off (little acid fumes)(and gases created in reaction), then mostly nitric fumes, then HCl fumes, 
Now Aqua Regia is a bit more complex than a single acid and water, and there are several chemical reactions going on inside (several gases being formed, we also have metals reacting with these chemicals, so it is more complex than one acid in water).
When we first start evaporating we are concentrating these acids vapors of water and the gases formed escape, but once these acids and metal salts concentrate (the fumes begin to contain more of the acid, (also the boiling points change), and the acid solution may suddenly boil over at a certain point even though you have not raised the temperature, then after this acid has mostly been eliminated the solutions boiling point may change again as mostly just one remaining acid is left with the metals salts dissolved.

What I am trying to say, keep temperature below boiling point, you want it to evaporate not boil (fumes will come off below boil) (think how the sun can evaporate water from a pool), (the sun does not need to boil the water), this slow evaporation will remove fumes as dilute acid mostly water as the solution concentrates the acids azeotrope and then more nitric (NOXX fumes), will be in gases.
Take note here:
When solution gets to a certain concentration you will see tiny bubbles form around edge of pot, is a sign that you may get a boil over, even though you did not change the temperature of the solution evaporating,(quick turn down the heat)( this is where nitric will start boiling off violently seems like it is trying to come out all at once) (boil over and loose your gold), by watching closely after acid concentrates and turning down heat here you will prevent that, after a little bit (gases escape the heat can be turned up again (you can relax you passed what I call the nitric boil over point).

Points to remember slow evaporation do not boil.
Do not breath fumes.
When starts to concentrate watch closely for small bubbles (they are subtle small bubbles), lower heat until reaction stops (reacting),

(A water mist spray bottle is always handy when most any type of solution tries to boil over, the water sprays down bubbles, cools and dilutes so gases dissolve so keep a mist water spray bottle handy).
Concentrate to thick syrup but not to salts (or baking gold salts to vessel (here is where Hoke recommended few drops of sulfuric acid in solution, that would help to prevent salts from forming so easily and also help some to rid nitric),
Add just a little HCl (not too much your just getting the solution diluted some and (keeping wet from forming salts with more heating, and driving off some remaining NOXX gases (nitric fumes), I repeat this three times. the last time I dilute four time volume with water, let sit overnight or longer for silver chloride to precipitate.

Throw that urea in the yard your grass and gold will be better for it.

Ok I am tired and flapped my jaws enough, I have not had much sleep so I do not even know if any of this makes any sense or not. Good night.


----------



## kadriver

Butcher, I just logged on to check the forum. I am leaving town for a day, so my gold is just sitting there in solution until I get back.

I will read your detailed post and try to answer questions you have about the process I use.

Thank you for your interest and your help!

When I get back I will take more photos of filtering and dropping, melt etc.

See you then!

kadriver


----------



## butcher

I am trying to post picture, of asepto bulb syringe, and pippet.





edit: wow it worked, now if I can remember the instruction my buddy gave on how to do this.


----------



## butcher

Kadriver, I forgot to mention Harolds trick for helping to rid nitric.

here is a post he made:

"By the way, when you evaporate, there's a little trick that can save considerable time, and assure that you consume any free nitric. I used to add a button of pure gold to my solutions when I started the evaporation process. So long as you have free HCl present, it will consume the free nitric by dissolving a portion, or all, of the button. By weighing the added button before it is introduced to the solution, you can determine how much gold was consumed, so you can make determinations of yields of the starting materials. "

Harold


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## Oneal58

You have got eyes watching you Kadriver! 8)


----------



## Oneal58

Hi Butcher, boy have I been going at it the wrong way! I have been going from container to container, filtering and filtering again and again, now I barely have any of the gold powder from the 5 days of running the sulphuric cell left. I think I have it all locked up in saved filters, I hope. I should have been asking more questions but thought I could make my way through the process without having to bother anyone again.
The first thing I am going to do tomorrow is go get me a big syringe and some hose, maybe 2 and decant that way from now on. Stay with one container, Why wasn't I thinking? I have read this somewhere already but I just got it. :shock: 
As fine as those gold particles are when they come out of the sulphuric cell, they must be just the right size to fit into the holes in the filters I am using. Each time I filtered I would lose gold to the filters and I could not wash the gold back out. 
*Question 1-What brand filters do you use?*

Oh Well, Live and Learn, One thing for sure, hard lesson learned, don't be ashamed to ask questions. I am seeing more clearly now. 
Hopefully, I am going to make my first melt tomorrow. 
BY THE WAY! I found out what happened to a lot of my gold from the sulphuric cell run. (TAKE A LOOK AT WHAT I FOUND BELOW!)I was dissapointed on the (returns) after so much work when I filtered the sulphuric? I opened the cabinet that I have the diluted sulphuric from the cell stored in, that I filtered twice! Look what I found laying in the bottom of the jars! One thing for sure, gold particulate will not settle in full strength sulphuric in 4 days. This was diluted by 2/3rds and still didn't settle out in 2 days completely! But Syringe and hose from now on for me anymore!
P.S.
*Question 2- What's the best way to clean a crucible,* which could very possibly have some gold still locked up in the Borax coating? I use this crucible to incinerate gold filled items only (whole jewelry pieces), before nitric treatment, nothing else.
Thanks Butcher, your last post answered my questions I had.
Oneal58


----------



## jimmydolittle

What kind of torch are you using? Looks like some of the powder did not melt.


----------



## butcher

Oneal, 
We call that a melting dish the crucible is taller and looks like a cup,
You can use a little bit of soda ash and borax, I would slowly bring your melting dish up to temperature, sprinkle on some borax (20 mule team soapwill work), use torch to try and get the metal to pool into one ball at the bottom of dish,(pushing it around with torch flame). And then add a sprinkle of soda ash (sodium carbonate), (you may find sodium carbonate in powdered automatic dishwasher soaps), the soda ash will make flux more fluid when hot and easier to poor off, it can help clean dish, but it also corrodes off a layer of dish into the flux. a pair of tonges or plyers to lift and pour dish.
When heating or melting in your dish, take note that what you have your dish setting on can act as a heat sink and suck your heat from your melt (especially if the torch your using is just barely hot enough for the job).

you could make a strong wire stand to sit the dish in (elevated off of the heatsink), or you could make a strong wire dish holder, where you could hold melting dish in your hand while heating with torch in other hand (while cleaning the dish).
Just keep your hands off of the red hot dish, and torch flames, trust me its hot you do not need to touch it to find out. :lol:


----------



## kadriver

Oneal58 said:


> they must be just the right size to fit into the holes in the filters I am using. Each time I filtered I would lose gold to the filters and I could not wash the gold back out.



Oneal58 - save the filters that have gold trapped in then. You can get it out in one of two ways, the first one is the funnest:

1) fold the filter paper that you suspect containes gold a couple of times. Then, carefully tear it into pieces and place the pieces in a relatively clean melt dish. Cover the torn up pieces of filter paper with borax - about a tablespoon or more. Then, with the torch on very low flame, melt the borax onto the pieces of filter paper in the melt dish. Keep adding borax as you go and the ashes will cling to the molten borax and not fly out of the dish. As the ashes begin to disintegrate add some more borax until all the ashes are gone - they just kind of dissappear. The heat will have completely burned off all the paper and ashes. If there was gold in the filter paper, then you will see some tiny balls of gold suspended in the molten borax. Use your flame to push all these tiny balls into one big ball. Turn off your torch and let the gold ball harden slightly. Then, before the borax solidifys, grab the ball of gold with tweezers and dunk it into some cold water. Squeeze the gold ball with pliers to remove the borax glass.

OR

2) When you do another batch of gold later on, at the point where you will be dissolving your gold in aqua regia, just add the gold laden filter paper in with the other gold you will be dissolving. The filter paper is no match for aqua regia and it will completely disintegrate. You can then filter out the disintegrated filter paper when you filter the rest of the AuCl. Any gold in the filter paper will dissolve in the AR and the disintegrated filter paper will get trapped in the filter funnel. The draw back is that you may have other, undesireable material in the filter paper that could get into your final AuCl solution. But here is the beauty of a second refining - the undesireable metals and material will be removed at the second refining - if you refine it twice.

I just did a couple of old filter papers and got about 1.3 grams of gold out of them using method 1 above.

Many people on this forum would never allow gold to get into the filter paper. Instead most will want to allow the solution to settle completely, then pour off the clear liquid thus retaining ALL values. This is the preferred method. There is no good reason to put gold into your filter paper if you can avoid it.

The reason I had gold in filter papers was because I had a deadline to meet. The last couple of bars I refined and sent in were rushed because I called and locked in the spot price before I had the refined gold bar ready to go!

This caused me to rush and I had to filter the liquid after dropping the gold. Some of the gold was still suspended in the liquid.

Some of the gold powder was so fine that it made it through the filter paper and into the filter flask. When that happened I ran the filtered liquid back through THE SAME filter paper for a second pass. 

To do this, I move the buchner funnel with the filter paper in it to a second filter flask and attach the vacuum line. I can then pour the liquid from the first filter flask back through the same filter paper that is now sitting on top of the second filter flask. This second pass through the filter paper usually does the trick and all traces of gold (that I can see) are trapped in the filter paper and ready for treatment by either method 1 or 2 described above.

kadriver


----------



## Acid_Bath76

Oneal58 said:


> Thanks Geo,
> I will put this to use, I really appreciate your response. I am printing all my replies and making a notebook of the replies for references. Thanks,
> Oneal58
> 
> 
> 
> Geo said:
> 
> 
> 
> 
> 
> butcher said:
> 
> 
> 
> Making ferrous sulfate (FeSO4), also called copperas or iron sulfate.
> 
> Copperas is green in solution or in crystal form.
> 
> Ferrous sulfate is good to use to precipitate gold from acidic solutions.
> 2AuCl3 + 6FeSO4 à 2Au (s) + 2Fe2(SO4)3 +Fe2Cl4
> 
> Iron sulfate will also precipitate platinum from boiling hot solution if pH 7.
> 
> FeSo4 crystal can be used to detect dissolved gold in solutions in the spot plate,
> This is useful also if the gold is in solution with another precious metal, we can use the copperas crystal to test for gold in one dish of spot plate (brown ring) this precipitates the gold and remaining solution moved to another dish in spot plate and tested for other precious metal.
> 
> Copperas crystals (green) these crystals will oxidize easily if not stored properly, dry (acid low) and exposed to air (turning brown) the brown crystals will not precipitate gold, most all copperas I have found in garden centers has oxidized and is useless for our needs here.
> 
> The green copperas crystals, when made should be kept fresh in storing, I will keep them wet, few drops of sulfuric acid to keep them acidic, store in air tight plastic container (screw on plastic lid with seal an old stump remover bottle is what I use), they have a very long shelf life this way.
> 
> It is as easy to make a large batch of ferrous sulfate, as it is to make a small batch of copperas.
> 
> You need as pure iron as you can get (not steel), soft Iron laminates from old transformers, or electric motors, is what I use.
> 
> An old transformer cut iron laminate welds (hacksaw or angle grinder Etcetera), remove copper winding an save (to rewind another transformer, old motor, use as wire, or throw in your copper scrap metal pile), separate the iron laminates, cut into small pieces (with tin snip’s), use torch to burn off shellac and oils, add this Iron to dilute sulfuric acid (10% H2SO4), (the dilute acid is best as iron can passivate (not dissolve) in strong sulfuric acid), you can dilute battery acid (one part 32% battery acid to two parts water), or dilute the drain cleaner in water.
> 
> :shock: Always add the concentrated sulfuric acid to water slowly watching the temperature rise from reaction).
> Never add water to concentrated sulfuric acid it will boil out and splash all over you burning you severely or blinding you}
> 
> The iron will dissolve slowly in cold solution, heating will speed the reaction, you can boil this solution of iron metal and dilute sulfuric acid because the sulfuric acid has such a high boiling point so gases evolved are mainly just water in fumes.
> I use a Pyrex Mr. coffee pot, or white corning ware casserole dish on solid iron metal burner electric hot plate.
> 
> After as much iron as will dissolve (dissolves into the concentrating acid) lower temperature and pour this green solution into another jar, letting un-dissolved iron metal and carbon settle well.
> 
> Filter solution back into evaporating dish and boil down to crystals, when you get a few inches of crystals cool solution somewhat then pour into a clean jar let cool more and crystals settle, decant liquid back into boiling vessel and make more crystals, this concentrated solution can be used also.
> 
> 
> 
> 
> i dont mind being corrected and really appreciate someone taking the time to point out any errors i may make in my comments as im still learning.the laminates your referring to can not be pure iron or even close to it.pure iron is a crystal and does not bend easily without breaking such as castiron.the soft laminates from transformers is an alloy that can be searched on the web.(i did) so i wouldnt look foolish saying this but can contain as little as 85% iron with Ni or Co these can be bent double and be flexed many times before breaking,iron will not stand up to these stresses.
> 
> the crystals i spoke of look more like aqua-marine but according to wiki copperas crystals are green if pure.
> 
> Click to expand...
Click to expand...


I do the same thing. Print out formulas and topics that I like to reference often. The last thing I want to do is bring my laptop or $80 book to the work space and accidentally spill something on it. $2 binder, $5 package of document protectors, $5 of printer paper: total around $15. Cost of doing something right the first time: priceless.


----------



## kadriver

Butcher, 

Thank you for that tip from Harold. I will find a way to incorporate it into the process that I use.

Here are a couple of photos of some gold beads I recovered from treating gold laden filter papers in a melt dish with low flame and borax. The process I used is a little further back in this post.

They probably have some other material in with them, but I plan to add these to my next batch of karat scrap and refine - then they will be purified!

Thanks for looking.

kadriver


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## kadriver

butcher said:


> I have never added urea to a silver nitrate solution.
> I do not under stand why you guys would do that?
> The silver would precipitate just fine without it.
> If you had excess nitric it would just dissolve a little more copper to replace the silver.
> Or you could add more silver to use up the nitric.



When I process my silver, I used to use 1.22 ml of nitric for every gram of sterling or 925 scrap jewelry that I was going to dissolve.

The silver dissolved quickly and completely with this much nitric acid. But, using 1.22 ml nitric created a problem for me. After all the silver was dissolved there was excess nitric acid in my silver nitrate.

So much so that when I added my copper, the silver nitrate solution would start for bubble and put out poisonous brown fumes. The copper would be eaten away in just a few minutes. Plus the cemented silver looked funny and it would begin to float.

To solve this problem, I added a spoon of urea, sometimes two, and stirred vigorously. There was so mich nitric acid that the container would nearly boil over!

But after I added the urea, the problem was solved. No more brown fumes and the silver cemented out nice and pretty.

I experimented with using just 1 ml as opposed to 1.22 ml of nitric acid to digest my silver. The result was very positive - no more excess nitric acid and no more urea. 

I usually have a few small pieces of silver in the bottom of the container and, like you said, I just add these to my next batch. But just as often the silver will be completely dissolved - especially if the silver was from sterling bowls or candle holders.

I still add a little urea (about 1/2 teaspoon) before I cool and filter the silver nitrate solution. If I get a big reaction, I add a little more until the reaction is still there, but very slight.

I have had the nitric acid be used up so completely that the silver would not cement out when I put the copper in.

When processing gold filled scrap (which these batches are few and far between for me) I use urea to kill excess nitric in the solution from the initial nitric acid treatment. I use 3.55 ml of nitric acid for every gram of gold filled scrap that I process. Got this number from Steve's DVD.

I have only done about four batches in total of gold filled scrap over the year and two or three months that I have been refining. My experience is lacking in this type of refining.

In the future, I may start processing the gold filled items with less nitric acid, and just do several treatments - adding small amoounts of acid then checking to see if all the base metals have dissolved.

By the way, this is the first time I have used hydrochloric acid to treat the gold foils and mud. The reason I have never done HCl treatments in the past - ignorance!

Butcher, you set me straight when you posted the process earlier in this post. I printed it out and used it as a reference to process this batch Thank You!

kadriver


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## kadriver

butcher said:


> another tool I use to decant with is the plastic pipette, you can get down to the last drop without picking up powders,(a trick I use is cut the bulb off a pipette and stick its tube onto my larger suction bulb, now I can reach further down a jar, and have a small opening on the end to control how fast the liquid suck out (so as not to move liquid in jar to disturb things, or get larger volume than pipette could alone or reach the last drop way down in the bottom of jar.



This is an excellent tip. I will have to remeber it the next time I am trying to get the liquid out without disturbing the settled material in the bottom of the container - thanks again.

kadriver


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## kadriver

butcher said:


> Kadriver I notice you keep moving you metals around from one container to another (pouring to decant solutions),



Butcher:

I used a large coffee pot to dissolve the base metals. I think I had nearly 2 liters of nitric acid and distilled water in that coffee pot to do the reaction.

After filtering and incineration, I put the gold mud and foils in that tall beaker to aid in settling after adding the hydrochloric acid. The large coffee pot may have caused me some problems when I tried to remove the hydrochloric acid - that is why I transfered the foils and mud to the tall beaker.

I am still new to this type of refining. I only have limited experience with gold filled scrap. I appreciate all the pointers you can give to help me along.

Thanks - kadriver


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## Oneal58

Hi Butcher, couple of questions, 
I have some old grinding wheels of various sizes and shapes. I have a couple that are round, about the size of the (melting dish). 
*Question 1- Can I take regular (fire bricks) and grind me a place out in the firebrick to sit the melting dish? Will this take away from the total heat applied or help to hold the heat longer?*
I have an Iron stand but it seems that when I take the heat off the melting dish it cools back down really quick and was just wanting to know what you thought of this fire brick idea? 
*Question 2-* Take a look at the picture I loaded of the Stump Out that everyone has told me contains Sodium MetaBisulfite. I pulled the MSDS sheet on this Stump Remover and it contains 100% Potassium Nitrate? Do I have the wrong Stump Out here. I have contacted a friend of mine who is rounding me up some old open transformers. I want to use the MetaBisulfite untill I can make my own Sulfate you have outlined the procedure of above. 
Thanks Butcher,
Oneal58




P.S.
*Question 3*-I also have lots of porcelain pieces left over from my days on the auction block. I have a lot of heavy gold decorated pieces as well. Has anyone ever tried taking the gold off of these pieces? Is there enough there worth messing with? On some of the very high quality pieces such as Minton there is a lot of gold decoration, thick also. Take a look at the pictures below also. Porcelain is the last step in kiln firing temps before turning something into glass. High Quality Porcelain is fired at 2552 degrees F. compared to earthenware which is fired at 2192 degrees F. Why wouldn't one of these Oyster Dishes serve as a melting dish? I have lots of them. Will this porcelain explode or will it take the heat? I guess I could just put the torch on the pieces and exit the building?















butcher said:


> Oneal,
> We call that a melting dish the crucible is taller and looks like a cup,
> You can use a little bit of soda ash and borax, I would slowly bring your melting dish up to temperature, sprinkle on some borax (20 mule team soapwill work), use torch to try and get the metal to pool into one ball at the bottom of dish,(pushing it around with torch flame). And then add a sprinkle of soda ash (sodium carbonate), (you may find sodium carbonate in powdered automatic dishwasher soaps), the soda ash will make flux more fluid when hot and easier to poor off, it can help clean dish, but it also corrodes off a layer of dish into the flux. a pair of tonges or plyers to lift and pour dish.
> When heating or melting in your dish, take note that what you have your dish setting on can act as a heat sink and suck your heat from your melt (especially if the torch your using is just barely hot enough for the job).
> 
> you could make a strong wire stand to sit the dish in (elevated off of the heatsink), or you could make a strong wire dish holder, where you could hold melting dish in your hand while heating with torch in other hand (while cleaning the dish).
> Just keep your hands off of the red hot dish, and torch flames, trust me its hot you do not need to touch it to find out. :lol:


----------



## Oneal58

Hi Jimmydolittle,
I have 2 types of torches, I have the Mapp Gas torch and the acetylene outfit. I tried the acetylene torch on just heating the gold filled items up to red hot to burn off impurities. I haven't got the hang of incinerating the gold filled yet and melted some of it with the acetylene torch. So I use the mapp gas for just incinerating, (cleaning) the gold filled before I put into Nitric. The Mapp Gas torch will get everthing red hot and not melt it, that is what I try to accomplish to clean (burn off the impurities). Some of these old gold filled watch bands are almost full of krud and God knows what else?
I will probably use the acetylene torch when I get more familar with the temperatures required to incinerate and not melt the Gold Filled, it does a much quicker job. 
Thanks jimmydolittle,
Oneal58


jimmydolittle said:


> What kind of torch are you using? Looks like some of the powder did not melt.


----------



## Oneal58

Kadriver, we are watching, watching, watching, keep putting up those pictures. 
Oneal 58


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## Oneal58

Butcher, where did you find that asepto syringe? CVS, Drug Store?
Thanks for all your post and everybodies post. I just don't know what I would have done without you Guys. I really do not think this would have been possible without each and every one of you. 
Thank You, Thank You, Thank You. 
Oneal58


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## philddreamer

"Take a look at the picture I loaded of the Stump Out that everyone has told me contains Sodium MetaBisulfite."

The one in the picture it's not Stump Out by BONIDE. What you have there is 
Stump Remover by SPECTRACIDE, a totally different product.

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=7746&p=71243&hilit=bonide#p71243

Take care!

Phil


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## Oneal58

Thanks Phil, where are you finding the correct Stump Out?


----------



## Oneal58

Thanks Everyone, I just can't say this enough! 
Oneal58


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## kadriver

Oneal58:

The Stump Remover that you have pictured is the incorrect item.

The ONLY place that I have found that sells Stump Out by Bonide is at Home Depot. It is on the shelf with pesticides and other lawn chemicals.

It comes in a one pound white plastic container with a purple lid. Ask the front desk to guide you to it.

The lable says, "Stump Out" by Bonide. 

You can see a picture of the container and label in this video:

http://www.youtube.com/user/sreetips?feature=mhee#p/a/u/0/HNq3Tp99XOE

I have not found it sold anywhere else (but it is probably sold at other stores).

I have not checked walmart - if anyone finds it someplace else, then please let me know.

kadriver


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## kadriver

Here is a photo of the dissolved gold from the gold filled batch. In this photo the solution was allowed to settle overnight.


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## philddreamer

"Thanks Phil, where are you finding the correct Stump Out?"

Home Depot... but try a beer or wine supplies store near you. I found good grade SMB for less than $4.00 per pound @ one close to me.

Phil


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## kadriver

The solution was filtered to remove solids and precipitated lead sulfate. The lead sulfate was precipitated out of the auric chloride (AuCl) solution when I added drops of sulfuric acid just prior to filtering.

The settled liquid was carefully poured into the buchner funnel under vacuum. I poured all the clear liquid in first, then poured in the mud and filtered it last.

I rinsed the filter and none of the mud appears to have made it into the filtered AuCl in the flask.

If it did, then I would have to refilter several times through the same filter paper until the solution was crystal clear.

This is why I have two filter flasks, so I can move the funnel from one flask to the other to refilter the liquid over and over through the same filter paper. 

Goldsilverpro taught me this technique and it works quite well.

The filtered solution appears clear, but it has a green color.

I have had AuCl solutions that were green in the past.

I will just drop the gold as usual using Stump Out (sodium metabisulfite) made by Bonide.

I will post move photos as I get the time to prceeed with this batch.

Thanks for looking, more to follow...

kadriver


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## butcher

Oneal,
Firebrick can be used to make a furnace, or to hold a melting dish.
Note: there are several kinds of firebrick, two types I will mention now,

1. The baked clay type (could come in several colors red white Etc.) used in-home fireplaces (harder and absorb heat and hold heat easily).

2. Then there are very porous fire bricks used as insulation in boilers, furnaces and so on, these are very porous like pumice (volcanic rock full of tiny air bubbles which act as insulator do not absorb or hold heat easily), these bricks (usually white) are easily carved or sawed with hand tools like knife saw Etc.,

Both of these types of bricks have uses, but also when using them to build furnace or small dish furnace you will need to choose the right one for the job intended here for your purpose the second type would serve the purpose.

If you have a couple of dollars, Laser Steve has made some excellent little melting furnaces from two of the second type of fire bricks, carving out the place for melting dish (with space under dish so propane or Mapp gas torch can heat with flame under dish and also keeps the dish from having intimate contact with brick so brick will not act as heat sink and take all your fuel and flame to heat brick, this helps the heat to do its work on metals inside the dish, Laser Steve sold these for about the same price you could buy the bricks for (but he done the work of carving them just for you) It's a great buy from a great guy, while your there maybe order a couple of melting dishes or other supplies you may need,

I miss Steve being on the forum like he used to be we all learn so much from him, (that dirty word (work) has kept him from here as often).


As far as using a ceramic dish or pot for a melting dish (forget that idea) unless you had a furnace that you could control the temperature (raising and lowering at will) the dish would break, also think even then the glaze is like flux, or flux and metal flux slag can act like glaze, the clay in dish used may absorb your metals or they may chemically react with your metals in the melt.

The melting dishes or crucibles we use for melting our values, clay mixes with properties needed not to give you the troubles mentioned, actually these dishes and crucibles are cheap especially if you consider how they are made and the value you can have in the melts we do here.
Incinerations of dirty materials you could use stainless steel, or the white corning ware or vision ware dish, 

Not recommended, you can even melt in a wood block (I have used pine and oak) thick so as not to burn through the wood, I have done this with gold and dirty copper metals (the charcoal formed also helps to reduce the copper to metals so heat does not oxidize it).
I have also used a fire brick to melt metal in (dish shape carved in it, or used a stack of sheetrock blocks (it would absorb silver in melt into sulfates so silver is lost into sheet rock), although I may used these for very dirty melts, I have also made some of my own melting dishes from various clays and refractory, I am not recommending any of these methods in this paragraph as they have there own sets of problems, and each has a chemistry involved when using them in the melt, and if you do not understand that you can be losing value by using these.

Gold on glass and ceramics, is a source of gold, using HCl/Bleach to remove gold from them, the gold looks like more on the dish than is actually there, but is easily removed and recovered, I would not do just a couple of dishes, as unless you break the dishes the container or bucket used to leach the gold, and amount of acid you need to soak the dish in is large (plastic dish pan, large glass bowl, or plastic 5 gallon bucket), and you do not want to use a lot of acid for very little gold to dissolve in it (save up a pile of dishes before stripping them).


Torches: with acetylene / oxygen set you have a choice of tip sizes and types, as well as fuel/oxygen settings, using these for there purpose needed is important (whether heating welding melting and so on, also what part of the flame and distance to work is also important in the job your doing.


----------



## Oneal58

Boy, the things you can learn here. Thanks Everyone, Butcher I am going to pick me up one of those firebrick furnaces from Steve. And a few more things I need also, as you said, great prices. By the time I drive 30 miles to town to buy something, it will cost me less than I can pick it up on Steve's Site. Sounds as though you can save a good amount of fuel with the furnace also. 
I am currently going back through Hoke's Book page by page by page. Doing the test, following her line by line and doing as she says. This time I am taking notes but I believe my notes are going to end up being larger than her entire book? I have already filled up 2 notebooks, no kidding and am on my 3rd. I guess it's because as I get and understand what she says, I put things in my own words (staying with my train of thought) which always ends up being longer than her's? 
Thanks to Everyone, I am going to finish up Hoke's again before I start back up. I
I am not going anywhere, I will be here, just observing more. When I ask questions again, hopefully they will not be something I should already know out of Hoke's Book. Saves everyone a lot of typing and time, which gets more valueable day by day. 
Thanks Everyone,
P.S.
Kadriver, thank you for taking the time to do what you are doing! 
Oneal58


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## butcher

Oneal,
Very wise choice, (I am glad your light is coming on), reading Hokes book and doing the experiments will give you an insight you’re missing now.

As far as note book I have several note books written, problem is as you learn these books need rewritten (may I suggest a notebook with hole punched paper in binder, so pages can be removed, rewritten, rearranged. added later), and another problem is sometime there seems a feller does not have the time to add all of the useful info to his notebook from all of the information everybody share here on the forum, also my collection of data (paperwork) is filling up my living room, if this keeps up they will have me on a TV show (the data hoarder).


----------



## Oneal58

Butcher, I really get it. 8) I have even started leaving the back of each page blank now so I can go back and add information later. But the binder idea is a great one, I am just a little too far along to start that now with where I am at. I will start after I fill this 3rd notebook up I am on now. Then that's the way I will go. It's a shame I didn't get this information a week or so ago. But I do have the empty back page that will help some when I run across variations to the text.

I stole my wifes turkey baster, didn't even know she had one. It works great! No more filtering for me unless it is a have to. It works like a charm! 
*Question1*- Will the hard plastic White Chlorox Jugs hold up to the nitric and hydrochloric, I don't think it would the sulphuric from the way it burned through the toilet tissue plug earlier? If they will work what's the (best method) to neutralize the chlorine that is very hard to get completely out of these jugs? Seems almost impossible to wash completely out of the jugs with plan water, still smell after 5 or 6 hard shaking washing's? *Sodium Bisulfite* seems to be the answer, but how much to a gallon jug already washed with water several times?
*Question 2*- I have plenty of 1 quart glass canning jars. But just a few of the quart sizes. These have the porcelain inserts with the zinc tops. If they have the porcelain/glass inserts in the tops of the lids will they be OK to store acids in?
*Question 3*- Which acid will I end up with the most volume of. I have 1 large crock with a lid I would like to use for it. It is glazed inside and outside. So far, it would seem I will end up with the most diluted/neutralized Nitric Acid. Is this correct? I hope not to let any of the acids build up and get too far ahead of me? I am just thinking that I will save the Nitric up and recover what (PM's) that's in there after dropping the silver. But those recoveries will come a little later, after more experience and knowledge. 
Thanks Butcher,
Oneal


----------



## butcher

The solutions saved, consider what they are and choose appropriate container.
I will NOT normally save solutions that are NOT loaded with metals (these metal salt solutions I will save in plastic jugs (old HCl jugs, sulfuric jugs, old Clorox jugs,) or plastic 5 gallon drums (chemicals came in) glass gallon jugs like apple juice jugs with finger hole, change metal lid to plastic. basically all my lids or covers are plastic I save old food jars or pickle jars, and plastic lids. Trying to use the jug the acid came in that made this salt solution as much as possible.

Some solutions like nitric the storage vessel may need to breath somewhat (as temperature changes or acids decompose from light or time) point here some acids like nitric you may need a lid that allows some pressure to release (most lids will normally) corks (or whittled wood plug) wrapped in Teflon tape can also be used if not permanent.

Copper nitrate or copper chloride solution can also be stored in old HCl jug.

If your concerned about the small amount of bleach after washing out you old bleach jug, you could pour in a tiny amount dilute ammonia and wash out the ammonium chloride.
or just let sit in sun open to air to dry (next summer :lol: ), personally I would not worry about the residue in a gallon of spent solutions.

You will find (like you did with your sulfuric cell washes that powders will settle out of spent solutions after they sit for a long period of time), I usually save these powders as they may contain traces of values.

Treat solutions for waste as needed, save for reuse as needed,

I do not know if this helped with your question.

Try and find the syringe bulb in the picture above, that and pipettes I have found them at drug store, but you could order them also (not sure where), they will work better than the turkey baster, fluids won't drip back into solution as easily (tips are different) and bulbs will hold up better to solutions we use. (I do not spend much money on lab ware, using mostly kitchenware or jars, but a couple of dollars on these suction tools are worth it to me).


----------



## Harold_V

butcher said:


> Try and find the syringe bulb in the picture above, that and pipettes I have found them at drug store, but you could order them also (not sure where), they will work better than the turkey baster, fluids won't drip back into solution as easily (tips are different) and bulbs will hold up better to solutions we use.


Yep! A turkey baster is pretty much worthless for lab work. 
I used to use irrigation syringes, purchased from medical supply houses. They're perfect for that little shot of water that is often needed. They're not expensive and have a terrific lifespan, even used around acids. I do not recommend they be used _to dispense _acid, however. 

Harold


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## butcher

Hello Harold,
I have used the asepto bulb syringe, and pipette (pictured above), to siphon, transfer, dispense acids, and other solutions, including waste solutions, (except fresh nitric acid), without problems, one will last almost a year before bulb starts to determinate (then its purpose is waste transfer tool), I will even transfer, or siphon nitrate salt solutions (with some free nitric), and gold chloride solutions from aqua regia, many times these solutions are boiling hot also. Keeping the bulb from acid as much as possible, and rinsing bulb with spray bottle after use extends its life, I do not know what plastic these bulbs are made from but they hold up very well. A Very handy tool.


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## Oneal58

Thanks Butcher, Harold. I have a bag of pippets I bought a while back. They are thin plastic, I don't expect to get too much out of them before there shot. I got to go to town today. I am going to try and find one of those asepto syringes. I found a medical supply house and am going to check out what they have. 
*Question1*- I have large stainless steel funnels and pans and pots by the dozens. My oldest sister works with the school system here. She takes care of getting the food for the cafeterias in the schools in this district. So, I get all the used cooking oil to burn in my diesel truck. I get all the throw away stainless steel when it gets damaged a little, large cans that the food comes in for the children and such things as that. I have read that using Stainless Steel will cause you to pick up trace amounts of other metals (nickel, possibly tin) if used while processing. But for storage, how about that? All these large pots, 3-5 gallon pots have loose fitting lids, the lids just sit on top the pots? 
Question 2- One last question, how about cold temperatures. Should I always keep the stored acids above freezing? 
Thanks Fellows,
Oneal


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## butcher

Stainless steel should not be used to store you solutions.

Glass, and appropriate plastic container can be used for storage of used solutions.
Acids glass will be usually better,(if I buy an some types of acids in plastic jugs (these jugs are usually not suited for long term storage) I will move to glass containers), venting of acids must also be considered in different environments or concentrations.
http://www.google.com/#sclient=psy-ab&hl=en&site=&source=hp&q=storage+of+cemicals+and+used+solution%27s&rlz=1R2RNQN_enUS457&psj=1&oq=storage+of+cemicals+and+used+solution%27s&aq=f&aqi=&aql=&gs_sm=e&gs_upl=2407l38907l0l43422l41l41l0l24l0l0l953l12672l5-5.12l17l0&bav=on.2,or.r_gc.r_pw.,cf.osb&fp=497a0dbec56255c7&biw=590&bih=328

Temperature can be very important to storage, usually cold temperatures are not a problem for acids or used solutions (except in extreme cold environments), heat on the other hand can deteriorate acids, as well as light, exposure to air, or other chemicals.
Acids can also build pressure in containers from formed gases (from decomposition) from heat light Etc. depending on acid type, (venting must be considered).

Study the acids you use, understand how to use, store, handle, safety precautions, their properties and reactions to metals, and so on.


Acids can act different on metals depending on concentration, some types of concentrated metals will passivate some types of metals, but this same acid diluted will attack that metal (so the same metal container you may have bought the acid in may not work to store the dilute acid in)

Generally you can store a metal salt solution (metal + acid = salt solution of that metal) in the container the acid came in.
But this is not always true, say I bought concentrated nitric in stainless steel container, and made it dilute or into copper nitrate, I could not store that in the stainless container.

These metals salt solutions are generally less trouble to store, but they are still very corrosive and can still put off acidic fumes that can corrode your materials in your shop or storage environment.

Labeling what you have stored is a must (handy MSDS should) be kept. Label should last when bottle sits for long time.

Location of storage is also a concern, away from children or animals, from being broken exposure to heat, light, other chemicals, or air, proper containers (for length of storage or conditions of use.

Well someone could write a whole book or many books on this one subject, and I am no author.


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## Oneal58

Thanks Butcher, 
Well, I can see right now I have some changes to make. I got my used, new, diluted with water acids Etc;, stored in the same cabinets. Though they are in different areas of the Cabinets and a few feet apart this is not going to work and will be seperated tonight. What if the sulfuric acid (diluted 2/3rd's by water) from my cell run that I have stored in the end cabinet had a container failure. Then just by chance I had another acid that had a leak in the container. So, (water to acid) which could turn into a dangerous situation very quickly! I am going to have to build sealed partitions in the cabinets to be sure I keep 1 particular acid in that area and if a spill occurs this acid cannot get to the other acids. I am also going to go back and date each used acid, why it is in the cabinet and how it was used, previously. I have got some changes to make to the way I am storing my acids. With my memory, or lack of it, this is a must for me! 
I will take your advice and study the characteristics (acids) when full strength, diluted, hot, cold, containers, Etc;,. Put the MSDS Sheets on the front of the cabinets for quick reference, if needed. I want to stay safe and I realize knowing what I am dealing with is the only way to do this. 
As always, thanks Butcher for the very important insights that you give me. As I said before, you just can't buy this type of information. 
I told you all I hated to see anything wasted. The cans I get from my sister I make projects out of. I just finished this one last week for the parade I went to Sat.. It was for a Wizard of Oz Float, I made it for a friend. I know it has nothing to do with refining gold but recycling (which we all do) in refinning is a very big subject. Take a look at my wifes new boyfriend below Butcher. Of course she is a Wizard of Oz Collector. I also make him in a 6 foot tall version. I have friends lined up wanting one though. I just don't have much time to work on any of my other projects now. 
Thanks so much Butcher!
Oneal


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## kadriver

Hello:

I had to filter the AuCl because there was some solids still in the solution.

I used two flasks and tranfered the funnel and used the same filter paper about 5 times to get all the solid out that I could.

The solution was a little clearer, but it still had some solids.

I then transfered the green colored AuCl to a tall 1000 ml beaker in preparation for dropping the gold with Stump Out.


----------



## kadriver

While stirring vigorously, I began to add the Stump Out to drop the gold.


----------



## kadriver

It dropped very easily and you can see it changing colors


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## kadriver

I heated the liquid to get it to settle quickly - this worked very well and it settled in about 10 minutes.

Then I filtered the clear liquid - you can see that there was still some suspended gold in the solution and it got trapped in the filter paper as I poured it in.

I kept washing the precipitated gold until the wash was clear, each time I poured the wash liquid through the filter - washing the gold trapped in the filter paper with the water used to rinse the gold powder in the beaker.


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## kadriver

Here is a shot of the filter paper full of gold - the filtrate was clear with no traces of visible gold - it all got trapped in the filter.


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## kadriver

I transfered the washed gold powder into a corningware casserole dish for drying the gold powder before melting.


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## kadriver

I rinsed the gold powder out of the beaker with distilled water from a squirt bottle.

This put an excessive amount of water in the dish with the gold and water takes a long time to evaporate - even when heated.

I use a folded up piece of paper towel and tilt the dish to get all the clear water to one side of the dish.

Then I dip the tip of the paper towel into the water, being careful not to get any of the particles of gold sucked up into the paper towel.

It very effectively removes all the standing water and saves lots of time while waiting for the gold powder to dry so I can melt it into a button (or a bar if there is enough gold powder for that).


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## goldenchild

So it sounds like the heating technique worked well. 8) Just one thing. The picture of you pouring the gold chloride. Its looks a bit cloudly like it could have been put through a filter one more time. I think very thorough filtration is sometimes overlooked. You can drop that nice brown clumpy sponge from solution even in a very dirty solution if youve filterd thoroughly. That may possibly be why your solutions were taking so long to settle. Keep the pictures coming Kad. We love pictures!


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## kadriver

While I waited for the gold powder to dry, I took the filter paper and held it with tweezers over the heat to dry it out. With the burner on high, it took about 15 seconds to completely dry.

Then I tore it up into pieces and put it in a melt dish and covered with lots of borax.

Using a torch with the flame on low, I slowly melted the borax over the pieces of filter paper containing the gold from the filtering earlier in the post.

I made a video of this process. I will edit the footage and produce a short video and post it later tonight or tomorrow.

The photo below is a shot of the piece of gold that I recovered from the filter paper. 

The filter paper gets completely erradicated during this process - no traces of it are left in the melt dish. And the melt dish is clean from all that borax.

If fact, I used the same melt dish to melt the dried powder coming up in the next shot.


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## kadriver

Thanks goldenchild - I filtered the solution about 5 times through the same filter paper, the last couple times there was no change in the clarity so I gave in and decided to drop the gold as this was a recovery. I will add the resulting button to my next batch of karat scrap for inquarting.


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## kadriver

Once the gold powder was completely dry, I transfered it to the same melt dish I used to recover the gold in the filter paper. It was still hot!


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## kadriver

I also added the piece of gold I got from the filter paper to the powder before I melted it.


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## kadriver

Here is the resulting button before getting a bath in dilute sulfuric acid to remove the borax that clung to it.


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## kadriver

Here is the button taking a bath in warmed, dilute sulfuric acid.


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## kadriver

Here is the new button posing with the other three pieces I recovered from filter papers.


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## kadriver

A shot of the reverse side of the button.


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## kadriver

I had calculated that there should be about 5.75 grams based on the amount of scrap gold filled material I started with. I conservatively estimated that the resulting gold button would weigh about 4 grams.

To my astonishement the button weighed in at 9.2 grams!

I was very pleasantly surprised. There must have been way more gold on those filled and rolled gold watch covers and bracelets that I used.

Some of them were real old - what a wonderfully rewarding experience it was to have recovered this much gold from this batch!

Many thanks to this forum and to those who helped me along in this process.

kadriver


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## kadriver

Here is the video I made showing how to recover the gold powder that gets trapped in a filter paper using a torch, melt dish and borax.

The filter is incinerated and completely destroyed leaving no traces.

[youtube]http://www.youtube.com/watch?v=GlozdhFuExk[/youtube]

Comments and critical input welcomed and appreciated.

kadriver


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## Oneal58

Kadriver, you missed your calling. Instead of Flying around with those Stewardess you should have been teaching? No,on second thought, I think flying with the Stewardess wasn't too bad of a choice? Would have been a hard choice to make??? Wife's ironing right now? :lol: 
Thank You Kadriver, just saying you did an absolutely wonderful job somehow just doesn't give the amount of credit that your hard work deserves!!
Just like everyone on this site, saying thank you anymore just sounds empty now, just isn't enough anymore for the amount you give to others like me. Who did not stand a chance witout you!
Oneal


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## HAuCl4

Great descriptions and photos Kadriver!. 8) 

Only comment I can think right now is that if you intend to re-refine the gold at a later stage, it's best to keep it in powder form and not melt it, but you already know that.

Cheers!. 8)


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## butcher

Another option is using Harold's trick, and GSP's trick.

GSP's trick "(use minimum amount of nitric when making aqua regia to dissove gold)"

Harold's trick "(use Kadriver's shiny gold button to see how well you done with GSP's trick, to eliminate excess nitric from aqua regia)" 

(well not a direct quote)


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## kadriver

Thanks to all for your kind words.

kadriver


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## HAuCl4

butcher said:


> Another option is using Harold's trick, and GSP's trick.
> 
> GSP's trick "(use minimum amount of nitric when making aqua regia to dissove gold)"
> 
> Harold's trick "(use Kadriver's shiny gold button to see how well you done with GSP's trick, to eliminate excess nitric from aqua regia)"
> 
> (well not a direct quote)


I like the "no nitric" trick the best for dissolving gold powders. Nitric has become expensive and a hassle to obtain (In some places it has become a controlled substance requiring police permits for purchase, etc, etc, etc). 

A few people I have setup are using inquartation and parting with sulphuric acid, and those that want finer purity after that use HCl and Clorox or Sodium Chlorate or something else. No nitric acid at all anywhere, except for assays. :shock:


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## kadriver

I remember reading Harolds tip on adding a gold button, but I cannot remember where.

Can someone post a link to Harolds description of adding the gold button while adding nitric acid to ensure the nitric is used up?

I would like to copy it and print it out for my notes.

I used to pre-mix the aqua regia and add it slowly to dissolve the gold. Sometimes the gold would be completely dissolved and I would end up with aqua regia sitting in the container, unused.

I like the idea of adding just hydrochloric at first, them adding small amounts of nitric acid slowly over time until all the gold is dissolved.

I used this method to dissolve the gold that produced the button in this post.

Thanks - kadriver


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## philddreamer

Kad, it's been posted several times, one way or another, but, this is the copy I saved in my notes about a year ago, I hope it helps: 
"Q-goldenchild: Where does Harold talk about saving a button to get rid of excess nitric?
Answer: I don't have a clue where I may have made mention, but it is a process used ONLY if you evaporate. When all of your feed has been dissolved, a weighed button of gold is then added to the solution, which would be kept warm enough for evaporation. As the solution concentrates, any free nitric will dissolve some of the button, or even all of it, assuming there is an abundance. 

This process is used to avoid using urea. I never used urea at any time. Preferring to evaporate, but more importantly, to use only the amount of acid necessary to do the intended job. You get amazingly good at judging after you've refined for a while. 
However, I found it far faster to use a slight excess of acid when dissolving the values instead of trying to hit it dead on. That insured all values were dissolved when processing wastes that contained other substances, such as filings from a jeweller’s bench. A slight excess insured the customer lost no gold. The added button eliminated the free nitric problem without effort on my behalf. I evaporated, regardless, because I preferred to keep my solutions highly concentrated. YMMV.

One word of caution, if you elect to use an added button of gold, do not be mislead by a lack of activity on the button as the solution gets concentrated. The cause can be due to the lack of free HCl, so to insure that is not the case a small amount of HCl should be added to the solution as activity subsides. An excess of HCl does no harm, unlike free nitric. 
By weighing the button before, then after it has been used, you can determine how much gold you added to the solution. That was important for me, because I ran individual batches for each of my customers. I had to know their yield in order to settle. Harold"

When using AR, I first add the HCl to the gold, then some peroxide; start to heat the solution & as the reaction starts, I add a small increment of nitric. When the reaction slows or stops, then I add another small increment of nitric; I do this until all the gold is dissolved. 
I always calculate the amount of acids needed for the digestion of the gold.

Take care!

Phil


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## kadriver

Thats it - thanks Phil


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## Oneal58

Hi Butcher, this is Oneal. 
Just wanting to touch base with you. I had a bad experience with UREA neutralizing solution and I have decided to try the method that you described in an earlier post. 
I made AR yesterday, dissolved my values from the sulhuric cell and also the gold filled foils. 
Reduced by evaporation down to 1/2 of volume, added a few drops of sulphuric to drop what tin/lead/Etc;, that I could. I reduced another 1/2 by evaporation, I was busy but I think that the nitric reaction you were talking about happened while I was busy and I didn't see it happen. I then added back 3/4 distilled water and let AR sit overnight. There was white powder in the bottom of the beaker that I used, a good bit this morning? I decanted by way of siphon and left the particulate in the bottom of the original beaker. 
There was so much whitish Tin/silver/lead/Etc;, in the bottom of the original beaker I have decided to run the now dark yellow AR through the method you outlined earlier. Your method of evaporating down to syrup and adding a little HCl. Then run the process a couple of more times. 
My question is should I add a few more drops of sulphuric acid before getting AR too near to being a syrup? After these processes I will increase volume by 4 times with distilled water, let sit overnight and drop gold tomorrow?
What is your preference to use the MetaBisulfite to drop the gold, a warm or cold solution?
Any guidance here would be appreciated Butcher. 
Thanks Butcher,
Oneal


----------



## butcher

Oneal, 
Glad to see you using the evaporation method, make note when evaporating of the first evaporation (if excess nitric) that as solution gets concentrated you should watch reaction carefully, watching for those small bubbles to start to form (point nitric wants to come out all at once), and turn down heat (or just lower heat the first run) also do not leave solution evaporating and cook to salts (burning gold to bottom of vessel).


When dissolving gold many people will make a mistake and use way too much acid for the volume of gold, this would mean a very long evaporation time to concentrate all of this excess acid.
They also tend to add way to much nitric acid (wasting it) and it will take time to remove.

Best approach would use minimum acid needed (HCl), and adding minimum nitric needed in small increments to dissolve gold, this would leave most of the gold saturating the acid and almost no nitric to evaporate, in this perfect mix adding a bit of gold to the evaporation would quickly use up nitric (so one could basically eliminate the excess nitric with just heat and almost no evaporation.
So keep this in mind as you process. 


(Not adding urea to contaminate their gold solution)
(Although a prill can be used to see if nitric is still in solution)


The SMB I am normally not too concerned about temperature (others may be), (as long as temperature is not extremely cold or hot, and then I may try and change temperature) (another reason if from dirty solutions I get colloids then I may heat to boil).

but I do keep in mind that if solution is cold it will hold SO2 gas longer (good), but I it may take longer for reaction to take place, (and solution will not mix on its own from heat rising).
If solution is hot my SO2 gas may escape so fast that the reaction (although reaction faster with heat) will not have time to take place, mixing well is more important to me than temperature as long as it is not extremes.


Hope fully that white powder contains some silver, save it rinsed and keep wet, when you’re ready to deal with it we can discuss it.

Sorry if this does not give you clear instruction (it’s just the way I see it others may have a different opinion).


----------



## Oneal58

Thanks Butcher, been evaporating for hours. Got to get back to the old house. Thanks for the information. Getting close, got to go back out. Talk to you a little later. Oneal


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## Oneal58

Hi Butcher,
Came back in for just a minute, it's really cold out there. 
I have decided due to the amount of particulate drop I had this morning in the bottom of the beaker, to add a few drops of sulphuric again. Maybe 15 more minutes and AR will be syrupy. Add enough HCL to dilute ( a little) evaporate again, same process 2 more times. Then add 4 times volume of distilled hot water. Put up, covered. See what is what tomorrow. 
Thanks Butcher,
Oneal
P.S.
Really excited, anticipation is building, want to see what comes out of the sulphuric cell gold plated stripping and the krud filled watch band tops tomorrow when I drop.
If I can come out with a nice looking button (from this dirty stuff) you will probably hear me, as we say down south, give a loud (Holler) in Oregon. 
Will let you know, got to go, going to get through this before I stop, even if I see the sunrise tomorrow morning. 
Hopefully things will come out good, then I will feel more confident starting on the karat items. 
Thanks a million Butcher,
Oneal


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## Oneal58

Hi Butcher, 
That's the problem, if I had a piece of pure gold I would have used it a long time ago. I used what little piece of pure gold I had on a test. I hope to have some pure AU from now on though handy. Would have saved a lot of time. 
Trying to warm up again, getting really cold out. 
Thanks Butcher,
Oneal


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## philddreamer

"That's the problem, if I had a piece of pure gold I would have used it a long time ago. I used what little piece of pure gold I had on a test. I hope to have some pure AU from now on though handy. Would have saved a lot of time." 

Oneail, have you learned how to calculate the amount of acids required to dissolve your metals yet? If not, it would be a very good idea to learn now. It will cut down the time spent on evaporating the nitric.

To me, the "fun" of this hobby starts when I sit down with my scrap PM's, paper, pencil, my calculator & I start figuring out how much gold I could recover; then calculate how much silver for the inquarting & then how much nitric & distilled water for dissolving the base metals, & how much HCl & nitric will be needed for dissolving the gold, & so on. 

Just my dos centavos!

Kindly,

Phil


----------



## Oneal58

Hi Phil, 
I just learned how to calculate the quantities of chemicals required to refine X amount of gold this week Phil. I have been studying Hoke's Book again. Not just reading this time like I did the first time but studying it. Doing the test she recommends and trying to follow her to the letter. 
Trouble is I have had this gold lot going for the past 3 weeks. I got into all the trouble before I knew what I know now.
But from now on you bet I will (not) add more chemicals than I should. I will weigh every single piece of metal and keep up with every single ml of chemical applied! I would rather re-process some of the material than waste my acid and triple my work. 
Believe me when I say, I have learned my lesson.
Thanks Phil, I wish I had of listened better a month ago!
This I can say to all the noob's, listen to the people on this site, don't take any shortcuts. Why? Because they aren't any short cuts!
Oneal


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## Oneal58

Hi Butcher, or anyone familar with this process. I finally got down to my 3rd evaporation and had added my 3rd few drops of HCL. I evaporated for another hour after my last add of a few drops of HCL. I had nothing but black syrup in the vessel. So thick it would not even swirl in the container. I had added a few drops of HCL but I thought I had evaporated that off. I thought that the nitric and the few drops of sulphuric was long gone also. When I added water, (made sure it was very hot water) to this little bit of black syrup in my container I got a violent reaction with lots of brown fumes!! I think this was telling me that I still had an acid or a couple of different acids still left in that black syrup in the bottom of that container. 
My question is, why did this happen? Should I have waited for the vessel to cool before diluting with hot water. I thought the acids were long gone, I had no reactions going on in the vessel and no smell of anykind. But when I put that hot water in there it started jumping out of the tall beaker. I am just glad I was using a tall beaker. Some still jumped out of the beaker. There must have been acids left in that black syrup that I missed somehow? Is this right? I am glad I was standing behind a partition I had made for just this purpose or it would have got me!
What did I do wrong, didn't heat the black syrup long enough to drive off acids. I was aware of this, but the syrup was starting to get hard, I had to stop Evaporating? Every indication said that the acids were gone? What happened, I do not want that to happen again!
Thanks, Oneal


----------



## niteliteone

Oneal58 said:


> Hi Butcher, or anyone familar with this process. I finally got down to my 3rd evaporation and had added my 3rd few drops of HCL. I evaporated for another hour after my last add of a few drops of HCL. I had nothing but black syrup in the vessel. So thick it would not even swirl in the container. I had added a few drops of HCL but I thought I had evaporated that off. I thought that the nitric and the few drops of sulphuric was long gone also. When I added water, (made sure it was very hot water) to this little bit of black syrup in my container I got a violent reaction with lots of brown fumes!! I think this was telling me that I still had an acid or a couple of different acids still left in that black syrup in the bottom of that container.
> My question is, why did this happen? Should I have waited for the vessel to cool before diluting with hot water. I thought the acids were long gone, I had no reactions going on in the vessel and no smell of anykind. But when I put that hot water in there it started jumping out of the tall beaker. I am just glad I was using a tall beaker. Some still jumped out of the beaker. There must have been acids left in that black syrup that I missed somehow? Is this right? I am glad I was standing behind a partition I had made for just this purpose or it would have got me!
> What did I do wrong, didn't heat the black syrup long enough to drive off acids. I was aware of this, but the syrup was starting to get hard, I had to stop Evaporating? Every indication said that the acids were gone? What happened, I do not want that to happen again!
> Thanks, Oneal



Oneal my friend,
Glad to see you are still working on getting this done the right way.
I've been following you but have been quiet since Your in good hands that know more than I do.

It looks like your process of evaporating down to remove excess nitric is not quite right. In this process you are not removing acids. You are only evaporating excess nitric acid out of solution. All others must stay in solution.

From what I have read you are evaporating to far. you want to stop before the solution turns to syrup then double remaining volume with fresh HCl. 
(example) You start with 800ml solution. Evaporate down to approx. 200ml. them add back to solution 400ml fresh Hcl. do this 2 more times with 400ml each time. (not a few drops)

Let the solution cool some before adding any water as hot acid solutions are more reactive than cool solutions. Then add the water slowly 25ml at a time. It is not a good thing to add water to concentrated acid to begin with ( as you saw what usually happens) and since your solution was super concentrated from all the evaporation and not enough HCl addition, You had a loaded canon waiting to go off. 

Reread Hokes book on evaporating excess nitric and write down the proceedure so you have it at your bench when you do this the next time. it's a good thing you had that shield to stop the acid from splashing on you.

Hot super concentrated acids are really dangrous and We don't like it when our family gets hurt. again I'm glad you are OK. Be careful.

I hope I got this right if not can anybody correct anything I got wrong so i can learn the best way too.

Goodnight Oneal and all.
Tom C


----------



## butcher

Oneal,
Here is my take on the situation, when solution is first made you had water, HCl, nitric, gold, (possibly silver lead and some other base metals).

When you first begin to evaporate the majority of vapors is water (and gases of reaction), then as you proceed and most of water is gone then the nitric vapors come off, the nitric in solution concentrate (with HCL), when nitric and HCL get concentrated nitric fume are much more concentrated (I believe this is the point nitric will boil over if temperature is not lowered then when most of the nitric vapors off), not all of nitric escapes as I think a portion will azeotrope with HCL), then HCL also concentrates (gold bonds most of the chlorides as a gold salt) any free HCL will vapor off leaving gold salt solution. if driven to dry powder I believe the gold would reduce to metal as the chloride gases off, (but some gold would also become volatile in these fumes and vapor a good portion of valueable gold up in smoke).

The above description is way overly simplified (to give an idea of what happens). The fumes are not purely one gas, and there are combinations of gases forming and escaping.

Now I did not mention the sulfuric acid you added, sulfuric acid has a very high boiling point, and will not evaporate with the temperatures your using.

I think you may have added more H2SO4 than needed, and you went down to a very thick syrup, with your gold chloride salts so most all of the free HCl was evaporated and you concentrated the sulfuric acid solution (gold salts) then you added water to concentrated sulfuric acid.


Now think about the rule about adding water to concentrate sulfuric (and warning how it is so violent of a reaction).

Here if you had added some HCL (20%HCL in which 80% is water), you would have diluted solution and the sulfuric acid, so water reaction might not have been so violent.

Just a little too much sulfuric, and maybe a little thicker syrup than necessary,

Live and learn?

This is just my thinking (not being there and seeing),


----------



## Oneal58

Thanks fellows, I appreciate your help. 
I will go back through HOKE'S Evaporation Process (again) before attempting anymore. This scared me, I could have easily been laying up in the Hospital today? 
I have taken a couple of pictures of what is left of the solution. It is not nearly as concentrated as it was before I started. It was so yellow I could not even see through it in the beginning. I fear I lost a lot of values in the, now what I call an explosion. How this small coffee pot stood up to the reaction I have no idea, but glad it did. I have some of the solution in the bottom of my dish, floor, wall, partition, Etc;. How do I recover the solution that is in the dish? If I mop it up with filters and just put into my next AR Batch?
This is my question, take a look at the center of the vessel, in the bottom of it. It looks like a mound has formed. Is this mound made of gold there, it sure looks like gold. It is sitting among whitish powdery looking material, probably more tin, lead, Etc;. But this mound, what is it, is it gold that participated out somehow in the reaction. I got you a picture of it, it puzzling me?
Oneal


----------



## butcher

Oneal58, 
That is a nice yellow color; looks like you have done a good job of removing the base metals. I am impressed.

Yes it is most likely gold in the bottom of the beaker, gold will not dissolve in sulfuric acid, and when you evaporated to thick syrup you removed most all HCl, and maybe a portion of chlorides that were locked up in gold salts, these chlorides may have exploded off in the violent reaction as chlorine gas when your beaker erupted by adding water to the concentrated sulfuric acid and gold chloride solution, thus reducing to elemental gold.

The other impurities in this gold in the bottom of your beaker can be washed out or the majority of them can be.

I would decant the yellow solution from these gold and impure powders; the yellow solution will hold more pure gold. And we do not want to precipitate the purer gold in solution into the (now reduced gold and lead and silver salts).

After washing the powders (the gold in bottom of your beaker we can return them, to the other gold you will precipitate from this solution later).

After decanting (decant and filter yellow liquid into clean vessel). You can precipitate gold from this pretty yellow liquid. (Wash any precipitated gold using Harold's instructions.

Leave gold powders now reduced in your beaker (gold, silver chloride, lead salts in beaker), add water and boil (raise temperature to boil slowly, we do not want to thermally shock the glass), after boil lower temperature so powders settle well (no moving action from heated beaker stirring solution), then we will decant the solution (lead Chloride dissolved in hot water, precipitates out as white crystals when cool). May need to repeat depending on how much lead we need to wash out.

Now these powder contain gold and silver chloride (here we could re-dissolve gold to remove it from silver chloride, (OR) dissolve silver chloride from the gold, I would choose to dissolve silver chloride, 

(But to do this you must follow directions closely as silver compounds in ammonia can be dangerous if allowed to dry), keep wet and acidifying make them safe),

Add ammonium hydroxide to gold and silver chloride salts (household ammonia), (real ammonia is better but harder for me to get), heat solution but (DO NOT COOK DRY). The heat does not need to be too high as ammonia will gas off at low temperatures, this solution will change silver chloride salts to a silver Amine solution (silver will be soluble and we can be wash the silver from the gold), decant this warm solution to clean jar, let it cool in this jar (you may have picked up some gold (which will settle) if so we will separate these.

Silver in this silver amine solution is precipitated by adding HCl, (this acidifies the solution making it safe), this gives you back your silver chloride powders, the solution becomes Ammonium chloride solution (I save all my ammonium chloride solutions to make salts later).


Hot water rinses help in washes.

(What we have done here is very similar to Harold’s washing of gold powders)

I did not give all of minute details here but a general overview of how I might approach this.


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## Oneal58

Hi Butcher, thank you for the compliment. I don't want to get my hopes up again just yet though. I have been too confident a couple of times prematurely already? But thanks Butcher for the much needed encouragement. 
I am just getting back in today. Had something to take care of this afternoon. Going out to start back up again. Will keep you informed of progress. 
Thanks Butcher,
Oneal


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## Oneal58

Hi Butcher, or if Butcher is busy anyone who has an idea what I am doing wrong? 
I dropped the gold (SMB) and washed good several times in hot steaming water. I added HCL to powders 3 times and heated, decanted, wash, repeated. Last time I washed with distilled hot water several times before adding ammonium hydroxide. Decanted, rinsed several times with steaming hot water. Then 1 final wash in HCl/BOIL decanted rinsed several times with hot steaming distilled water. 
Each time the solution would get low I would get this loud popping in the beaker. The Gold is popping like popcorn, I have to keep the beaker covered because the small pieces of gold will jump out the beaker. Sometimes a little nugget will surprise you and shoot off with a loud noise? 
I feel that I may have acids (HCL) locked up in the gold somehow or I used too much (SMB) to drop with and it's locked up in the gold? But I washed and heating many times? When heated these pockets of gas/acid are exploding. Every once in a while 1 will pop to the extent I am afraid it may break the beaker I have the gold in? Every picture of gold I have seen on the forum looks like powder after being dropped. The gold that I dropped has very small nugget like structures (characteristics) to them? Why is that?
Am I on base here and what do I do, keep heating untill the popping stops completely?
Thanks Butcher,
Oneal


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## Oneal58

Hi Butcher, when melting your gold button. Do most refinners use Borax on this forum? I know it depends on how particulate/crud you have floating on your gold. If your gold is pure enough though that you have no crud. Doesn't the button pick up the borax on the bottom of the button from the melting dish anyway? You have to use warm sulphuric to get this coating of Borax off after the melt, how long does this usually take, to get the Borax off and is there an indicator that will key you in when the Borax is gone.
Thanks Butcher,
Oneal


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## qst42know

> is there an indicator that will key you in when the Borax is gone.



The borax glass will go milky white and fall off.



> Gold is popping like popcorn, I have to keep the beaker covered because the small pieces of gold will jump out the beaker.



Drying too fast causes steam explosions to eject some of your gold. Low heat till mostly dry would help, then drive it hotter.


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## butcher

Oneal, 
STOP WET THE POWDERS.
Remove from Heat.

You may have made a fumilate,
It does not sound like you have followed Harold's wash procedures correctly.

If this is the case you may have made a very dangerous substance.


The ammonia (metal compound) should be made some what acidic and washed.

Get this into a safe condition or stay away from it.

We can discuss this further later.


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## Oneal58

Hi Butcher, checked back over Harold's instructions. I followed them exactly. I cut heat down to a simmer, reaction stopped. 
I just got through melting the gold button, didn't use any Borax on it. I didn't see any type particulate or crud on top of the button and went ahead and melted it. I counted to 5 mississippi,is that enough? Picked up the button out of the melting dish and went for the water. The button stuck to my pliers and I missed the water. The button landed on the floor, I picked it up again and made it to the water this time but it was already cooled down. 
The buttom looks terrible because of this. 
Can I re-melt the button again, causing no harm and maybe using a little Borax this time? Pictures of the ugly button is below. It should have been 5 times bigger but as all of you know I lost a lot of values on several occasions. As Butcher said it, LIVE AND LEARN. I know I can do better the next time, I have already started on another batch. I have developed this fever this afternoon but I don't feel sick, wonder what it could be?
Will it hurt to re-melt it to get a better looking button?
Thanks, Oneal


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## butcher

Oneal, you scared the crap out of me, I thought you were in danger, with that gold exploding after adding ammonia.

Edit: Well after cleaning my pants, and looking at your button Good job.
please do more study before making any more gold buttons, I sure would hate to see something happen to my friend.


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## qst42know

It looks pretty good even roughed up. 

Save the button to add to the next melt.


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## Oneal58

Butcher, I would like to meet you one day my friend? Thank you for your concern, all your consistent help and always being there for me. I know I got a long way to go yet, but it feels good to have that little button in my hand. Who knows, when I get to turning out some bars, instead of buttons I may just pay you a visit 1 day. How far are you away from YellowStone, WY.? I think you have to go across Idaho, don't you? I have always wanted to go there with the wife/grands. Maybe I could run by to say Hello, and just to shake your hand in thanks?
Well, got to go see what my Nitic bath is doing, catch you in a while.
Thank You, my friend!
Oneal




butcher said:


> Oneal, you scared the crap out of me, I thought you were in danger, with that gold exploding after adding ammonia.
> 
> Edit: Well after cleaning my pants, and looking at your button Good job.
> please do more study before making any more gold buttons, I sure would hate to see something happen to my friend.


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## Oneal58

Thanks qst42know, that's exactly what happened. Lowered heat, gold stopped popping. Checked back on Harold's post back in 2008 and saw that he had mentioned this popping also. 
Thank you for your help.
Oneal



qst42know said:


> is there an indicator that will key you in when the Borax is gone.
> 
> 
> 
> 
> The borax glass will go milky white and fall off.
> 
> 
> 
> 
> Gold is popping like popcorn, I have to keep the beaker covered because the small pieces of gold will jump out the beaker.
> 
> Click to expand...
> 
> 
> Drying too fast causes steam explosions to eject some of your gold. Low heat till mostly dry would help, then drive it hotter.
Click to expand...


----------



## butcher

Oneal, 
I guess I misread your post, or read into it, and did not see rinsing out of the ammonia (or acidifying it), the Bang of the gold drying by gold popping, did scare me, I really thought you could have been in danger and with out seeing what you discribed I did think more than steam was possibly causing this reaction (was afraid what might happen if you continued heating, or went to melting, I had emailed Harold, GSP, Lou and Quest 4 to know, asking for their help, as I had seen your post was from ealier this morning, and was afraid you may have tried to melt this, and with no updated posts thought you could be headed for the hospital or worse. (the email's to others were deleted)(quest4toknow was online), I am so glad qst42know was right and it was just steam eruptions.

I do not know how far I am from YellowStone, WY. but I would also like to shake your hand someday,and meet you in person, just what little I know of you your a man I would like to meet, (and I don't care about meeting many people,I stay away from them for the most part, farther away the better).


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## The Refiner49er

Hi All-

It has been a long time since I posted or asked questions here, but I am back into refining and would like to add a thread to this subject...

I am currently processing fairly large quantities of gold filled items, and as a result have substantial volumes of depleted nitric acid that likely has silver content, of which I want to recover. I have been reading through the forum and see a number of options, but would invite and appreciate any input on the best way(s) to collect and refine the Ag component from the waste acid.

I also see many complaints about the accessibilty to nitric acid and it's relative high cost. To share my experience in this regard, I used to make my own nitric acid, and it works OK, but does not come close in performance to commercial grade (68%), and I found a source here in Portland Oregon which is Univar USA Inc. Note that it must be purchased in 165# SS kegs, and the deposit on the container is $400 (yikes!) but the acid ends up costing about $15 per gallon; Univar is a national chemical supply company with many locations, just thought those who have high consumption requirements might want to know.

Anyway, please return any appropriate feedback on silver nitrate recovery from nitric acid, thanks!


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## qst42know

Have you tested this used nitric with DMG for palladium?

Your test result will indicate some choices.


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## The Refiner49er

Hmmm, no I haven't tested for Pd and honestly never thought to do this, and as a refiner have not done much at all with this PGM metal. Is there a chance that gold filled jewelry and eyeglasses really contain significant percentages of palladium? Most of what I am processing is older stuff, I am sure there is probably a fair amount of silver in the spent nitric.

I see many references to cementing out the Ag with a copper plate, but because I do not always completely consume the nitric, it must first be neutralized; after all, copper is not cheap these days either! Moreover we are talking about many GALLONS of solution as the result of this commercial endeavor, and the last thing I want to occur is to inadvertantly accumulate large volumes of waste chemicals that still contain values. I am currently storing in white 30 gal HDPE drums but want to develop a system soon for complete recovery then dispose the vacant solution rather than have it sitting around, as I see it as another liabilty.

Thanks for your input!

John


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## qst42know

If you included white gold filled in your processing some of this will be white from palladium, some from nickel.

Some tests will give you a better Idea if it's worth cementing on copper. If you have no Pd or very little you can skip the copper and collect silver chloride with HCL.


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## The Refiner49er

OK, thanks! I will pick up some DMG, any suggestions as to a source? Also, if you don't mind could you elaborate further on the HCL process for dropping the silver such as acid ratio/volumes and any other steps in preparation/recovery? I assume if Pd is present then this metal is dealt with first, then recover the Ag?

If Pd is indeed a justifiably payable metal, I am thinking now it would be prudent to separate the white gold from the yellow and handle the wastes individually.


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## qst42know

I bought some DMG from a seller on eBay but he dosen't have anything current.

Some here have dealt with this company. It's a little expensive from them but a gram will do many tests.

http://www.abprospecting.com/sitebuildercontent/sitebuilderfiles/furnche18.jpg


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## butcher

We generate waste that can be used, or should I say we make some useable chemicals or metal powders we can think of as waste that are not waste but are useable products.

In industry many of the chemicals we buy are actually waste from a process that company’s would have to pay big money to get rid of, like sulfuric acid, they should pay us to take it off there hands, these company’s will find a use and market there waste instead of pay to dispose of it, Hmmm we have SO2 gas that will cost us if we pollute air from our process, and when we treat these fumes we make sulfuric acid, that would cost us money to neutralize and dispose of, what can we sell this for maybe drain cleaner, or clean up some of it and sell it as battery acid, or sell this to some other company to use in there processes.

One example: the chemical by products like potassium bisulfate (white salt) from making nitric acid can be used to make ferrous sulfate, or this sulfate can be used like sulfuric acid in reactions, or in fusion to make rhodium soluble in water.

There are many chemical byproducts we generate that can be crystallized and reused like ammonium chloride.

If I have a caustic waste, I can use it to neutralize an acidic waste.

Copper I chloride powders, I will pour my spent solution’s into a bucket of these copper chloride powder, some copper from these powders will go into solution and be replace by silver gold or PGM that may have been in solution as traces.

I keep recovery stockpots, and refining stockpots.

Copper cemented from treating waste, these can be cleaned up and used to cement values from solutions, keeping me from using more copper (that is sellable scrap).

If I have a (used) copper nitrate solution that has some silver and possible PGM, I may save this to dissolve some more copper that could have some silver or gold plate, I will heat this use copper chloride solution with copper plated article, (concentrating solution for less volume later), this will dissolve much of the copper I have added, cement out values, and lower the volume of the copper nitrate solution, (I can also add some oxidizer if needed like hydrogen peroxide or more nitric if needed to get more copper to dissolve in this solution), I can also add sulfuric acid and some copper and distill NO2 gas (bubble into little water and hydrogen peroxide) to make nitric acid from this used copper nitrate solution, or crystallize the copper nitrate, heat the salt to make nitric from the gas generated in reaction.

Sometimes I use my cemented waste metals from a previous waste treatment to cement metals from the next batch of fresh waste acids (saving me adding new metals), or I use a basic or caustic waste solution from treating a previous batch of waste to lower the pH of the new batch of acid waste (helping me save chemical), (this is hard to explain) 

Basically do not always think of a used solution, chemical, or byproduct as being a waste, think how can I reuse this in my recovery processes, but also consider are you lowering the purity of metals in this recovery process if I do this with the solution I am working on.


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## kadriver

Oneal58:

I just seen your gold button - congratulations!

Man that thing looks like pure gold to me. Way to go!

I know your wife is pleased to see it. Thats over $200 bucks.

Good for you. 

You should be able to remelt it without any loss. You can add some borax also, just make sure to pluck the button from the dish before the borax hardens.

I like to use stainless steel tweezers. For me, pliers are too big and bulky.

Also, You mentioned that you had felt ill.



Oneal58 said:


> I have developed this fever this afternoon but I don't feel sick, wonder what it could be?



The first time I melted some silver, I did not use a respirator when I was doing the melt.

I remember breathing the smoke from the melt. I had worked around hot metal from welding and brazing when I was in the Navy, so I did not think there was a danger.

The next day I was flat on my back in bed with a flu like illness. I am fairly certain the illness was from breathing those molten silver vapors as I did the melt.

I don't know if molten gold vapors are like molten silver vapors, but I know for a fact that breathing the vapors from melting silver will make a person very sick!

From that time forward, when melting metal, I always wear a 3m respirator with #95 particulate and vapor filters. I have never gotten sick from melting metal since.

Great job on your pure gold button!

kadriver


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## Oneal58

Hi Kadriver, and everyone. 
Thank you Kadriver for the compliment. I sure hope it's nearly pure. I went through the extra steps to try to make the button pure. I double re-fined, recovering my gold first, inquarting and refined again. I went through the lenghty process of Harold's (making gold pure) steps also. I plan to do this on every batch I run. I want to develope a reputation that I have (nearly) pure gold, without the electroplating process. I just don't want to keep that amount of gold in solution all the time to do the electroplating process. I have a piece of 24K gold antique Jewelry, or it is marked 24K. My button has the same color as this piece of 24K Jewelry that I have. This piece is so soft you can almost roll it up with your fingers. So, I am hoping that I got it at least .995. The pictures I loaded are close to the color but just doesn't capture the true color of the piece. 
And just to think that this small button came from crud filled watch band tops and what was left of the powder I got out of the Sulphuric Cell run. 
*QUESTION 1-*Kadriver I burned my filters last night, the way I saw you burn yours. I am surprised at how much value these filters were holding?? After you got through with your burn did you incinerate the values to add to your next batch, or did you try to claim them while they were in the pot? Nitric is not going to touch this recovery so which way is the best way to go here? I know they are very dirty, smut, trash, metals other than gold, Etc;, but this recovery from the filters is mostly gold too? There is no paper left, nothing but smut, dirt, trash, Etc;, but mostly gold?
*QUESTION 2-I didn't run the filter papers from the AR filters.* I just didn't understand the physics of burning the paper with the gold in solution? With this yellow AR in the filter paper, what will happen to it if it is burned. If the gold does revert back to solids, wouldn't if be so fine that more than likely it would be blown away , just when you added lighter fluid to burn the filters?
Seeing what these filter papers were holding sure has made my mind up that any decant will be done with syringe and hose from now on, no doubt about it. I will filter the decant (while draining with hose) but the first porcess will not be straight to the filters! I am happily surprised that a lot of the work I put into the Sulphuric Cell process has showed up in the filter papers. 
KADRIVER, I have been told I have a strange sense of humor. When I referred to having a fever after melting the button but didn't feel sick, I wasn't referring to my health. I meant I had caught the (GOLD FEVER). 
Thank you for your concern however! Thank you in advance for your answers! Kadriver, I still got that fever but I can't take my medicine for it today. The wife has laid the Law Down for today, and I quote, "there will be no work on Sunday", "no matter what"!
Oh well, got to go watch the Grand's in their Christmas Play, talk at you later.
Thanks Kadriver,
Oneal


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## kadriver

Oneal58 said:


> QUESTION 1-Kadriver I burned my filters last night, the way I saw you burn yours. I am surprised at how much value these filters were holding?? After you got through with your burn did you incinerate the values to add to your next batch, or did you try to claim them while they were in the pot?



I didn't catch the meaning of your fever (I do now that you have explained it).

The filter paper that I burned yielded a piece of gold that weighed 0.2 grams. Normally, I would save it and throw it in with my next batch of karat scrap.

But in this case I added the 0.2 gram bead to the gold powder that I had recovered from the batch of gold filled scrap that I processed.

I melted the 0.2 gram piece from the filter paper burn, in with the gold powder from the gold filled scrap recovery because it was from that batch.

That 0.2 gram piece contributed to the total weight of the gold button that I recovered - I think the button weighed 9.2 grams (which blew me away because I was expecting only 5.75 grams).

I usually add the button from the gold filled batch to my next batch of karat scrap. This particular 9.2 gram button went into a batch of karat scrap that I processed this weekend. I finished the gold bar last night - it weighed 3.37 troy ounces.

I posted a picture of the bar in the Gallery. You can look at the picture by going to this link:

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=61&t=12292




Oneal58 said:


> QUESTION 2-I didn't run the filter papers from the AR filters. I just didn't understand the physics of burning the paper with the gold in solution? With this yellow AR in the filter paper, what will happen to it if it is burned.



Anything that has that yellow color contains gold. The filter papers from the aqua regia filtering should have no color in them when you get done with the filter operation. If they still appear yellow, then you should rinse the filter with distilled water until all traces of the yellow color is gone from the filter and the water runs clear.

Once all the AuCl is rinsed from the filter paper, I usually just throw mine away. Sometimes there is some silver chloride in the filter paper - but not enough to bother with (this is only my opinion and there may be others who disagree with throwing this filter paper away).

I was very happy to see that you got a nice piece of gold from all of your efforts. Any gold that was lost due to error was the price paid for a top quality refining education! We get better as we gain experience, and there is no substitute for experience.

kadriver


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## Oneal58

Thanks Kadriver, 
*Question 1*-So you transfered the gold powder to the melting dish from the pan, what did you do, sweep it out with a little broom? Then melted into button and added it to your main run. What did you do with all the smut left on the pan, does this smut contain any gold? Or just wash it out with dawn detergent, and a scrub pad. I know that using a steel wool pad would not be too smart to use here to clean the pan due to the habbit of these pads leaving pieces of metal behind and possibly scuffing off some of the metal/finish from the pan. I have a plastic looking scrub pad, would this be fine to use to clean the pan.
*Question 2-* I have a coule of ounces of silver nitrate from the silver drop with copper/urea. Expect to have even more after this last run. I don't want the silver to get too far ahead of me. 
I have read many post on how to recover this silver. Also read HOKE'S method, it seems everyone does it a little differently.
*QUESTION 2_*What process do you use, other than to put into filter, run suction and pour hot water over silver until solution runs clear. Is this the best apporach or you use a little different approach now? 
Question 3-What purity can I expect out of this dropped silver nitrate. Is it going to be higher than .925, what I started with? I have watched several videos on this process and also read a lot of material. Just want to touch base with you before I melt the silver. Have watched your video's on pouring your silver, (resulting beautiful shinny silver bars). I see you pour into a graphite mold to do this. Do you still use this method? I would rather not have to polish when melted and poured, as yours look. I know you pre-heat the mold but do you use anything else on the mold prior to heating to keep melted silver from sticking to the graphite mold. I have watched video's that the person had to break the molds apart to release the bar of silver and then had an involved job cleaning the silver bar afterwards. I would rather not go that route. *Question 3- *I found a suction pump at Wal-Mart. It is 4-D-cell battery operated and when you put your finger over the suction side of the pump it has a pretty good suction. It is light, small, very easy to move around and can be attached to the beaker with little effort. It was only $16.00 if I remember correctly. It was sold to deflate large matresses with, do you think this suction pump would work.
*Question 5-* I see you had a guage, adjustable suction? Is there a goldilocks point on the suction side you have to reach to get the reaction you want? If so, I could put a slide across the inlet to adjust the suction if I needed to. What do you think?
*P.S., 
Just remember Fellows, anyone can ring in to my post regardless of who they are addressed to and I mean any of my post. The more the merrier. I love this forum because of the different points of views. So anyone ring in that may have an idea or see I have overlooked something. 
Thanks Kadriver, Thanks to Everyone! *
Oneal


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## The Refiner49er

If you don't mind, I would like to contribute to the methods I use for gold. Personally I have followed Harold's advice to the letter, and other than when the pregnant solution is filtered and evaporated, I use the same beaker throughout the entire process. This includes dissolution and precipitation, the washing steps with water, dilute HCL and ammonia; and once the Au powder is ready to be dried I simply put the well drained beaker in a warm oven, no more than 190 F and in a few hours it is dry without attendance or issue with steam "popping". If the powder is clean all that is needed is some tapping and sliding around to separate it completely from the vessel, then straight into the melting dish without tools. I have all my glass marked with it's respective tare weight, so it is easy to know what you have after drying. Nothing revolutionary, just a simple system with minimal handling.

John


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## Harold_V

Oneal58,
A comment on your double refining. 

You made mention that you inquarted for the second refining. Not necessary, and may work against you. 

There is one, and only one reason why we inquart. It's as simple as this. Because gold and silver can not be in (acid) solution at the same time, the problems created when one tries are difficult to overcome. That's true unless the ratio of gold/silver is proper. If you try to dissolve gold alloy (any that contain silver), the balance of silver often prevents aqua regia from dissolving the gold because it forms a hard crust around the object. Once that happens, the gold inside is totally isolated from the solution, even when it is heated to boiling. Dissolution stops. That is true of pieces with a heavy cross section, but may not be true of small or thin pieces, that may be fully penetrated before the hard crust can form. In such a case, no problem aside from the less than clean solution that results. 

The same problem exists when you attempt to dissolve the base metals from a gold alloy that contains more than 25% gold. In practice, by hard boiling even 40% gold alloy can be leached, assuming it is not of heavy cross section. 

So then, the desired target for parting the two metals, gold from silver, is a ratio of 25% gold, 75% silver (or base metals, with a 75% ratio including base metals). That permits dissolution from relatively heavy cross sections of melted (inquarted) alloy. It also yields gold that is honeycombed, and retains its original form. That's a desirable quality, so the gold doesn't disintegrate, making separation from the nitrate solution difficult, or time consuming. When gold is properly inquarted, the resulting nitrate solution will be absent of particulate matter entirely (assuming distilled water is used), so it can be readily poured off so processing can continue. If you go much below 25% gold content, that is no longer true. 

There is a bit of non-agreement about this matter. Some prefer to crush the gold, assuming it will be better stripped of base metals and silver, although, in practice, it isn't. It is a waste of time, yielding no benefits so long as you carry out the preliminary digest properly. 

So then, what I'd like for you to take away from my position on the soap box is the idea that when you re-refine your gold, do nothing more than wash it well. If you intend to immediately re-refine, there isn't even need to dry. You'll come to understand that the once refined gold will dissolve very quickly, which is far different from gold that has been melted. This second refining, assuming you have NOT added silver (inquartation), offers a second opportunity for traces of silver, which have followed the gold, to be eliminated. To have added silver a second time defeats that purpose. 

Harold


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## kadriver

Oneal58 said:


> Question 1-So you transfered the gold powder to the melting dish from the pan, what did you do, sweep it out with a little broom? Then melted into button and added it to your main run. What did you do with all the smut left on the pan, does this smut contain any gold? Or just wash it out with dawn detergent, and a scrub pad.



When I get to the stage of drying the gold, it is usually quite pure after many washings with distilled water. I have not seen "smut" in my drying pan in a long time. The smut in your drying pan is an indication that the gold powder was not pure. When pure gold powder dries, it leaves no residue - unless it is dirty from not being washed properly.

I have seen "smut" in my gold drying pan in the past though. It would bake onto the corningware casserole dish that I was using to dry the gold powder in. Its been a while, but I think I just washed it out.

When the gold powder is dry, it is very clean and I can loosen any that clings to the bottom of the corningware dish by simply giving the dish a light swirl. The loose particles of gold hit the stuck particles and loosen the clinging pieces. Some may be stuborn, and I use a stainless steel spoon to pull any that sticks away from the dish.

I use the same stainless steel spoon to transfer the gold powder to the melt dish. I use a single melt dish for several melts, then retire it to inquarting when it starts to get dirty looking.

I would not use any sort of metal dish to dry your gold powder in. It seems that this could cause contamination - use a corningware casserole dish with a handle.



Oneal58 said:


> Question 2- I have a coule of ounces of silver nitrate from the silver drop with copper/urea



I'm not sure I understand this question. Do you have cemented silver metal that you recovered by putting copper in the solution and cementing the silver out? 

If you have powdered silver metal from cementing the silver out of silver nitrate solution with copper, then you can wash the silver powder and melt into a nice button depending on how much you have. 

It should be about 98% to 99% pure silver metal, depending on how careful you are about keeping small pieces of copper out of the silver during cementation with copper, and how thoroughly you wash the cemented silver powder.

Or you can wash it and put the silver powder in a jar and save it for later when you set up a silver cell. Then you can melt it into anode bars for your cell.

I melt all my cemented silver into anode bars for my silver cell.



Oneal58 said:


> What process do you use, other than to put into filter, run suction and pour hot water over silver until solution runs clear.



In the past, I have put the silver into a large (1000 ml or 2000 ml) beaker and kept adding boiling distilled water and stirring then pouring off the wash water - usually through a filter to catch any powder that tries to escape with the wash water. 

I did this over and over until all the color was gone. once the rinse water was clear, I then tested the wash water with some HCl. I take a small (10 or 20 ml) sample of the wash water and add a few drops of HCl to the sample. If there is still silver nitrate being washed out of the silver, then the sample will turn cloudy with silver chloride formation. When the sample of wash water stayed clear, I was confident that the silver powder was clean (of silver nitrate). Then I dry and melt or save the silver powder for later.

I still use a graphite mold I purchased of ebay. I have three identical molds. One is reserved for fine silver only, the next for fine gold only, and the third is for casting anode bars.

These molds have a slight taper to their sides, about 15 degrees if I remember correctly. This tapper allows the bars to slide right on out when you turn it over.



Oneal58 said:


> It is light, small, very easy to move around and can be attached to the beaker with little effort. It was only $16.00 if I remember correctly. It was sold to deflate large matresses with, do you think this suction pump would work



I don't have any experience with one of these, but I am guessing it is pretty light duty and probably would not last long working with the acids.

I use an HVAC pump 2.5 cfm I purchased from Harbor Freight. It is a nice heavy duty pump. From what I have read on this forum, the oil has additives that neutralize acids, but the oil must be changed frequently.

I used one for about 15 months before it finally froze up. I confess that I never changed the oil during that entire 15 month period. I just bought a new one and the price had increased from $79 last year to $109 in November 2011.

I plan to change the oil at least every couple of months on this one to see if I can make it last a little longer.

the gage is from a diesel engine test kit also from Harbor freight. It cost $14.95 last year. It has a nice big dial that is easy to read. I have a small petcock type valve right after the gage connection. I can throttle the vacuum going to my flask if I need to. 

The amount of suction I need varies from time to time. Sometimes I need just a little vacuum (like when I am washing cemented silver with boiling distilled water). I will turn the vacuum pump on and let it draw down to 10 or 15 inches Hg vacuum.

Other times I peg the gage at full vacuum (such as when filtering AuCl that has silver chloride in with it). Even then, with the vacuum gage pegged out, it can take hours to filter the AuCl. 

Having to endure one of these marathon filtering sessions due to silver chloride formation in my AuCl is great incentive to make sure that all the silver bearing liquid is removed (through careful washing) before dissolving the gold.

I hope you can glean some helpful tips from this post.

kadriver


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## Oneal58

Hi Everyone, thank you so much for sharing your knowledge.
Harold, I understand completely, *now*! I came to my senses, right after I added the silver to inquart that it just didn't make sense? I felt I had high quality, very clean gold and hadn't even ran it through your process of (making gold pure), yet? So why in the world would I put a foreign unwanted material back into the metal I sought after so diligently. Call it beginner's luck or maybe checking and triple checking the amount of silver I put into the gold with the inquarting formula I came through the process fine, this time, *but the last time*. I must have hit the nail on the head by blind luck, but I came through the inquarting with absolutely beautiful gold. Throughout all the HCL/Ammonia/HCL boils and washes I had a porduct that I could pour off the clear liquid almost void of any moisture and the gold stayed in a clump in the bottom of the beaker, didn't move at all. Easiest thing in the world to decant the liquid. I was expecting to have powder, it was not powder. I mentioned in an earlier post the gold looked granular. It stayed together almost like, (lack of a better phrase) it had magnetic properties? I didn't expect this and thought I had done something wrong? I really didn't feel good about the final product until I had the gold red hot in a ball in a new melting dish and seen it was void of any foreign material. I have watched enough videos on the subject that I seen I didn't have the crud, foreign materials that usually accompanied the gold that others had in their videos. That's why I didn't use any borax, no need for it. 
But yes, I understand, no need to inquart. A waste of time and creates a lot more trouble, not to mention that it extends the length of time to refine, considerably. 
Thanks Harold, Thanks Everyone! You are appreciated!
Oneal


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## Oneal58

Thank you Kadriver, I really do appreciate your help. Oneal58


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## Oneal58

Hi Butcher,
How are you today my old budddy, my old friend who's intellect is astounding on chemicals/refining/Etc;. Who has held my hand through the thick and thin, who was always there for me, no matter what! 
Now, I know, now you are saying, well what does he want now, he is baiting me up, he wants something? (Southern Slang)?  
Well, since you brought it up?  
I am getting low on Nitric. I have enough to run maybe 8 more ounces of gold filled but that's about it.
I have watched so many videos on making Nitric that I know them by heart. Have also read a lot on making it yourself. 
I know how you are about chemicals and trust your advice beyond compare!
Do you have a favorite process you use to make your Nitric. I have plenty of Potassium Nitrate Fertilizer, I haven't been able to find any Sodium Nitrate and I have looked. I have ammonium nitrate but from what I have been told, it's best to stay away from using it.
Could I impose on you and ask you which process you use while making your Nitric? I have a condenser and have bought the things I needed to condense with. But from what I am seeing I could get by with around 50% nitric, hoping I can get close to this and not have to condense? 
If I could get your personal recipie it would very much be appreciated? 
Thank you Butcher, if you feel you don't need to do this for some reason, it will be fully understood. I would just rather go with your directions than go with anything I have watched or read somewhere else. 
Thanks Butcher, 
Oneal58


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## butcher

Oneal, 
Below is one I posted, I really like it, one of my favorite’s actually I tried to explain this process I came up with, one on one of the first posts I made coming to the forum, I could not type then and was not very good at computers or the English and grammar, running all the sentences together (I may have gotten a little better now but sure you guys still have a hard time with my skills in this matter), I was a newbie, and had been lurking for a while before deciding to post, so I had an admiration of Harold, GSP, (Chris), Irons, Lou, and others, well I made my this first post trying to share my process, Harold chimed in saying he could not read a word I said, (man that hurt, I almost said to heck with this forum and quit then, but Ragbone chimed in, and calmed down my hurt pride, and I stuck with the forum trying to make my posts where Harold could read them), (Harold has taught me much not only in gold refining but in other walks of life, funny how a man who you have never seen, but you look up to can make such a difference in your life, never met Him but will always consider Him a friend and mentor
I also make nitric the cold method Laser Steve’s recipe, it is the best I have found (I have studied nitric intensely), this solution, works well for everything but silver (but you can distill it and then it is good for silver. So this is the method I suggest you begin with, there is also much information of this process here on the forum.

I have also made fuming nitric, but there is no need to make that or use that. 
So 68% is the strongest you need (used in aqua regia), and more dilute to remove base metals and silver.
Always distill homemade nitric for silver.
I have made many posts on the properties of nitric acid, how to concentrate it, and its azeotropic nature, I will not go into that again now,
There are other processes to make nitric, I will not mention now, as it would just clutter this page.

I can process gold plated pins and make nitric acid at the same time here is my favorite process “Kill two birds one rock”, the principles here have many uses not only with the process stated here, and can be adapted to other processes.

You can use lab glass, distilling rig, but I still use my old pickle jar.

Process for pins, nitric acid and copper sulfate
Kill two birds one stone

A few principles:
You need sulfuric acid with nitrate (salts) to create nitric acid,
Gold will not dissolve in nitric acid alone,
Copper will dissolve in nitric acid evolving NO2 gas. 
NO2 gas bubbled into water can form nitric acid.
NO2 + H2O --> HNO3
NO gas also evolves; oxygen will convert this to NO2,
NO + O2 --> NO2 
So: if we add a little H2O2 to this we have oxygen and water, we can convert NO gas to HNO3,
NO + H2O2 --> HNO3

Gold will not dissolve in copper nitrate or copper sulfate.
Nitric acid will evaporate from a solution at a much lower temperature than a sulfate will.
2 NaNO3 + H2SO4 --> Na2SO4 + 2HNO3 
Nitrate fertilizer + sulfuric acid àsodium sulfate + nitric acid.
In our case we are using copper to help.
Copper dissolving in nitric acid evolves NO2 and NO fumes.
Cu + 2 HNO3 --> CuNO3 + 2NO2(g) + 2 H2O
When we distill this copper nitrate we remove the Nitrate and leave the copper sulfate behind, diluting this to retrieve our un-dissolved gold.
Cu(NO3)2 + H2SO4 --> CuSO4 + 2HNO3
Copper sulfate is water-soluble.

(Copper sulfate solution we make here is soluble while hot, but will crystallize out as bright blue crystals if allowed to cool, (copper sulfate crystals once formed are harder to dissolve) than if we keep them hot while diluting the solution not allowing them to crystallize).

This is my method for pins (which can be adapted to distill copper nitrate solution to make nitric acid) or adapted for use with other chemicals and processes.

(This process can be adapted to other recovery or refining methods to kill two birds with one stone, like recovering nitric or aqua regia while dissolving karate gold)

A distilling unit rig (I have a nice lab distilling unit), but I like my homemade kit, and use it for this process, my unit has survived many distillations, but as with any distilling glass precautions must be observed,

Some supplies I use: 
(My Pickle jar distilling kit) 
Large pot with handles
Sand
Canning gallon pickle jar
A lid for gallon jar --made from 1/2" thick Teflon,(or the plastic wood they make decks out of HDPE I think) turned on a lath beveled edge to tightly fit jar, small lip on top edge, a hole in center for tight fit of 1/4" hose.
8' 1/4" Teflon hose
Long neck bottle
(For this bottle either loose fitting Teflon cork with hole or just use tape)
Gallon bucket of ice water
Double burner electric hot plate 
(Ground fault protected electrical outlet)
Fiberglass catch tray for burner to sit on to catch any spill
Pyrex coffee pot
Some wire, plumbers Teflon tape, cloth tape, electricians black tape
New battery sulfuric acid 10 cups, (we will boil down to 6 cups)
Cup of sodium or Potassium nitrate fertilizer
One pound of (copper) gold plated pins no solder (cut to expose copper to acid)
(Teflon will withstand temperature and fumes of these acids)
(A nearby box of baking soda and water for safety)

Required:
Understand the dangers of these acids, and precautions to take, understand the danger of the nitrous gases formed, and precautions to take, understand the principles of distilling and precautions needed, understand glass cannot withstand thermal shock (rapid temperature change).

Never cool or lower temperature to boiling reaction vessel without removing line to condenser,(which can cause suck back of cold solution into hot boiling flask breaking it through thermal shock),always remove tube before lowering heat on boiling flask,

Work outdoor using breeze or with fume hood, take safety precautions.

Double hotplate sits on fiberglass catch tray; ground fault electrical source is used outdoors

10 cups of sulfuric battery acid boiled down to 6 cups in the Pyrex coffee pot on one burner boil down to 6 cups and cool. To boil off some water in the acid, it will still contain some water (We will use this cool sulfuric acid later),
(We could also pour concentrated sulfuric acid drain cleaner into water to dilute it).

The large pot, pour a couple of inches of sand in bottom of it spread flat, the gallon canning pickle jar is sits on this sand centered in the large pot and sand poured in between pots metal and outside of pickle jar, to make a boiling reactor with a sand bath. This will help to protect our glass from thermal shock, (sand bath around pickle jar), allowing heat to change slowly, and can act as catch basin if we make a mistake. The 1/4" Teflon hose fits tightly into Teflon lid for our gallon pickle jar boiling reaction vessel, we will be collecting NOx gas from this vessel, so hose just in through the lid just a little ways, to capture gasses formed in reaction vessel.
(Later we will tape on this lid, and tie it down)
(Get tape and wire ready and handy within reach, we will need it as soon as acid is added later)
Get ice water in gallon bucket (plastic ok) this is for cooling our gases and condensing them, our collection bottle will sit in this bucket, 
Put small amount of water in the long neck bottle (collection bottle for condensed nitric acid) for NOx gas to bubble through water, (I add a little H2O2 peroxide to help conversion, it is not necessary), put one end of the Teflon 1/4" hose into this collection bottle all the way down into bottom of bottle so gases bubble through water and hydrogen peroxide inside, (through a loose fitting Teflon cork or else just tape hose to top of bottle, air, and some gas will need to escape from this bottle, and we do not want to prevent this with a tight fitting lid), this long neck bottle needs to sit down in iced water of bucket to condense gas to liquid, and we need to hold it down in ice water (it wants to float till it fills), so we tie in down into ice water bucket, this is our condenser receiver for the NOx fume's which will bubble into water in this longneck bottle and convert to nitric acid, a few loops of this hose is under ice water to help condense fumes also.

Set large pot sand bath with our fancy pickle jar boiler reaction vessel on cold electric hotplate, put one pound solder free (copper) gold plated pins, (cut to expose copper to acid I cut mine small for more exposure), in reaction vessel, add one cup of sodium nitrate fertilizer, (with lid and tape handy ready we will need to put on lid to contain brown NOx fumes in next step), pour in cooled 6 cups sulfuric acid on these, quickly put on Teflon fitting on lid and taping on the with Teflon plumbers tape first, then bandage cloth tape, then black electrical tape sealing this lid well, the insulated solid copper tie wire is tied to one handle of the pot over top of lid on jar and tied to other pot handle, this will hold down the lid when pressure builds, 
As soon as you pour the sulfuric acid on the nitrate fertilizer and copper, red brown nitrous gas NOx begins to form, so getting lid on quickly and taping to seal is needed, we will need no heat yet, as it creates its own heat from chemical reaction, turning burner on warm will start to heat pot and sand, with time, the heat will saturate sand and starts to warm the jar. When reaction slows (bubbling in receiver slows) and pot is warm raise heat a little, (little bit at a time) giving time for heat to reach and react chemicals as red fume slow, or gas bubble slow in receiver, we want a steady few bubbles, not too fast we only want the gas to go to the condenser and receiver. (There is a point to where nitric will concentrate to azeotrope in the boiling flask and reaction begins to get more vigorous with red fume’s of NOx gas), keeping a steady stream of bubble into our receiver is our goal, not liquid the blue liquids from our boiling flask).

Caution we do not want to change temperature on glass fast, this thermally shocks glass and will crack or break it, always keep this in mind.
Do not lower the temperature of the boiling vessel, with the hose in the condenser receiver, always remove this hose from the receiver first allowing it to suck air, (this higher temperature in the boiling vessel creates a pressure, and if we lower the temperature on this boiling vessel, it will go into a vacuum, this will suck the cooler condensed liquid back into this hot boiling flask, thus causing thermal shock and cracking our jar, by removing this hose first it just suck’s back air, and not liquid, as the pressure lowers in this boiler reaction vessel.

(I preheat a coffee pot of water, just below boil for procedure below, starting the water heating before hand)

We do not want to evaporate this now forming copper sulfate to a dry salt, we just want to drive out the formed nitric acid, so we evaporate to thick syrup, (I have noticed a color change from blue-green to blue-blue as the nitrates are driven out of the copper sulfate),
After we have evaporated down to syrup.

NOTE:
We want to remove hose from the condenser receiver, before lowering temperature.
(See caution on suck-back of these cooler liquids when lowering temperature of reaction vessel, thermal shock),
We can let cool before diluting this copper sulfate syrup, but this will form salts and it takes more water to dilute, (that may be best for you as this step if not done properly can thermally shock your boiling vessel), I use the water we heated above (on second burner in coffee pot, getting this water to about the same temperature of this syrup, and very slowly adding this boiling hot water to the syrup to dilute it, starting with just drops at a time, not pouring in all at once, this dissolves the blue copper sulfate syrup and leaves gold shells and powder from pins.
Allow this dilute copper sulfate liquid to settle the gold, and then decant liquid from gold and filter solution.

These gold foils will need further treatment to refine to pure gold.

This copper sulfate can be evaporated to nice blue crystals of copper sulfate for other chemical reactions, or for an electrolytic cell or other uses, wall mart sells them at a high price to keep roots from growing in sewer lines.

This nitric acid tested for strength, and evaporated to 68% concentration azeotrope if necessary, cool, stored in amber nitric bottle with proper lid put out of light (light breaks down nitric). Store in safe place for later use in recovery or refining

Distilling copper nitrate, (adding copper or gold plated copper can assist creating NOx fumes in boil, which also is a way I get gold plating from Pins. killing two birds one stone) would get nitric back from this copper chloride solution, bubble NOx gas into water, for dilute nitric, which can then evaporate water from dilute nitric until 68%HNO3 azeotrope, (many acids form azeotropes), so if just evaporating a dilute nitric solution, below the boiling point of the acid (for the concentration that the acid is at the time in solution), would boil off water (or other volatile components if in solution), making the acid more concentrated in solution, up to the azeotrope of the acid, which for nitric is about 68%, further boiling would only boil off the 68% solution till dry, meaning it cannot be further concentrated by this method, by using the boiling point information a person can have a good idea if they are boiling off acid or just water, the concentration can be tested with specific gravity, or judged by how it attacks metals.

(100% H2O) boils @100 degC density 1.00.
20% HNO3 density 1.115- boiling point 103 degC.
30% HNO3 density1.180 boiling point 107 degC. 
50% HNO3 density 1.310 boiling point 116 degC.
70% HNO3 density 1.413 boiling point 121.5 degC.

(Pure HNO3 boiling point is about 83 degC, so you can see the boiling point goes up as the nitric is less concentrated, till about 68% azeptrope (nitric acid’s highest boiling point about 120 degC), then as we get more dilute towards just water the boiling point falls toward the boiling point of water 100 degC).

As you can see the boiling points change with how concentrated the acid is. Keeping below the boiling point most all of your acid stays in solution, and mostly water vapors off, above the boiling point acid leaves solution in vapors with the water. 
Other acids and have reaction similar to this. For more information you can study the azeotrope of acid, boiling points, acid concentrating, I have also posted this information on forum in other posts.

{Basically we made nitric acid with nitrate fertilizer and sulfuric acid, nitric acid distilled off in condenser bottle, the copper helping to drive the reaction, dissolved copper from the gold making copper nitrate in solution in boiling vessel, and since we had a slight excess of sulfuric when we distilled out the nitric fumes (making nitric acid ) we left sulfuric acid in boiling flask which forms copper sulfate solution, and gold foils, which we will dilute the copper sulfate with boiling hot water before allowing to cool so we can seperate gold foils from copper sulfate solution}.


I have added some points to this post today; here was the one posted and some questions answered about it,

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=38&t=6199&hilit=kill+two+birds+one+rock

Read and understand dangers involved before attempting, this method it is safe I have done it many times, but precautions must be taken, and dangers must be taken into account.

My hope is this is readable and understandable, and someone will gain information or it will spark ideas in others.

Butcher


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## Oneal58

Hi Butcher, I appreciate it buddy, I knew you could be counted on! You truely are a wonderful person and I appreciate you! 
Butcher, I follow 95% of the process but have a few questions here and there. Mainly just on quantities/expected returns/ weights of gold pins/plus copper, Etc;. such things as that. Maybe the size of the long neck bottle (wine?) and how much water to put into it, such things as that. Just the odds and ends of the process. But let me gather up everything I need and put it together and I will make sure and clear up that other 5% before I even think about starting up, I promise.
I got to get me a double burner, been looking for one at the consignment shops (like Kadriver found) that lucky rascle, but haven't found one. I will have to look at it like this, by the time I go by a few gallons of nitric I will have bought a double burner a couple of times over. Butcher the Nitric I have been using is around 68% industrial grade ( I think) so the strength sounds good to me. I don't think I would need anything stronger unless something changes? I got my mind on Platinum already but that's another story. There are several Salvage Yards (hundreds of cars of all kinds) right around me with all the salvage title car/truck rebuilder's in this area. But I haven't even touched on what's involved there yet. Had my hands full with what I have going on now. 
Give me a few (or more)days and I will get back with you. 
I got to start building my grandaughter a playhouse tomorrow for Christmas. That will take me a week I am sure. Got to keep it hid from her as well, so that's a problem. I guess I will build it behind the old house where she knows not to go near. That might work. Anyway, my daughter keeps changing the plan on me. It started out being about 70 sq. feet and now it's up to 110. I told her is she didn't stop messing with the plans I might as well build her a new house!
But thanks Butcher, I really,really, appreciate you. 
I will be back on in a few hopefully, if I can keep my daughter from changing those plans anymore. 
Talk at you later Butcher, THANKS!!!
Oneal


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## butcher

My hot plates have solid Iron burners with heating coil under iron plate I like these better than the type kadriver uses (coil type burner), I believe the heat is distributed more evenly (less likely for hot spots on cookware, I get mine for just a little over twenty dollars new at BiMart store, I also grab one if I find it in second hand store for a few dollars, you could also use a propane or gas burner with the sand bath.

If using the coil type electric burner or gas type burner I would put a steel plate, or wire screen between burner and cookware to distribute heat evenly.

That is a big playhouse maybe we can see a picture of it with that cutie bug of yours smiling big inside it?


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## Oneal58

Hi Butcher, you got it. I will send you one through a personal email. I am so protective of her I just don't want her picture out there on the web, if you know what I mean? I trust everyone on the site, but now and again you have visitor's come through that you just don't know about. I guess I watch too much news about missing or worse children. I would not allow my daughter to put herself or the kids on facebook or any place else for that matter.
If I could get my hands on that kind of person that would hurt a child, well, that's all I need to say about that! I am sure you can understand why I am like that by her and my grandson. But I promise to send you a picture day of or day after Christmas. I am sure my daughter is going to keep me busy on this thing right on up to Christmas Eve. She is just too much like me I guess. 
Every project I start, I say I am going to keep it simple. It always ends up on the upper end of rediculous. 
Got to go to work on it now. It's just warmed up enough for me to get outside. Cold snap here, unusual for here this time of year? It's still in the low 40's outside, that's cold for here and for me at my age, with the blood thinners I am on. 
Talk at you later. 
Oneal


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## The Refiner49er

Butcher-

I must say that you have made some really great posts regarding nitric acid, manufacturing and recycling/reuse of refining byproducts, and other dynamic methodology. Thanks for the boiling point references.

John


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## butcher

John thanks, just trying to share what I learn, this forum and members here have taught me so much, I just want to try and give some tidbits back.

Oneal,
I do understand your not wanting your little angels picture for the world to see, and it is a shame that-that evil does exist, I too would not put a man who would hurt an innocent child behind bars and feed him, even torture or death, may be too kind for that kind of slime of man and the earth.

Only problem being out there building the playhouse is your granddaughter is missing her gramps spending time with her, maybe you can have her help you build some parts of the playhouse, do not tell her what it is she is building, like a wall door or window, these parts you could take around back and install them without here seeing the building going up, and when she finally sees her playhouse and the window she helped her grand pappy build she will like it even more, as she had fun and learned working with you, and also sees her work in her little house, she could also help grandmamma make the curtains for her window, not knowing what she is sewing. Since this forum is about gold I should keep to the subject about gold, I think the smile on her face when she sees her playhouse will be pretty and golden.


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## Oneal58

Hi Butcher, 
I hope you and your family (as well as everyone else here on the site) had a wonderful Christmas and I wish you'all a Happy New Year!
I finally got the playhouse for my grandaughter finsihed at 4:00 a.m., Christmas morning. On top of that I have had to work with a case of the flu the last couple of days. I have been in bed ever since. I have just gained enough strength to say hello to everyone and say that I will be back to my aggravating self hopefully in a couple of days asking questions again.
Butcher, I hope to start up on the process of making the nitric acid with your instructions you posted for me. I just want to clarify a couple of things before I get started. 
Question 1- I don't have any gold plated pins, but have plenty of copper tubing. I have plenty of god filled jewelry but I don't know what the metal content of the jewelry is? If I saw the tubing into 1/4 inch sections will this be OK to use, only?
Question 2-I have a really long neck bottle, one of these that has been heated and stretched, if you have ever seen one? Will this work, probably 18-20 inches tall. Does the distance that the Noxx gases has to bubble through the water/peroxide make a difference. In your opinion how many inches of water/peroxide do I need in the condensor bottle? Percentage of %peroxide to %water? WIll the 3% peroxide from Walmart do the job or do I need to condense the peroxide? 
Question 3- In the gallon pickle jar? How high up on the pickle jar reactor do I need to pour the sand up to? And just to veryify, keep 2 inches of sand beneath the jar while heating, is this correct?
Question 4- About how much nitric do I expect to condense from the quantities given in the instructions below. Also have you ever tried making twice the amount at one time? 

Question 5 - This question has nothing to do with making nitric, but I am confused about driving off excess nitric in other solutions?
Temperature, when driving off Nitric acid from solution I can tell what temperature the solution is by when the solution boils with nitric in it? If I am trying to drive off nitric by evaporating, I must make the solution boil to drive off the nitric? Gradually lowering the temperature as nitric is being driven off, is this correct? 
Question 6-Also, will a floating glass thermometer work here? If not what type thermometer do you use? 
Butcher I hope to feel good enough to get started on this tomorrow or maybe the next. I still have a fever and feel weak but can't wait to get back to refining. Thank you for your continued support Butcher. I am going to send you a picture of my little angel's playhouse today if I can get the engery to go take the picture. 
Thanks Butcher,
Oneal

Question


butcher said:


> Oneal,
> Below is one I posted, I really like it, one of my favorite’s actually I tried to explain this process I came up with, one on one of the first posts I made coming to the forum, I could not type then and was not very good at computers or the English and grammar, running all the sentences together (I may have gotten a little better now but sure you guys still have a hard time with my skills in this matter), I was a newbie, and had been lurking for a while before deciding to post, so I had an admiration of Harold, GSP, (Chris), Irons, Lou, and others, well I made my this first post trying to share my process, Harold chimed in saying he could not read a word I said, (man that hurt, I almost said to heck with this forum and quit then, but Ragbone chimed in, and calmed down my hurt pride, and I stuck with the forum trying to make my posts where Harold could read them), (Harold has taught me much not only in gold refining but in other walks of life, funny how a man who you have never seen, but you look up to can make such a difference in your life, never met Him but will always consider Him a friend and mentor
> I also make nitric the cold method Laser Steve’s recipe, it is the best I have found (I have studied nitric intensely), this solution, works well for everything but silver (but you can distill it and then it is good for silver. So this is the method I suggest you begin with, there is also much information of this process here on the forum.
> 
> I have also made fuming nitric, but there is no need to make that or use that.
> So 68% is the strongest you need (used in aqua regia), and more dilute to remove base metals and silver.
> Always distill homemade nitric for silver.
> I have made many posts on the properties of nitric acid, how to concentrate it, and its azeotropic nature, I will not go into that again now,
> There are other processes to make nitric, I will not mention now, as it would just clutter this page.
> 
> I can process gold plated pins and make nitric acid at the same time here is my favorite process “Kill two birds one rock”, the principles here have many uses not only with the process stated here, and can be adapted to other processes.
> 
> You can use lab glass, distilling rig, but I still use my old pickle jar.
> 
> Process for pins, nitric acid and copper sulfate
> Kill two birds one stone
> 
> A few principles:
> You need sulfuric acid with nitrate (salts) to create nitric acid,
> Gold will not dissolve in nitric acid alone,
> Copper will dissolve in nitric acid evolving NO2 gas.
> NO2 gas bubbled into water can form nitric acid.
> NO2 + H2O --> HNO3
> NO gas also evolves; oxygen will convert this to NO2,
> NO + O2 --> NO2
> So: if we add a little H2O2 to this we have oxygen and water, we can convert NO gas to HNO3,
> NO + H2O2 --> HNO3
> 
> Gold will not dissolve in copper nitrate or copper sulfate.
> Nitric acid will evaporate from a solution at a much lower temperature than a sulfate will.
> 2 NaNO3 + H2SO4 --> Na2SO4 + 2HNO3
> Nitrate fertilizer + sulfuric acid àsodium sulfate + nitric acid.
> In our case we are using copper to help.
> Copper dissolving in nitric acid evolves NO2 and NO fumes.
> Cu + 2 HNO3 --> CuNO3 + 2NO2(g) + 2 H2O
> When we distill this copper nitrate we remove the Nitrate and leave the copper sulfate behind, diluting this to retrieve our un-dissolved gold.
> Cu(NO3)2 + H2SO4 --> CuSO4 + 2HNO3
> Copper sulfate is water-soluble.
> 
> (Copper sulfate solution we make here is soluble while hot, but will crystallize out as bright blue crystals if allowed to cool, (copper sulfate crystals once formed are harder to dissolve) than if we keep them hot while diluting the solution not allowing them to crystallize).
> 
> This is my method for pins (which can be adapted to distill copper nitrate solution to make nitric acid) or adapted for use with other chemicals and processes.
> 
> (This process can be adapted to other recovery or refining methods to kill two birds with one stone, like recovering nitric or aqua regia while dissolving karate gold)
> 
> A distilling unit rig (I have a nice lab distilling unit), but I like my homemade kit, and use it for this process, my unit has survived many distillations, but as with any distilling glass precautions must be observed,
> 
> Some supplies I use:
> (My Pickle jar distilling kit)
> Large pot with handles
> Sand
> Canning gallon pickle jar
> A lid for gallon jar --made from 1/2" thick Teflon,(or the plastic wood they make decks out of HDPE I think) turned on a lath beveled edge to tightly fit jar, small lip on top edge, a hole in center for tight fit of 1/4" hose.
> 8' 1/4" Teflon hose
> Long neck bottle
> (For this bottle either loose fitting Teflon cork with hole or just use tape)
> Gallon bucket of ice water
> Double burner electric hot plate
> (Ground fault protected electrical outlet)
> Fiberglass catch tray for burner to sit on to catch any spill
> Pyrex coffee pot
> Some wire, plumbers Teflon tape, cloth tape, electricians black tape
> New battery sulfuric acid 10 cups, (we will boil down to 6 cups)
> Cup of sodium or Potassium nitrate fertilizer
> One pound of (copper) gold plated pins no solder (cut to expose copper to acid)
> (Teflon will withstand temperature and fumes of these acids)
> (A nearby box of baking soda and water for safety)
> 
> Required:
> Understand the dangers of these acids, and precautions to take, understand the danger of the nitrous gases formed, and precautions to take, understand the principles of distilling and precautions needed, understand glass cannot withstand thermal shock (rapid temperature change).
> 
> Never cool or lower temperature to boiling reaction vessel without removing line to condenser,(which can cause suck back of cold solution into hot boiling flask breaking it through thermal shock),always remove tube before lowering heat on boiling flask,
> 
> Work outdoor using breeze or with fume hood, take safety precautions.
> 
> Double hotplate sits on fiberglass catch tray; ground fault electrical source is used outdoors
> 
> 10 cups of sulfuric battery acid boiled down to 6 cups in the Pyrex coffee pot on one burner boil down to 6 cups and cool. To boil off some water in the acid, it will still contain some water (We will use this cool sulfuric acid later),
> (We could also pour concentrated sulfuric acid drain cleaner into water to dilute it).
> 
> The large pot, pour a couple of inches of sand in bottom of it spread flat, the gallon canning pickle jar is sits on this sand centered in the large pot and sand poured in between pots metal and outside of pickle jar, to make a boiling reactor with a sand bath. This will help to protect our glass from thermal shock, (sand bath around pickle jar), allowing heat to change slowly, and can act as catch basin if we make a mistake. The 1/4" Teflon hose fits tightly into Teflon lid for our gallon pickle jar boiling reaction vessel, we will be collecting NOx gas from this vessel, so hose just in through the lid just a little ways, to capture gasses formed in reaction vessel.
> (Later we will tape on this lid, and tie it down)
> (Get tape and wire ready and handy within reach, we will need it as soon as acid is added later)
> Get ice water in gallon bucket (plastic ok) this is for cooling our gases and condensing them, our collection bottle will sit in this bucket,
> Put small amount of water in the long neck bottle (collection bottle for condensed nitric acid) for NOx gas to bubble through water, (I add a little H2O2 peroxide to help conversion, it is not necessary), put one end of the Teflon 1/4" hose into this collection bottle all the way down into bottom of bottle so gases bubble through water and hydrogen peroxide inside, (through a loose fitting Teflon cork or else just tape hose to top of bottle, air, and some gas will need to escape from this bottle, and we do not want to prevent this with a tight fitting lid), this long neck bottle needs to sit down in iced water of bucket to condense gas to liquid, and we need to hold it down in ice water (it wants to float till it fills), so we tie in down into ice water bucket, this is our condenser receiver for the NOx fume's which will bubble into water in this longneck bottle and convert to nitric acid, a few loops of this hose is under ice water to help condense fumes also.
> 
> Set large pot sand bath with our fancy pickle jar boiler reaction vessel on cold electric hotplate, put one pound solder free (copper) gold plated pins, (cut to expose copper to acid I cut mine small for more exposure), in reaction vessel, add one cup of sodium nitrate fertilizer, (with lid and tape handy ready we will need to put on lid to contain brown NOx fumes in next step), pour in cooled 6 cups sulfuric acid on these, quickly put on Teflon fitting on lid and taping on the with Teflon plumbers tape first, then bandage cloth tape, then black electrical tape sealing this lid well, the insulated solid copper tie wire is tied to one handle of the pot over top of lid on jar and tied to other pot handle, this will hold down the lid when pressure builds,
> As soon as you pour the sulfuric acid on the nitrate fertilizer and copper, red brown nitrous gas NOx begins to form, so getting lid on quickly and taping to seal is needed, we will need no heat yet, as it creates its own heat from chemical reaction, turning burner on warm will start to heat pot and sand, with time, the heat will saturate sand and starts to warm the jar. When reaction slows (bubbling in receiver slows) and pot is warm raise heat a little, (little bit at a time) giving time for heat to reach and react chemicals as red fume slow, or gas bubble slow in receiver, we want a steady few bubbles, not too fast we only want the gas to go to the condenser and receiver. (There is a point to where nitric will concentrate to azeotrope in the boiling flask and reaction begins to get more vigorous with red fume’s of NOx gas), keeping a steady stream of bubble into our receiver is our goal, not liquid the blue liquids from our boiling flask).
> 
> Caution we do not want to change temperature on glass fast, this thermally shocks glass and will crack or break it, always keep this in mind.
> Do not lower the temperature of the boiling vessel, with the hose in the condenser receiver, always remove this hose from the receiver first allowing it to suck air, (this higher temperature in the boiling vessel creates a pressure, and if we lower the temperature on this boiling vessel, it will go into a vacuum, this will suck the cooler condensed liquid back into this hot boiling flask, thus causing thermal shock and cracking our jar, by removing this hose first it just suck’s back air, and not liquid, as the pressure lowers in this boiler reaction vessel.
> 
> (I preheat a coffee pot of water, just below boil for procedure below, starting the water heating before hand)
> 
> We do not want to evaporate this now forming copper sulfate to a dry salt, we just want to drive out the formed nitric acid, so we evaporate to thick syrup, (I have noticed a color change from blue-green to blue-blue as the nitrates are driven out of the copper sulfate),
> After we have evaporated down to syrup.
> 
> NOTE:
> We want to remove hose from the condenser receiver, before lowering temperature.
> (See caution on suck-back of these cooler liquids when lowering temperature of reaction vessel, thermal shock),
> We can let cool before diluting this copper sulfate syrup, but this will form salts and it takes more water to dilute, (that may be best for you as this step if not done properly can thermally shock your boiling vessel), I use the water we heated above (on second burner in coffee pot, getting this water to about the same temperature of this syrup, and very slowly adding this boiling hot water to the syrup to dilute it, starting with just drops at a time, not pouring in all at once, this dissolves the blue copper sulfate syrup and leaves gold shells and powder from pins.
> Allow this dilute copper sulfate liquid to settle the gold, and then decant liquid from gold and filter solution.
> 
> These gold foils will need further treatment to refine to pure gold.
> 
> This copper sulfate can be evaporated to nice blue crystals of copper sulfate for other chemical reactions, or for an electrolytic cell or other uses, wall mart sells them at a high price to keep roots from growing in sewer lines.
> 
> This nitric acid tested for strength, and evaporated to 68% concentration azeotrope if necessary, cool, stored in amber nitric bottle with proper lid put out of light (light breaks down nitric). Store in safe place for later use in recovery or refining
> 
> Distilling copper nitrate, (adding copper or gold plated copper can assist creating NOx fumes in boil, which also is a way I get gold plating from Pins. killing two birds one stone) would get nitric back from this copper chloride solution, bubble NOx gas into water, for dilute nitric, which can then evaporate water from dilute nitric until 68%HNO3 azeotrope, (many acids form azeotropes), so if just evaporating a dilute nitric solution, below the boiling point of the acid (for the concentration that the acid is at the time in solution), would boil off water (or other volatile components if in solution), making the acid more concentrated in solution, up to the azeotrope of the acid, which for nitric is about 68%, further boiling would only boil off the 68% solution till dry, meaning it cannot be further concentrated by this method, by using the boiling point information a person can have a good idea if they are boiling off acid or just water, the concentration can be tested with specific gravity, or judged by how it attacks metals.
> 
> (100% H2O) boils @100 degC density 1.00.
> 20% HNO3 density 1.115- boiling point 103 degC.
> 30% HNO3 density1.180 boiling point 107 degC.
> 50% HNO3 density 1.310 boiling point 116 degC.
> 70% HNO3 density 1.413 boiling point 121.5 degC.
> 
> (Pure HNO3 boiling point is about 83 degC, so you can see the boiling point goes up as the nitric is less concentrated, till about 68% azeptrope (nitric acid’s highest boiling point about 120 degC), then as we get more dilute towards just water the boiling point falls toward the boiling point of water 100 degC).
> 
> As you can see the boiling points change with how concentrated the acid is. Keeping below the boiling point most all of your acid stays in solution, and mostly water vapors off, above the boiling point acid leaves solution in vapors with the water.
> Other acids and have reaction similar to this. For more information you can study the azeotrope of acid, boiling points, acid concentrating, I have also posted this information on forum in other posts.
> 
> {Basically we made nitric acid with nitrate fertilizer and sulfuric acid, nitric acid distilled off in condenser bottle, the copper helping to drive the reaction, dissolved copper from the gold making copper nitrate in solution in boiling vessel, and since we had a slight excess of sulfuric when we distilled out the nitric fumes (making nitric acid ) we left sulfuric acid in boiling flask which forms copper sulfate solution, and gold foils, which we will dilute the copper sulfate with boiling hot water before allowing to cool so we can seperate gold foils from copper sulfate solution}.
> 
> 
> I have added some points to this post today; here was the one posted and some questions answered about it,
> 
> http://goldrefiningforum.com/phpBB3/viewtopic.php?f=38&t=6199&hilit=kill+two+birds+one+rock
> 
> Read and understand dangers involved before attempting, this method it is safe I have done it many times, but precautions must be taken, and dangers must be taken into account.
> 
> My hope is this is readable and understandable, and someone will gain information or it will spark ideas in others.
> 
> Butcher


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## The Refiner49er

Oneal-

I will let Butcher answer the bulk of your questions, but from everything I know you should not boil a solution to effect evaporation. Boiling may cause you to lose values, keep in mind that with any pregnant solution if small particles or mist manage to escape the container, any dissolved metals shall be included, and with a highly concentrated solution the losses can be substantial. For depleting nitric, I believe the very best method is what Harold advises, specifically to place a 24K gold button in the solution AFTER filtering during the final stage of AR to consume the excess nitirc. I myself have adapted this strategy when I am in a hurry, by using gold powder from a previous precipitation, and whatever does not dissolve simply contributes to the weight of the new batch. Either way you can weigh whatever gold is used to keep your yield calculations accurate.

In regards to a way of measuring temperature, I personally like a "point and shoot" infrared thermometer, and Harbor Freight Tools has one that is fairly inexpensive at $30 TO $40. Of course this reads surface temp and not the actual liquid, but still a great way to keep tooling out of the acids and very fast/easy to use.

Hope you feel better soon.


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## butcher

Question 1- I don't have any gold plated pins, but have plenty of copper tubing. I have plenty of gold-filled jewelry but I don't know what the metal content of the jewelry is? If I saw the tubing into 1/4-inch sections will this be OK to use, only?

ANS.
The process killing two birds with one stone, making nitric acid and removing gold from pins is best used when you have gold pins to process, it would work using copper but in my opinion unless you needed copper sulfate, it would be a waste of material, time and trouble, to just use this method to make nitric unless your de-plating gold from copper,

In this case I would use Laser Steve’s poor mans cold nitric recipe, following all of its instructions and then distill the nitric acid if usinit for silver.

Dilute nitric acid can be concentrated to 68% by evaporation, but for most processes we dilute nitric any way.
Question 2-I have a really long neck bottle, one of these that has been heated and stretched, if you have ever seen one? Will this work, probably 18-20 inches tall. Does the distance that the Nox gases have to bubble through the water/peroxide make a difference. In your opinion how many inches of water/peroxide do I need in the condenser bottle? Percentage of %peroxide to %water? Will the 3% peroxide from Wal-Mart do the job or do I need to condense the peroxide? 

ANS
You only want as little water and peroxide as possible, if your using 35 peroxide I would only use that without water as it already mostly water, the longer the bubbles stay in solution the better the gas and water convert to nitric acid, but then the more water you add the more you dilute the nitric acid, starting with as little water as possible in receiver, that the gas has to bubble into in my opinion is best, as the very first portion to distill over will add water to your receiver as time goes on the bottle fills there is more solution for the gasses to bubble into, when making several batches I will use previous batch of nitric which gives me more volume of liquid for bubbles to flow through, also a dilute solution of nitric can also be used to bubble the NOx gases into to some what concentrate the dilute solution and convert NOx gases into more nitric acid.


Question 3- in the gallon pickle jar? How high up on the pickle jar reactor do I need to pour the sand up to? And just to verify, keep 2 inches of sand beneath the jar while heating, is this correct?


ANS 
A couple of inches of sand for jar to sit on and I would put sand almost up to level of the solution in jar, the height here is not that critical, you just do not want jar to touch sides of pot and create hot spots, also being able to see the reaction in jar is nice feature.
Question 4- about how much nitric do I expect to condense from the quantities given in the instructions below. Also have you ever tried making twice the amount at one time? 

The distilling (boiling reactor need room for expansion of liquids, foaming and so on you do not want to fill the vessel very full, and have solutions boil over into your condenser, the ratio’s I gave for the pickle jar worked well for me, after many experiments these seemed to be best proportions for this.
If your distilling just nitric acid I would say keep the solution less than one third volume, the more room in vessel for expansion and foaming the better.

Question 5 - This question has nothing to do with making nitric, but I am confused about driving off excess nitric in other solutions?
Temperature, when driving off Nitric acid from solution I can tell what temperature the solution is by when the solution boils with nitric in it? If I am trying to drive off nitric by evaporating, I must make the solution boil to drive off the nitric? Gradually lowering the temperature as nitric is being driven off, is this correct? 

ANS
No need to boil, if you see some fumes coming off solution when heating these fumes are forming gases from liquids in solution, vapors of liquids will vapor off way below a solutions boiling point, as the solution concentrates the boiling point of solutions also change (as will the point of evaporation), 

Nitric acid in solution once the solution concentrates in the evaporation dish will get to a point where the nitric wants to boil over all of a sudden (when getting concentrated I pay very close attention watching for the very small bubble that form on outer edge of solution these small bubble give me the clue I am at this point of boil over, lowering heat at this point and having my mist water bottle handy to mist with water saves me from boil over at this point (after this reaction completes I can usually raise heat back to where I get good evaporation of gas fumes and do not have to worry about boil over again.

Question 6-Also, will a floating glass thermometer work here? If not what type thermometer does you use? 


ANS
I normally do not use a thermometer, but when I do just to see what is going on I use an infrared thermometer, it allows me to just point at several places and see what temperatures they are (thermometer in not necessary but can be nice feature).

Butcher I hope to feel good enough to get started on this tomorrow or maybe the next. I still have a fever and feel weak but can't wait to get back to refining. Thank you for your continued support Butcher. I am going to send you a picture of my little angel's playhouse today if I can get the energy to go take the picture. 


We hope you get to feel much better soon.


Edit to help clarify a point:
When distilling we do boil a solution to form gases capturing the gases, but we do not want to boil to the point we get carry over of the solution that will contaminate or receiver vessel with substances we are trying to leave behind in the boiling reaction vessel.

When evaporating a solution to concentrate or to remove one component as a gas, we do not want to boil only evaporate the solutions, heating to the point of gases rising (fumes) from solution, very small reaction bubbles are ok, but these are different from large popping bubble’s of a boiling solution.


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## Oneal58

Hi Everyone, thanks for the clarifications on the nitric production. 
I have another problem now. I felt good enough to go over to the old house last night. I had a batch of AR ready to evaporate and finish up. I evaporated down to syrup, added Hydrochloride a couple of times, evaporated off then added a few drops of sulphuric for the last evaporation. Added 4 times the amount in distilled water and left to sit overnight. It got down to 31degrees F. last night, very cold for here. Anyway, I went over just a while ago and added the Sodium Metabisulfate (Stump Out). I used warm distilled water to dissolve the Sodium Metabisulfate. I added 4 teaspoons not wanting to come up short because this was my largest refine yet. I added maybe 1/4 of the Sodium Metabisulfate while stirring vigorously and nothing happened, I added more and the AR turned dark brown. Just like it did with my first refine. I thought I would see the gold droping out of solution. The gold drop never happened? I added the remaining Sodium Metabisulfate and still no drop. Thinking that my AR may be heavy laden with gold causing this, I mixed up another batch of Sodium Metabisulfate and poured in about 1/4 of it still stirring vigorously. Nothing happened, I poured in another 1/4 and still no drop. I have gold floating on top of solution and in solution but not dropping. The floating gold powders flock together for some reason? My solution was very cold, probably near freezing 34 Degree F. I was adding warm/hot Sodium Metabisulfate to the near freezing gold bearing solution. Thinking that I had put more than enough of Sodium Metabisulfate in to do the job I stopped and came in. So this is where I am at, a beaker full of Sodum Metabisulfate, Approximately 6 teaspoons in 800ml of fluid. Brown colored liquid that will not settle out. 
*Question 1*- Where did I go wrong and how do I correct it? Did I not get all the nitric out of the AR solution last night or did I have left over Hydrochloric and or Sulphuric that caused this? 
*Question 2*-Should I have warmed the AR before I tried to drop the gold? 
*Question 3*- I expect I have near 1/2 ounce of gold in this batch so I sure do not want to lose it. To correct this do I evaporate off all the Sodium Metabisulfate, down to powder and start over again? I can't figure out why the gold will not drop out of solution with more than enough Sodium Metabisulfate to do the job. 
*Question 4*- If I evaporate off all the liquid, I still have the Sodium Metabisulfate in with the gold now, right? 
Thank Everyone for your help, it really is appreciated.

NOTE! UPDATE, I went back over to the building. It had been about 2 hours or so. The Gold powders are starting to drop, the solution isn't clear but I can tell that the gold is droping out of solution. The scent of Sodium Metabisulfate is very strong in solution. I really don't think that I didn't put enough to do the job? By morning I suspect that all the gold should be droped but I still have the floaters. I stirring the top part of solution to try and get some of the floating gold to drop. I had some success with this but some refuses to drop from top of solution.
I thought I would wait untill morning to test solution with stannous chloride. The solution looks funny, not like the first gold drop I did. I have brown powders sticking to the sides of the vessel, especially at the level the solution is at (top). I washed and cleaned the vessel very good with Dawn detergent before I decanted the solution so I had a clean vessel. Still don't know what happened?
Thank you so much for your help. 
Oneal


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## butcher

Oneal,
You may go out later and find the brown powders settled (maybe with excess SMB), if not I would try adding just a little HCl and a good boil then let it cool and sit overnight see if that works to precipitate the gold, if nothing else you can use cementing on copper to recover the gold.

Did you filter before precipitation?
If it filtered easily tin is not your trouble.

Was solution a nice yellow, or at least yellow with just a hint of green, if so base metals are probably not your trouble?

You may have had low acid content in the gold salts?
Or may just have not given enough time for the reaction to complete under the conditions?


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## Oneal58

Hi Butcher, 
This was the second run on the AR. What I mean is that I had already added Hydrochloride and a few drops of sulphuric to the AR. Then distilled water and let sit overnight. The next morning I had a good bit of either tin/silver or lead in the bottom of the vessel after the first evaporation. So,this concerned me, I then decided to go back through the process again because of the amount of tin/lead I had from the first run. I was afraid I had tin/lead that carried over. So, I went back to the batch to make a second run/evaporation which was last night. This morning I only had just a little dusting of tin/lead in the bottom of the vessel. I had a nice clear yellow solution, much better than the first evaporation. The solution filtered about as fast as I wanted to pour it. I couldn't see any particulate in the second solution and was pleased with the result. I was expecting good results because of all the steps I had been through with this batch. 
*Question 1*- Can you overwork a batch of AR? I mean doing what I did instead of going ahead and dropping the gold the first time and then refine again. Which should I have done, just go ahead and drop after the first evaporation and do another refine or do what I did. What concerned me was seeing all the tin/lead or silver that had dropped out of the first AR. Did I overwork the solution taking the gold salts out of solution?
*Question 2*- I have went back out and taken another look at the solution. The solution is nearly clear now. Will it hurt to leave the Sodium MetaBisulfate in the vessel overnight. Will any of the Sodium MetaBisulfate crystalize out in the cold tonight or will it stay in solution?
But I did add Hydrochloride many times, not just 2 times. Probably 4 times, I wanted to make sure I got all the unwanted metals out. I added sulphuric a couple of times also. 
So, I guess the big question is, did I cause this due to going through too many steps to clean the solution? Should I have just went ahead and dropped the gold on the first evaporation and then just do another refine on the gold button instead of doing what I did?
Which would have been the quickest and easiest to do?
*Question 3*- Is there a sure fire way to tell when you have depleted all the nitric out of a solution short of dropping a pure gold button into the solution? If not, when you drop a pure gold button into a solution will you be able to tell if the nitric is spent because of no reaction at the button? Or do you just leave the button in overnight to be sure all the nitric has been depleted.
*Question 4*- Puzzled, if nitric will not dissolve high karated gold unless inquarted to around 75% silver, why would you put 24K gold into it (nitric) and expect a reaction? I have not refined any karated gold yet but am puzzled by this? 

Thanks Butcher for your time and help.
Oneal


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## butcher

Oneal. 
I am unsure what you mean can you overwork a gold solution.

Lets say we had a jar of water and we added salt, until we could no longer make salt dissolve, now we evaporated one of the volatile components in this solution (water), until we made a syrup of salt water,(note the salt like gold in our solution does not leave on evaporation),now we can add back water and redo this as many times as we want (unless we boiled too strongly and splashed some salt out we would still have as much salt as we started with.

Now our solution of gold similar to this salt water above except we have three components (besides mixes of these forming gases), water, nitric, and HCl, and in this order are they volatile in solution (not that they will evaporate as pure substances but the fumes of evaporation will mainly be composed of on of these in this order).

The way whisky is distilled the first distillation is more "rich" in the volatile gas,(higher proof) and if we condensed this gas(alcohol) (and did not drink it), and then redistilled it we could get higher proof the second or third time of condensing and redistilling, this same alcohol, (each cycle) a higher alcohol in condensate and less water is in fumes each cycle, and each cycle leaving a richer solution of water behind in the boiling vessel.
Also on the first run distillation the alcohol content is higher the first portion of gas in the beginning of the distillation, as the alcohol is distilled from the boiling pot the boiling point of solution also changes, and more water also vapors over with the later portions being distilled.

So when we evaporate out aqua regia the first fumes are higher in water content, as we proceed the fumes become higher in nitric, and upon concentration the fumes become high in HCl, but as we said these gases do not come out as pure substance and we may still have some nitric in our gold chloride syrup (some of this may have made nitrate salts I'm not sure), adding HCl we replace some of the HCl we may have boiled out from concentrating the solution (remember we are making a gold salt chloride that needs the Cl- from our acid with the Au+), (also the acid may help to change any nitrate salts forming back into HNO3 in solution) (which may be why we may see NOx brown fumes on addition of acid to the concentrated solution of gold salts, I am just guessing here), this also helps to keep solution acidic, and gold in solution as salts, also the HCl is 20%acid and 80%water so here we also diluted our gold salts (and also diluted any remaining nitric in solution).
So you can see we do not need to add high volumes of HCl after we do the first evaporation, adding excess HCl just means we need to evaporate off more water before the remaining nitric comes over again. Now with some more evaporation of this thick syrup wetted with some HCl evaporates off water mostly at first the after most of water is evaporated the fumes become more rich in remaining nitric then HCl. after this we add HCL to wet and repeat.

Evaporation would not be needed three times if we did not use too much nitric when we first dissolved the gold, we may get by with one evaporation, or using a little excess precipitant to overcome the small amount of excess nitric acid in solution, 

If only we just listened to the great advice of GSP, His advice of only using the amount of nitric needed to dissolve gold in the beginning.

Harold's trick of using the gold to remove excess nitric in aqua regia evaporation, here the nitric does not dissolve the gold, but if we have free HCL and free nitric in solution it will gobble up our gold button, if we did not have free HCl the nitric in solution would not touch the gold button much, or if we did not have any free HNO3 but had plenty of free HCL in the gold salts on evaporation you would not attack the gold button, mainly remember one of these acids alone do not dissolve gold but the combination of both of them will, also remember that excess HCl in the gold chloride salt does no harm, and can actually be a benifit (like when in the precipitation stage).

It is my opinion that other metal salts in solution can give troubles when precipitating gold, tin being one of the worst (forming gold colloids that stay in solution and will not come out.) even copper in higher quantity will lock up gold in the solution with copper, and the copper not releasing the gold from its bond, the purer the solution of gold chloride (without free nitric acid to redissolve the gold), the better and easier will be the precipitation and purer the gold powders.

get rid of trash early in the game, (trash in is trash out), or troubles getting back your gold.

Not sure if this helps or confuses you more?

I know your using your stannous test to tell if you have all of gold out of solution.

If you end up with SMB (from excessive use) you should be able to rinse these out of powders later, may just take you more rinses.

From your statement it is looking clear (assuming your talking of color, and not turbidity) then sounds like gold is precipitating, did you have to boil? 
Or was just waiting letting it sit to precipitate that brown powders?

color of the powders after washes, are also an indicator if they will need refined again for high purity. 

Glad to see you feeling good enough to brave the cold weather, I guess this hobby is motivating you to get out of that sick bed.


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## Oneal58

Hi Butcher, I just got back in from running the making gold pure process that Harold advises to do. I ran another HCL boil, dilute/decant, rinse/ repeat. I then added the ammonia hydroxide boil/dilute, rinse, reapeat and a final HCL boil, dilute, rinse/repeat. Checking decants with stannous. I dried gold powder that turned out to be granular in structure. I dried the gold, and came out with a very good looking button. I didn't drop this one and ended up with a nice looking clean button. One more run of this size will give me a troy ounce which I have already found a market for. 
I am at the beginning stages of understanding what you are saying about the chemicals and the parts each play in this process of refining. Trouble is, the more I understand the more I realize how little I know about them. I followed each and every thing you explained in your previous post. I see now instead of concentrating so hard on turning out good quality refined gold I need to make myself knowledgable about the chemicals I will be using as well. At first I didn't see why I needed to know about the chemicals, not in depth anyway. My thought pattern was on turning out the gold, my thinking was to just give me the amount to use and directions to put it to work and don't worry about what's happening during the process. But I am beginning to understand now that I truely need to study the characteristics of these chemicals to fully understand what is happening when I do the refine. Any quality refiner needs to know this part of the process, that I hope that I will be one day. 
Butcher, thank you so much for your mentoring me. I just don't know where I would be if you hadn't found me. Proably still struggling on the first refine. Thank you so much for your patience and ability to teach common folk that aspire to do greater more technical things. It really is appreciated, You are appreciated, I just can't say this enough. 
Good night Butcher, it's bedtime here in on the East Coast. I am running on empty now. Talk to you tomorrow Butcher, hope you have a restful night.
Oneal


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## butcher

Oneal. 
I am just a parrot, spitting out words I heard from others on this forum the thanks really goes to them.
I know your well on your way to becoming a good refiner.
good night.


----------



## Oneal58

Hi Butcher,
Should I evaporate my sulphuric acid down to make my (poor mans nitric)? I have read on some of the post that if you evaporate off about 60% of the sulphuric (drain opener)to fumming sulphuric you will get stronger nitric when making nitric. Is this correct? I didn't want to do this until I checked with you.
Also, I have used copper busbars I have accumulated through the years. Heavy gauge busbars for 3/0 and 4/0 wire. Will these do for the copper? Does the amount of surface area of the copper exposed to the Potassium Nitrate make a big difference? When copper hit near $3 a pound a while back I sold a good many of what I had but still have some left.
I have .925 sterling silver I want to refine, so I will need to condense some of the nitric I make. Would like to make it as strong as I could to start. I know that you have said the best I can do is about 68% without using a condensing unit. But I do have the set up to do this with, just that I am not ready to start on the sterling silver right now. Plus the 68% nitric will do just fine right now until I get through all the gold filled I have. I am going to triple the amount of the refine this time. I need to start processing larger lots so I need to get the nitric made. 
Thanks Butcher for your continued support. 
Oneal


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## jimmydolittle

Rooto stump remover is about 98% sulfuric from what I’ve been able to ascertain. I’ve never refined any silver, so I really don’t know what it would take to do that job. Most lawn and garden shops will have this product. Seems a waste to have to evaporate battery acid down to accommodate your needs.


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## goldenchild

The Rooto you can get at the store is 93.2% pure to be exact https://www2.itap.purdue.edu/msds/docs/12070.pdf. At 98% it would be the dark brown to black stuff. Even more dangerous than the lower percentile stuff. 

You will be hard pressed to make poor mans nitric that can dissolve silver. Usually too many nitrates are left in solution to effectively digest the silver. You would have to distill your nitric to get a better quality acid capable of digesting silver. Distillation comes with a whole other set of safety issues and concerns though.


----------



## Oneal58

Thanks fellows for the information on the sulphuric. I will go take a look at the Hardware Stores tomorrow, (rooto). 
I watched a video on how to purify potassium nitrate fertilizer, it envolved dissolving the potassium nitrate fertilizer in hot water and then letting it settle out the impurites that sunk to the bottom of the container? Then decant only the clear liquid off the top. The video didn't get into how to get the liquid back into a solid. I guess that would be just to put it outside and let the water evaporate off, leaving the solids behind. Or putting it in the freezer and letting it freeze, pour off the liquid and collect the crystals. I have seen 1 method that did this. 
Also I couldn't find Potassium Nitrate or Sodium Nitrate fertilizer when I first started with this endevor 2 months ago. The ammonia nitrate fertilizer I have until I know for sure how to handle it safely. Is there a method to take the ammonia out of ammonia nitrate fertilizer. Leaving only the nitrate salts behind? I have some ammonia nitrate fertilizer that I would like to make use of but am somewhat afraid to mess with it having the knowledge or lack of it right now?
Thanks in advance. 
Oneal


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## butcher

Poor man cold nitric acid, the very famous post by Laser Steve see below.

There are many way's to make nitric acid but this is the best method in my opinion for making nitric acid.

Steve done an excellent job figuring the proportions and solubility,
I tried to make it 68% before, using a little less water than his recipe, but found it was harder to get rid of salts, (the 50% nitric from this recipe works great as is, or can be concentrated up to 68% if wanted through evaporation (not boiling, just heating till fumes vapor off), and (can be distilled and purified for use on silver easily).(the sulfate salts do not react with gold so with gold distilling is not needed).
Many things we need about 35 to 40 % nitric acid like silver, or to remove base metals, and 68% or less for aqua regia.
(I do not want to confuse anybody, but if you note in the recipe Steve gives in link below he adds water and concentrate sulfuric acid (you can use a less concentrated sulfuric acid in the recipe, just figure in the water contents involved).

(http://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=315&hilit=concentrate+nitric+acid&start=20#p2572

If you are using nitric acid for silver it will need to be distilled, (boiling of gas fumes and condensing them), this will leave the sulfate salts formed (sodium or potassium sulfate salts), behind in the boiling vessel and will give you a purer nitric acid product (as long as you did not produce carry over too hard of boiling or bumping, of solution in your distilling rig.

The problem with using home made nitric without distilling on silver, is that silver will form sulfates easily, silver sulfate is only very slightly soluble, something like 55g in 100ml H20, so you would loose much silver to become silver sulfate powders, these are also more trouble to convert back into elemental silver before melting, so basically if working with silver and home made nitric distill your nitric first.


Distilling is really not hard at all, all you are doing is boiling a solution, capturing the gases and condensing them back into a more pure liquid, leaving the impurity in the boiling flask. As you can see in the post above I made a distilling rig out of common household things, you can get a lab-glass distilling rig for about 60 dollars on up, as hard and expensive as nitric is and if you do much with nitric it will pay for itself.

You can make concentrated fuming nitric, but it is dangerous and not needed for what we do. And I will not say how to make it here because it can have illicit uses.

nitric acid has an azeotrope of about 68%, this is the strongest you can make it using the cold nitric method, or if is made much weaker, this is the strongest you can get it by evaporating off water, but this is the strength you normally buy it at, and it is the strongest we would need to recover and refine with.

Acids strength can be tested by seeing how it reacts on metals or by measuring specific gravity of the acid.

you can make nitric acid out of ammonium nitrate fertilizer, but if not done right in can be very dangerous, so I normally will tell people on the forum do not do it is too dangerous, as I would feel terrible if I told somebody how, and a distilling rig blew up in their face.

Sodium nitrate works great and can be found easily as a fertilizer, you can even order sacks of this from garden suppliers on the intranet, potassium nitrate found as sump remover is easy for me to find (Lots of stumps around here), and it works great also.

Save the sulfate salts byproducts from making nitric acid, I use them to make several other chemicals, (or for fusion) in my refining lab.


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## Oneal58

Hi Butcher, 
Butcher, for the life of me I can not find the step by step instructions of making the nitric with Lazersteve's method. I clicked on the link you sent me and the site takes me to the pages where everyone is discussing the method but I can't find the step by step instructions by Lazersteve? 
I also have done many searches on Lazersteve's cold nitric method and each time I can find where everyone is discussing the method but I can never find the post by Lazersteve on the exact instructions? I guess this flu bug has effected my mind. But for the life of me I cannot find the link that is posted with the instructions on how to make the nitric with the method that you said to use? I don't understand this, I have looked many times and just can't find it.
Do I have to go to Lazersteve's site to find it? I have done that too with no luck.
I guess you will have to hit me between the eyes with it before I will see it today?
Thanks Butcher,
Oneal


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## Oneal58

Hi Butcher, after looking again I think I finally found a version of the method Steve said he was going to post. Steve posted on April the 23rd, 2007 the method below and then on the 25th of april he stated he had come up with a new method he would post later that was even better. I found the method he posted on the 23rd but I can't find the updated version he posted later that he announced 2 days later he was going to post? If you will for me, please just verify this is the latest/last post on the updated method that Steve uses for his cold nitric method. He said he was going to post an updated version but I just can't find it? So, I just don't know which one I have here. 
Sorry to be such a bother Butcher. I just want to make sure I am on the right, updated version of the method. I need to spend more time surfing the site to get more familar with it for sure.
Thanks,
Oneal

Reaction:

-Bring 100 mL of Distilled Water in a 500 mL pyrex beaker to 100 C
-Add the Nitre of your choice (202 gm K / 170 gm Na)
-Stir until Nitre is completely dissolved, let cool below boiling
-SLOWLY add 56 mL conc (96%+) Sulfuric Acid to Hot Nitre solution while stirring, DON'T allow the solution to boil! 
-Allow solution to cool to room temp (DO NOT SKIP - VESSEL WILL SHATTER IF PUT ON ICE WHILE HOT!!!)
-When vessel reaches room temp (25 °C) put the vessel in the freezer or on a salt water ice bath
-Let stand until temperature of mixture reaches -5 °C
-Let stand at -5 °C until all precipitate settles
-Pour the COLD solution off into glass container with tightly sealed lid DO NOT POUR OFF ANY OF THE SALT IN THE BOTTOM!!!
-Makes ~160 mL ~50% HNO3


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## butcher

Oneal that is the recipe to use, just follow the instructions, you are probably just looking too hard.
Pay close attention to how he says add chemicals, and cooling parts.

The only other recipee for nitric acid I can think of, was one Steve used, was where He used sodium bisulfate to act as H2SO4 in the reaction to make nitric acid with the nitrate salts.

Laser Steve's nitric acid recipe
-Bring 100 mL of Distilled Water in a 500 mL pyrex beaker to 100 C
-Add the Nitre of your choice (202 gm KNO3 Or 170 gm NaNO3)
-Stir until Nitre is completely dissolved, let cool below boiling
-SLOWLY add 56 mL conc (96%+) Sulfuric Acid to Hot Nitre solution while stirring, DON'T allow the solution to boil! 
-Allow solution to cool to room temp (DO NOT SKIP - VESSEL WILL SHATTER IF PUT ON ICE WHILE HOT!!!)-
When vessel reaches room temp (25 °C) put the vessel in the freezer or on a salt water ice bath
-Let stand until temperature of mixture reaches -5 °C
-Let stand at -5 °C until all precipitate settles
-Pour the COLD solution off into glass container with tightly sealed lid DO NOT POUR OFF ANY OF THE SALT IN THE BOTTOM!!!
-Makes ~160 mL ~50% HNO3
(protect from light, light destroys nitric in storage)

you can make lager batches at once:
approximate six times as much for above formula above I use in a coffee pot on hot plate :
6 x 100ml boiling water = (600ml H2O)
6 x 202g KNO3 = (1212 grams KNO3)
or
6 x 170g NaNO3 = (1020 grams NaNO3)
6 x 56 ml (98%) H2SO4 = (336 ml 98% H2SO4)
to produce approx 
6 x 160ml = 960 ml of about 50% HNO3


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## maynman1751

Could you then take this solution and evaporate it to get 68% Nitric?


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## Oneal58

Thank you Butcher, I have always been able to count on you, day in and day out. That means a lot to me and I will never forget it. I am truely thankful you are here!. As well as all the other members of this site!
*Question 1*-Butcher I noticed you have to use a little more Potassium Nitrate than you do Sodium Nitrate in the recipe? Why is that? 
*Question 2*-Also, can I use one of the methods to clean up my Potassium Nitrate and will it make a difference in the final product if I do? Or will I just be spinning my wheels going to extra work for no returns. As you have said, In what we do I need nothing more than 50% nitric and If I get that from Steve's Recipe why go to any other steps, do you see it this way? 
Butcher, I will probably finish up my gold filled Jewelry I have collected over the years in this next week or so. My final end goal has always been to get to the catalytic converters. There is just too much competition on the gold that is available and I don't want to have to run the roads to find it. 
I have friends in the junk car business that sell to catalytic converter buyers that come by their junk yards almost on a daily basis. They then sell to a buyer that then sells to a refiner. I live in a very rural area, middle of no where really. There are salvage title car/truck rebuilders on every country road here. Mostly farmers who could no longer make it farming for a living. I can think of 4 within 5-10 miles of me and 8 within 20 miles. Large junk yards with hundreds of cars, trucks, Etc;. I know that the catalytic converters are long gone on those hundreds of vehicles sitting in the junk yard though. But these guys (owners) work slavage sales almost on a daily basis and bring in new inventory almost everyday. 
I have talked to a couple of these yard owners and if I can cut out the middle men here I can offer them a little more for each converter. It's all about the money as you know and I could essentially cut out the buyers that do not do their own refinning. I hate to do that but my portion would be small and I would not put anyone out of a job or much of their income. I know they have to feed their family too. 
Now, from what I have learned so far this (recovering PM's from catalytic converters) 
is one of the best kept secrets in America. A lot of what I have read would take someone with a PHD to understand. I think it's written that way to discourage the regular guy from trying it. I pick up bits and pieces of how to go about refining converters but no where have I found the A-Z process. 
*Question 3*-Is there a good book you could recommend or does Lazersteve's Video on converters get into the detail that I am needing to know before I get started? 
I have been too busy trying to refine gold filled Jewelry to do much studying on the converters. This will change in a week or so. Do you have any advice on where and how I should start? 
Thank Goodness for this site, it would have been impossible for me to have taken on any of this without your help and the other members of this site so freely giving information to the common guy to accomplish these task. 
As Always, Thanks Butcher,
Oneal


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## butcher

Dilute nitric acid can be concentrated up to 68%, by evaporating off water, if not boiled fumes are high in water content, 
(After 68% azeotrope is reached both fumes and acid in evaporating dish would be 68% until all of the nitric evaporated).

you need more potassium nitrate than sodium nitrate in the reaction, (because of Moles), nope not the little critters in holes in your garden, but the molecular weight of atoms of these metals (sodium and potassium metal) in the chemical reaction, I will not go into more detail now, but these formulas are calculated by molecular weight of substances.

You can re-crystallize a salt to make the crystals more pure, (very pure), dissolving an impure crystal in a solution it is soluble in, (this case water), then heat to drive off water as fumes, until crystals form (when salts crystallize they try to reject most impurity), removing the crystals and repeating the process you can get very pure crystals.

As far as the nitrate fertilizer I usually would not worry about re-crystallizing them, if much dirt in fertilizer you can filter the hot dissolved sodium nitrate, before adding the sulfuric (my fertilizer where usually so clean I did not worry about it),
If you had traces of chloride in the fertilizer and you were concerned you could add a few drops of silver nitrate to your nitric to remove the chloride (as insoluble silver chloride in the bottom of the nitric acid) (I did not mess with this for home-made nitric, I can just use store bought if I was concerned about purity). Most of what I use poor-mans nitric for a trace of impurity gives me no problems.
Distilling is a good way to get purer nitric (leaving unwanted salts behind) and if any chloride did distill over using AgNo3 to remove them.
Just like re-crystallizing a salt, redistilling a solution also can be used to purify the solution.

I would just make the nitric from the fertilizer as is, unless your using it for very high grade chemistry the little impurity you will not notice (except for sulfate salt and silver as mentioned in above posts).
Again let’s just keep it simple as possible.

Hoke's, the forum, and information from LOU, Harold, and Laser Steve,and other's, you should be able to recover and and refine most anything even cats
(not house cats, no hope for learning about recovering them on the forum, ask palladium about recovering them).


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## Oneal58

Thanks Butcher, 
*Butcher, what is the wattage rating on your burners on your stove*? I ask because I find that a 900 Watt Burner is not big enough to bring a 800ml or greater solution up to steaming without giving it a lot of time. I have been looking for a double top solid burner for a couple of weeks or so. But every one that I am finding has only a 900 Watt Burner (large burner) on one side and a 600 or 750 watt burner (small burner) on the other. I have already exploded 2 clear pyrex casseroles on my stove, that's with a piece of thin stainless steel drilled full of holes used for an underplate on the element. I no longer use clear pyrex casseroles and use the white porcelain ones now after reading this happened to someone else on the site. I always use a catch basin under my container bearing my solution also, which steals heat away from the container with solution. Takes it a long time to heat up to steaming. I would like to find at least a 1200 Watt burner Stove on one side with a 600 Watt on the other side. This would still keep me within NEC Ratings for a continuous duty circuit, single phase 120V/20 amp breaker on #12 Guage wire. This would still leave me an amp to play with. 
So, I guess what I am asking is what size (wattage rating) is your largest element on your stove and is it solid. Also, do you use a catch basin container of some kind beneath your solutions, even with the solid element? If you have a larger element (1200 watt double burner (largest element) where did you find it and do you like it?
*One more question,* if you have a spill of gold bearing AR and mop it up with a paper towel. If you dry and then burn this towel does the gold revert back into a solid or are the particles so minute that they just float away in the smoke? Would it be best to wash the paper towels in Hydrochloric a few times, using fresh Hydrochloric for each wash until they are white again? Is there a better way to recover the gold bearing liquid they hold?
I ask this because I have some nice yellow paper towels that doesn't match the decor in the room where I am working.  I want to get the yellow back out of them/white goes better with everything in the room. :lol: I have the towels in a sealed container to keep them from drying out until I find out what to do or how to recover this gold. 
*One last Question*, when cooling the solution for the cold nitric method, how critical is it to keep the solution at -5 degree Celcius. If in the freezer will it not tend to go lower than -5 degree C. Do I keep taking it in and out of freezer to maintain this temperature? 
Thanks Butcher,
Oneal


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## butcher

The hotplates I use look just like these at sears, but I get mine at bi-Mart for a little over 20.00 new, much cheaper if I find it at second hand store.
http://www.sears.com/shc/s/p_10153_12605_SPM6296037902P?prdNo=7&blockNo=7&blockType=G7


I am not sure about wattage off the top of my head I can check later, but I measured the burner temperature before and I think it was something like 600 deg. F for large burner and 400 deg. F for small burner on high. (My guess around 1000 watt total)
The hotplates I use look like this, although I get mine at bi-Mart for a little over 20.00 new, much cheaper if I find it at second hand store.
I am not sure about wattage off the top of my head I can check later, but I measured the burner temperature before and I think it was something like 600 deg. F for large burner and 400 deg. F for small burner on high.

I will use Mr. coffee type coffee pots directly on the burner, but also I am very careful about thermally shocking the glass, I almost never have trouble with one cracking, unless I screw up, and change temperature to fast or try to heat with much salts or solids in bottom.

The white corning ware casserole dish will take much more abuse, and I can heat salts or layers of metals in the bottom of them or even incinerate in it.

If you are breaking vessels on hotplate then use a shallow pan with layer of sand (sand bath) between the burner and reaction vessel.

I also use a propane burner similar to camp stove, if I need higher heat, but for most things I like the electric burners.

do not change temperature of glass fast it thermally shocks it, also distributing the heat evenly helps so as not to create hot spots, also use thin glass made for heating (most thick glass is not made to heat).

your spill of gold chloride solution mopped up in paper towels is still gold chloride, burning the filters in my mind would be a mistake without first washing them in a dilute solution of sodium hydroxide, this will make the chlorides into table salt that is water soluble, and can be rinsed out, so that when you burn the filters the gold will not dissolve into the smoke. I am not sure if the smoke from chloride and gold is just chlorides or if it also forms chlorine gas, but it will dissolve gold and carry it away in fumes at these temperatures, neutralizing and washing away the chloride from the salt before incineration is what I do.
If you melt gold with table salt the fumes will carry off some gold, how much more would be carried of in the acidic chloride fume I do not know but would guess to say a considerable amount.
Just ask Harold' how much value he recovered from his fume hood.

The white corning ware casserole dish will take much more abuse, and I can heat salts or layers of metals in the bottom of them or even incinerate in it.

If you are breaking vessels on hotplate then use a shallow pan with layer of sand (sand bath) between the burner and reaction vessel.

I also use a propane burner similar to camp stove, if I need higher heat, but for most things I like the electric burners.

do not change temperature of glass fast it thermally shocks it, also distributing the heat evenly helps so as not to create hot spots, also use thin glass made for heating (most thick glass is not made to heat).

your spill of gold chloride solution mopped up in paper towels is still gold chloride, burning the filters in my mind would be a mistake without first washing them in a dilute solution of sodium hydroxide, this will make the chlorides into table salt that is water soluble, and can be rinsed out, so that when you burn the filters the gold will not dissolve into the smoke. I am not sure if the smoke from chloride and gold is just chlorides or if it also forms chlorine gas, but it will dissolve gold and carry it away in fumes at these temperatures, neutralizing and washing away the chloride from the salt before incineration is what I do.
If you melt gold with table salt the fumes will carry off some gold, how much more would be carried of in the acidic chloride fume I do not know but would guess to say a considerable amount.
Just ask Harold' how much value he recovered from his fume hood.


----------



## Oneal58

Hi Butcher, thanks for all your help. I will give you a rest tonight. I will follow your directions on everything you have answered for me today. I do really appreciate you.
BUY THE WAY, HAPPY NEW YEAR!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!!
SEE YOU IN 2012, Wow, time is just a flying. Hopefully this time next year I will be answering some simple questions instead of asking, asking, asking all the time. 
BUY THE WAY, HAPPY NEW YEAR TO EVERYONE HERE, ALL OF YOU ARE APPRECIATED. KEEP SAFE TONIGHT. 
A Southern saying, 
KEEP THE WHEELS BETWEEN THE DITCHES AND THE BOOGERS OUT OF YOUR BRITCHES!!!!!!!!!!!
Oneal


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## Oneal58

Hi Butcher/Everyone, I hope you'all had a wonderful holiday. 
I have ran into some problems with the formula below and hope you can get me back on track, or try and find the problem. 
I followed the recipe exactly you gave me, the one that is 10X's the amounts given in Steve's Recipe. 
1-Measured out exactly the amounts needed X 10, brought the distilled water up to 100 degree's C. 
2-Added the Potassium Nitrate, X10, and stirring until the KNOS had dissolved completely. 
3-Lowered temperature below boiling on solution and added ROOTO Drain Cleaner, 94% sulphuric, X's 10 
5-Stirred well and then took off heat. 
6-Let cool outside untill temperature was 72 degrees F.
7-Put solution in freezer, lowered to -5 degrees C. 
Butcher, I made 4 batches of this without stopping. I worked all night on it. Sun was coming up when I went to bed. 
I only ended up with no more than 250ml of solution on every single batch? I tested the Nitric and it is good strong Nitric. But I am only getting 250ml of Nitric out of each batch, the rest turns to rock hard salts?
I end up with rock hard salt in the bottom of each vessel, How in the world do I get this salt out of the 4 vessels I have it locked up it. It (salt) is rock hard? I have 4-12 cup coffee pots full of rock hard salt? 
Almost all, well all but 250ml turns into salt in the vessel. 
I am using soluable KN03 (Potassium Nitrate). The fertilizer is clean as far as I can tell? 
Butcher, I don't know what could be happening, I know I should be getting around 960ml out of each batch but I end up with mostly rock hard salts and 250ml of Nitric.
Do you have any idea of what is going wrong? I have checked and double checked the directions/amounts used and I have followed them exactly. 
Do you possibly know what is going on? 
How in the world do I get these rock hard salts out of my vessels?
Has anyone else experienced this with their method of making the Nitric?
Thanks Butcher, 
Oneal





butcher said:


> Oneal that is the recipe to use, just follow the instructions, you are probably just looking too hard.
> Pay close attention to how he says add chemicals, and cooling parts.
> 
> The only other recipee for nitric acid I can think of, was one Steve used, was where He used sodium bisulfate to act as H2SO4 in the reaction to make nitric acid with the nitrate salts.
> 
> Laser Steve's nitric acid recipe
> -Bring 100 mL of Distilled Water in a 500 mL pyrex beaker to 100 C
> -Add the Nitre of your choice (202 gm KNO3 Or 170 gm NaNO3)
> -Stir until Nitre is completely dissolved, let cool below boiling
> -SLOWLY add 56 mL conc (96%+) Sulfuric Acid to Hot Nitre solution while stirring, DON'T allow the solution to boil!
> -Allow solution to cool to room temp (DO NOT SKIP - VESSEL WILL SHATTER IF PUT ON ICE WHILE HOT!!!)-
> When vessel reaches room temp (25 °C) put the vessel in the freezer or on a salt water ice bath
> -Let stand until temperature of mixture reaches -5 °C
> -Let stand at -5 °C until all precipitate settles
> -Pour the COLD solution off into glass container with tightly sealed lid DO NOT POUR OFF ANY OF THE SALT IN THE BOTTOM!!!
> -Makes ~160 mL ~50% HNO3
> (protect from light, light destroys nitric in storage)
> 
> you can make lager batches at once:
> approximate six times as much for above formula above I use in a coffee pot on hot plate :
> 6 x 100ml boiling water = (600ml H2O)
> 6 x 202g KNO3 = (1212 grams KNO3)
> or
> 6 x 170g NaNO3 = (1020 grams NaNO3)
> 6 x 56 ml (98%) H2SO4 = (336 ml 98% H2SO4)
> to produce approx
> 6 x 160ml = 960 ml of about 50% HNO3


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## butcher

Oneal,
A couple of things to consider, were all of the potassium nitrate salts dissolved in boiling hot water before adding concentrated sulfuric acid, (if some was crystals you may not have gotten a complete conversion and still have nitrates locked up in the sulfate crystals).

Potassium salts seem less soluble than sodium salts to me (if your crystals formed too quickly you may have not gotten complete conversion or crystals may have just locked up some nitric in crystals), did you slowly cool and separate salts from liquid before freezing?

Either way, I would separate the liquid (nitric you have now), from cold crystals, put the wet crystals back the reaction vessel add just a little water not much (I would also give it a little 3% hydrogen peroxide but not necessary) then add a little sulfuric acid,(remember the rule about the danger, Do not add water to concentrated sulfuric acid). (we are not trying to dissolve these salts till hot, (this first addition of liquid is just to keep salts wet till we get them warmed up, so we do not burn them, (we can add more liquid later if needed).

Heat, till salts dissolve again, (my goal would be to get any water then acid we added just to about 68%), (about 2ml H2O for every 1ml H2SO4 added), and only adding as much of this to dissolve the crystals at just under boiling temperature, so starting with just a small amount of liquid at first, start raising heat (slowly raise heat, till glassware temperature comes up, remembering not to thermally shock your vessel), as heat is raised you may see you need more dilute acid to get all crystals dissolve just below boiling with good stirring.

Once all of the salts dissolve, slowly start lowering heat on vessel. I would not just turn off heat, but lower it about half way down, after solution cools some you may see some crystals already begin to form, (the slower we form the crystals the purer they will be), then turn off heat, but we want to cool this as slow as possible so the crystals of potassium sulfate will grow slowly as possible, once cool to about room temp and well settled, decant liquid from crystals, the crystals I save for the potassium sulfate salts, the liquid now put in freezer and freeze out more salts, I would keep the first batch of nitric you made separate from this second batch, and test each batch, (in small vessel like test tube’s or cups maybe on a gold plated pin or small piece of copper see how each react on copper, if reaction is similar then I would not worry about putting both batches in one bottle.

(I will add this, but I do not want to confuse you more), (if you don’t understand forget this paragraph and just use instruction above)
Now you have several batches of this, I may add just a little water then acid to each batch of salts (just enough to wet so I could make a thick slurry of each. then when I heated the first batch and had it dissolved into liquid, (using instructions above) and all dissolved just under a boil, add more of the remaining slurry of salts a little at time, stir well to dissolve to this hot mix with stirring once I had starting to get about 1/2" layer of salt in bottom (still hot and good reaction time, that would not dissolve) I would decant this liquid into next batch of salts (slurry of next coffee pot), (but taking care not to thermally shock glass pot, so you will need to lower heat somewhat of the hot solution pouring into cooler pot), basically what we are trying to do is re-dissolve all of the salts and re-crystallize them (for higher purity salts) and get any nitrates into a solution of a fairly good concentration of nitric acid, with as little as more added liquid as possible, You could even use some of the nitric you made earlier to do this with (instead of adding as much new water and sulfuric acid). 

I have a hard time explaining what I mean, it is easier for me to just see something and do it, than it is to explain to someone how I think, and explain to them how I may do it. (Trust me my mind is a jumbled mess of thoughts).

You may also find another explanation about how others have re-crystallized their salts


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## qst42know

I would guess some of your nitric is being held by capillary action in the salt crystals.

Something you could try on your next batch is to let your solution set at room temperature to allow some of the salt to form. Filter that out and then chill the solution. A more open crystal of the remaining salt may allow your nitric to drain out better.

You might try to gather some of the trapped nitric with ice cold water. Fill a vessel with ice and add some water. When it's good and cold pour some in the first coffee pot swirl it around a bit and drain into the next pot and then the next. Keep transferring the same water from pot to pot you should collect some dilute nitric with some dissolved salt. 

The remaining salts in your coffee pots will be water soluble.


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## Oneal58

Thanks Fellows, I appreciate your help. With what yall have told me, I might have a clue what I did wrong but not sure?
Here is what I did!
1-Measured out everything I would need first for all 4 batches I was going to run,my plan was to run each lot behind the other as quickly as possible. I then brought distilled water to boil on first batch. 
2-I then added KN03, all at one time, water temp droped immediately, I brought water temp back up, I noticed the KN03 salts wouldn't go into solution until the temperature reached about 90 degrees C. 
3-Once salts dissapeared I continued on up to boiling, 100 degrees C., stirring constantly. 
3-I lowered temp of solution to around 85 degrees C.. I then added the H2S04 while stirring constantly. 
4-It was cold outside and wind was blowing so I put containers outside so the cold wind could help to get the temp to lower quicker. I watched the temp on the vessels untill they reached 25 degrees C. I was about 15 minutes between all 4 of the batches I ran. I mean (after) all 4 had cooled to 25 degrees C., that took a while, a long while. It amazes me how these salts hold heat so well?
5-I then took the vessels straight to the freezer, as soon as each solution hit 25 Degrees C., I did notice that salts were already growing in containers before I got solution to freezer. 
6-As each solution hit -5 degrees Celcius I would go straight out and filter solution into HN03 Jug, within minutes. I knew the next one would be right behind the previous one. I did this one behind the other until I was through with all 4 batches. 
As I said, I ended up with less than 1100ml out of all the 4 batches. These 4 batches sure worked my tail off!

Here are some possibilities of what I did WRONG! Let me know? 
1-after salts dissolved in solution I carried the solution up to 100 degree C. and then added the *KN03 quickly*. 
2-I *did not* let solutions cool *(at)* room temp, I cooled down *(to) *room temp (25 Degree C.) *artificially*, outside with a cold wind blowing. I sit each batch up on a shelf outside so the wind could help cool it down quickly. 
3-I *did not* seperate liquid from salts before going into freezer, even though I already had salts forming/growing.
4-I *did not* allow any time between freezer and filtering into HN03 jug.

I did at least cover the salts with water hoping this was the right thing to do until I could find out what to do on the forum. There was not much room for much water, salts almost filled the coffee pots, (12 cup pots). I still have them sitting outside with water over the salts. 
From what you are telling me it's still not too late to try and recover some of the Nitric locked up in the salts? Can I follow your directions now to try and salvage some of the Nitric that I can still see in the salts?
Question-Can you point to any 1 or maybe 2 or more things that I did that I shouldn't have done?
Thanks, 
Oneal


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## butcher

Sounds pretty much like you covered anything I can think of.

Maybe I should have not told you about making big batch until you made a few small batch's first, to get the feel of things, it is usually better to learn to build a dog house before building the big house.


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## Oneal58

Hi Butcher, my personality traits I have gets me into trouble all the time. I will slow down to one lot at a time from now on. Doing just one lot correctly would have gave me the same return as working until the sun was coming up this morning. 
I will take everything you posted to heart and spend the time dissolving, letting solution cool at room temp, decanting solution before freezer trip, Etc;.
As always, thank you so much for keeping me straight. I know, it's a hard job to teach someone with such a hard head! I ask my grandson all the time where he got his hard headedness from? I guess I have been in denial all my life?
Thanks again Butcher,
Oneal


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## butcher

Oneal, actually you’re a quick learner, and I enjoy trying to help the best I can.

We have a mule named Rosy, and as stubborn as she is she fits right in with me and my family, nope we are not stubborn in our family, we are just mule headed.

When Rosy was younger I was training here to pull a cart and to log, was training her to the reins, I would yell get up, after a few tries she did, darned ole mule took off running drug me around the field about twice before stubborn ole me come to my senses and let loose of the reins, I thought I could hold on and not let her get away, it does not work that a way, a mule can drag you around like a sack of potatoes bouncing behind her, the sack of potatoes (me), just scared her more, while she is trying to get away from that sack of potatoes chasing her. I could not walk for about a month after that, so she was smarter than me and my stubbornness, she got out of work for about a month, till I could walk again.

After that every time I would log with her and yell get up, she would first start off at a run, (I never could break her of that habit), (not so much trouble when your in a cart, but when logging, I would have to try and keep out of the way of that darn log, after she got the log going good she would slow down and just pull it, and we got the logs to where we needed them, she pulled the cart well,
(Well) she only tore it to pieces a couple of times when she got spooked.

Rosy is 28 years old now and my daughter keeps her, she don't have to work any more, she’s retired. Spends her time wondering when her next treat and meal will be ready


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## Oneal58

My goodness,
I never thought I would talk to someone who has followed a mule as I have. My father was a share cropper and us children, 5 of us, would have to hit the fields everyday after school and work in the fields until dark. We hand picked our cotton in the fall and after we finished picking our cotton I would pick for others in the community for 1 cent a pound. To make a $1 bill was an all day job for a boy my age. My hands would be so sore and cut up I could hardly move them. During the summer we (traded out) with the tobacco harvest (the money crop). That means that we would go help other neighbors gather their tobacco on harvest day and they would come help us on our harvest day. We traded out with 3 different families (lot of work in 8 acres of flue cured tobacco) each family. Daddy always traded with people who had the same amount or as near the same amount of tobacco as we had. That put us working every single day and on Sat. during the summer gathering tobacco for 9-10 long weeks (sometimes longer) back then. So, in total that put us gathering approximately 32-35 acres of tobacco a week. Hardest work I have ever done in my life. Getting up at 2:00 a.m. with Daddy on our gathering day to first haul pre-filled barrels of water to the barn and pour onto the dirt floor in the barn. The floor of the barn would be hot after shutting down the burners, curing the tobacco took all week long. You shut down the burners the morning of the day you gathered tobacco. This water would make steam when the cold water hit the hot floor of the barn. The reason for this was that this brought the tobacco in Order (meaning, tobacco soaked up the water vapor) so you could handle the tobacco without breaking it to pieces. Then to unload the barn and working until dark. Lots of times we had to hang the tobacco in the barn after it was croped, hand strung and stacked. Waiting on the men to come out of the field to hang the tobacco (only women at the barn/1 man to stack tobacco/unload the drags). Then later in the fall we would hand break all our corn, stack the corn in piles right on the dirt and then come back and load the corn on a wagon and take it to the Packhouse. Packhouse held all the corn to feed the animals through the winter,(mules, cows, hogs, chickens, Etc that wasn't sold. Plus it held all the dried tobacco which had to be taken off of wooden sticks and hand wraped in bundles and stacked perfectly. My father could make a good looking pallet of tobacco, every bundle exactly bundled and stacked on those pallets. 
I could go on and on, I look back now and am thanful I was raised in such a manner. It sure made a man out of me at an early age. 
Getting to the point though, I got carried away. 
We had 2 mules that we used in the tobacco field, to plow land with, and all the other jobs you needed mule power. What I looked forward to was Sundays, I would ride Betsy all day long, from swimming hole to swimming hole. Something happened to Betsy one day and she would try to turn her head and bite me on my leg. I could not stop her doing this so I got off of her and was leading her to the barn. She came up behind me and bit me in the back, her teeth, thank goodness just did graze the skin, but I didn't take my eye off her again. I kept a close eye on her the rest of the way to the barn. She just didn't act right? The next day while I was leading her to the field she tried the same thing again. I told Daddy what was going on and he said she was just tired. He told me to unhook her and let her graze on the green grass for a while and use the other mule for that day. We used the mules to pull the drags of tobacco down the middle row in the tobacco field and a tractor to pull the drags of tobacco to the barn. But to tell you the ending of the story. My father asked a man that was trading out with us to go get Betsy and take her to the barn. As Freddie (man helping us) approached Betsy she lowered her head and ran straight towards Freddie. Betsy knocked Freddie down and was pawing him to death. My father seen what was happening and took up the swingle tree from the tobacco drag, quickly ran over and hit Betsy right between the eyes with it! My father was a big strong man and I could feel this hit myself from afar off! Well this must have knocked some sense into Betsy, she staggered a little and headed straight for the barn by herself. Freddie, on the other hand, went to the hospital for a couple of weeks. Many broken ribs, spleen damage, cuts, a concusion, Etc;. Daddy sold Betsy the following week. I felt bad for Betsy at the time, I never did care much for Freddie though. :lol: I for one missed the Sunday rides on her, she was the only one that you could ride. But I have followed a mule many, many times myself Butcher. I understand completely when you talk about how a mule operates and only too well the term muleheaded.
Well time for bed, didn't mean to get carried away. 
Thanks Butcher,Talk at you later. 
Oneal


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## Oneal58

Hi Butcher,
It warmed up above freezing today for just a short while. I noticed that the clear water that was sitting on the salts in the coffee pots have turned bronze colored and the salts had turned white? I had something to do today so it was late before I started to work on your instructions. 
I poured off a little of the solution that was on top of the salts and put a piece of copper wire in the solution. I just wanted to see if there was any HN03 in this bronze colored solution. 
Nothing happened, I then warmed the solution a little and could see some reaction, a very little, not much at all but the solution did have very dilute HN03 in it.
I poured off all of this solution from one pot, then added back 15ml of hot water. I also added just a little 3% Hydrogen Peroxide. Turned heat on low.
I was surprised to see that the salts dissolved very easily, quickly, without any addition of H2S04, expecting it to take a while I took my eye off solution just for a couple of minutes, when I went back the salts were dissolved,gone, without any stirring? Just when the solution warmed up a little the salts dissolved?
Then I lowered heat and added 25ml of H2S04. 
Lowered heat to warm and and let solution cool, I did not bring solution to boil at any time. 
I then took pot off burner, covered with a 5 gallon bucket and am letting the solution cool right now. I haven't been back out to check on the solution yet. I am going as soon as I finish here. It has been maybe 20 minutes. I have the room where solution is at 25 degree C. I am going to let solution slowly lower to 25 degree C. That's why I put the bucket over it. To slow the process of cooling down as much as possible. 
I am going to wait untill solution has reached 25 degree C. or has grown 1.5-2.0 inches of salts, in bottom of pot and then I will decant solution and place in freezer. 
*Question 1*- Why if I have a lot of salts form before solution reaches 25 degree C. Do I go ahead and decant or wait? 
*Question 2*- If Nitric is left open to atmosphere will Nitric evaporate out of solution even if cold, just above freezing? 
*Question 3*- Can I tell what strength of Nitric I have by watching it closely and slowly raising the temperature on solution untill it boils? If using the following method (your temperature Post) can I tell what strength of Nitric I have when the solution boils?
*(USING YOUR TEMPERATURE POSTING BELOW)*
If solution boils at 116 degree C. I take off heat and put in storage container, after it cools of course. That would be (50% HN03, that would be fine with me).
If solution boils at 103 degree C. (contains ony 20% Nitric) is it best to bring solution to boil or just let it steam untill solution concentrates to where it doesn't boil untill solution reaches 116 degree C.? I would want to do this without having to set up a condenser. If I rememeber your post correctly I reach Azeotropic Conditions at 68% anyway?
*YOUR POST A WHILE BACK*

*(100% H2O) boils @100 degC density 1.00.
20% HNO3 density 1.115- boiling point 103 degC.
30% HNO3 density1.180 boiling point 107 degC. 
50% HNO3 density 1.310 boiling point 116 degC.
70% HNO3 density 1.413 boiling point 121.5 degC.*

I will let you know what has happened when I return. 
Thanks, Oneal


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## Oneal58

Hi Butcher, just got back in. Nothing to report, some salts forming but just a little in the bottom. Temp. still around 96 degrees F. It needs to drop another 20-25 degrees or so before I decant. That bucket and blanket I put on the container sure slows things down as far as cooling. Salts seem to be on track right now. Checked the weather report, warming up a little tonight, low around 20 degrees. I am thinking I will just let the solution sit outside tonight instead of sitting it in the freezer. Giving solution plenty of time to react. It's already 22 outside, by the time I decant the temp should be around 20 degrees F. or close. I will just get up early and decant solution before it warms up any at all. I will let you know tomorrow how things turned out. 
I feel sure I rushed things last night, didn't give things time to react as you said. I cooled the solution down as quickly as I could last night. That north wind was howling bringing this cold front in. It was blowing directly on the pots of solution taking the heat away probably as quickly as it's ever been done. I thought it was a good idea and I was doing good! I didn't even consider reaction time as you said. I should have just left everything outside all night, out of the wind under a tarp or bucket. It got down to 18 degrees F. last night and didn't get above 20 degrees untill around 9 or so this morning. The weather was almost the perfect ice box for me but I didn't realize it. I turned the freezer down as low as it would go when I put the solution in the freezer. And then just as soon as the solution hit -5 C. I jerked the pots out of there and went straight and decanted. 
Oh well, you live and learn. I honestly didn't even consider reaction time at all. I just thought the temps were important to watch and that would get the job done. I think and hope I know better now? On this particular recipe, the slower the better and I didn't realize that until you told me last night. 
Thanks Butcher, one day I will get there. 
Oneal


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## butcher

Oneal, 
Lets look at the homemade nitric acid, using potassium nitrate (KNO3), sulfuric acid H2SO4 and water H2O.

2KNO3 + H2SO4 --> 2HNO3 + K2SO4 
(Not figuring the water)
KNO3 101g/mole (2moles 202g)
H2SO4 98g/mole 
HNO3 63g/mole (2 mole 126g)
K2SO4 174g/mole
Mole’s not that little thing eating turnips in your garden, 
(Molecular weight from periodical table)


This produced nitric acid HNO3 and potassium sulfate K2SO4

Both of these are soluble in water, the nitric acid is diluted by the water., but in this reaction it also helps us to get the sulfate salts out of the nitric acid we made, temperature and solubility of these salts is also used.

Solubility of the potassium sulfate salts K2SO4, 
7.4g/100ml H2O @ 0deg C, 
And 
24g/[email protected]

If you did not have, as much water in the reaction above your byproduct with concentrated sulfuric acid can be potassium bisulfate KHSO4 that is a lot more soluble in water, 36g/[email protected], and 122g/[email protected], this is one of the reasons we make the nitric with more water.

The strength of the nitric can be judged by its reaction on copper.
Measuring the density of nitric acid is the best way to tell what percentage the nitric acid is.

With water density 1g/[email protected], boiling point 100 deg C
Nitric acid at 20 degrees centigrade
0% (water) density 1.ooog/ml, boiling point 100deg C
20% HNO3 density 1.115g/ml, boiling point 103 deg C
30% HNO3 density 1.180g/ml, boiling point 107 deg C
50% HNO3 density 1.310g/ml, boiling point 116 deg C
70% HNO3 density 1.413g/ml,, boiling point 121 deg C
90% HNO3 density 1.482g/ml, boiling point 102 deg C
98% HNO3 density 1,503g/ml, boiling point 86 deg C

(Density concentrated sulfuric acid approx 1.83g/ml)

Remember if concentrating the nitric we do not want to boil it or get it up to its boiling point for that concentration, we just want to vaporize off the water, so we heat below the boiling point for the concentration we have (evaporation of water will happen way below the boiling point of water. so with this knowledge we can heat below 100 deg centigrade and concentrate our nitric acid.

Here is a solubility table.

http://en.wikipedia.org/wiki/Solubility_table

I Hope this helps
Butcher


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## Oneal58

Thanks Butcher, believe it or not I am starting to understand some of this language you are talking now. I didn't take any Chemistry Classes in School. I am going to ask my daughter to see if she can bring me home a basic Chemistry Book from the school. I feel I need some basic knowledge of Chemistry even if Hoke feels it's not necessary. It sure can't hurt any. 
I went out early this morning, still around 20 degrees F. outside. I decanted what Nitric I had off the salt crystals that formed overnight. I put a piece of copper into the cold nitric, nothing happened. I was dissapointed because just the smell of the solution told me it was somewhat concentrated. I turned the burner on and held the container with a sample of the solution and the piece of copper just above the coils without touching the coil. In just a few seconds the nitric was fumming brown gas. So, the recovery of the locked up Nitric in the salts was successful. I came back in the house, the cold was getting to me. I am on blood thinners due to my heart condition and I can't stand the cold anymore. I am going to do the same thing with the last 3 pots of salt I have. I am pretty sure this last Nitric I got is more concentrated than the first 250ml I got out of each batch. It's just so cold outside today and with me just getting over the flu I am afraid of working too much in the cold.
That's why I asked *how long Nitric will stay in a solution if kept cold*, in the previous post? Will any of the Nitric evaporate off slowly if solution is near or just above freezing? 
I have got to try and learn how to measure density. I know that there are density meters but can't I do the same thing with my scales. I think I have read where someone has found density by weighing liquid, using the formula 
Density= Mass/Volume. 
But what if I still have some dissolved salts in with the Nitric. I guess the only way to be sure there is no dissolved salts in the solution is to keep decanting and then putting the solution back in the freezer untill no more salts grow? If you have any dissolved salts at all in the Nitric solution you wouldn't get a correct density reading, right?
Thanks Butcher,
Oneal


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## butcher

oneal.
If the acid is very concentrated, many times the reaction on metals is actually slowed down, (which if you added the recommended water it would not be).

Notice that adding water formed K2SO4, which the salts are much less soluble, and when we freeze the solution much of the salts can be removed (not all, but most of them) I would not worry about tiny amount of salt when trying to get an idea of how strong the nitric is.

With specific gravity we can use test instruments to measure (like when we check specific gravity of a battery with that little tool with the floating balls or needle), I am not sure one of these would work for nitric, but it could be used for comparison I suppose, I just never tried it. 

Specific gravity we are comparing the weight of water to the weight of our acid in a 1ml sample (accuracy of sample in ml is necessary, we can weigh larger volumes to assist in accuracy), basically if milliliter water has a specific gravity of one or (1 gram per milliliter @ 20 deg centigrade), our same size one milliliter sample of acid weighs more, our one milliliter sample of 50% HNO3 would weigh 1.3 grams @ 20 degrees centigrade.
Again comparing larger samples improve accuracy of our readings of volume and weight comparisons.

Light will break down nitric acid to NOx gases, if nitric is very concentrated it fumes bad as NOx gas, more dilute the less fuming and loss as gas, temperature is also a big factor, gases do not fume as bad in cooler temperature and stay in liquids more.
I would be more concerned with light than with concentration and temperature of what nitric you’re working on now.


Getting a chemistry book and studying I highly recommend, many of the principles they use are what we are doing when we recover or refine.


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## Oneal58

Hi Butcher, 
Ok, I have looked and there are many types of Hydrometers but I see I would need the specific gravity Hydrometer if I used one or needed one? Solid glass to measure hot liquids, acids, Etc;, with. Lets say I measure out 100ml of water and heated to 20 degree Centigrade, exactly, or heat just above 20 degree centigrade and watch Hydrometer untill liquid cools to exactly 20 degree centigrade. I then take the reading from the Hydrometer, lets say the water (weighed/specific gravity/density) of 100grams @ 20 degree centigrade. Take that reading and measure out 100ml of my Nitric and it weighed/specific gravity/density of 131grams @ 20 degree centigrade. I would then know that my Nitric was 50% Nitric in solution referring to the chart you sent me. 
Butcher, Is there a mathmatical formula that you use if I ended up with my Nitric say with a specific gravity/density of 111.5 grams per 100ml @ 20 degree centigrade to come up with concentration. I can use the chart that you sent me in a previous post and know that I would have 20% Nitric Concentration. But I was just wondering if you used a formula to get that with? I can see that the same percentages does not hold true with each different concentration?
Also, could I just weigh the solutions on my scales, would this get me close enough if I use the 100ml size samples? 
Thanks Butcher,
Oneal


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## butcher

oneal,
Normally I am really not that concerned with knowing the exact strength of my nitric, as normally I dilute it anyway, and heating the dilute nitric acid when reacting with metals will also concentrate it as it is making metal nitrates, dilution also keeps some of the NOx gases from forming as gas, mixing NOx with water to from more nitric in solution, keeping the reaction in solution to dissolve more metals, instead of just fuming off as that red brown cloud.

Most of my work in recovery where I will use homemade nitric it is not that important to me.
I buy nitric for the processes where it may a concern, and will use it on silver or where I may be concerned with purity or concentration.


Personally if I was trying to get a rough Idea of concentration, a graduated measuring cylinder, these are tall and small in diameter (not sure what they actually call these measuring vessels), so accuracy is a little better, also they are filled to read the bottom of the curve in the top of the liquid (meniscus spelling?) also accuracy of scale would play a factor, but if you measured your acid and compare its weight to the same volume of water, the acid would be heavier with both at the same temperature. (Me I would not worried about lab accuracy as long as I got a close idea of the concentration especially for poor mans nitric acid)

http://www.handymath.com/cgi-bin/nitrictble2.cgi?submit=Entry

You could also try and buy a floating glass hydrometer; it is wine country here so they may have them where supplies are sold? But I do not feel it would be worth it here, it would be nice to know exact specific gravity and concentration of the acid, and would be useful to tweak your chemistry to try and improve the batches you make, but then again to me it has not been important enough to spend the money on one.


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## Oneal58

Thanks Butcher,
I get it. Thank you so much for your help. As you said, it would be nice to know what concentrations I am turning out. But once familar with Nitric and it's characteristics one can probably tell what strength they have just by dropping a piece of copper in it. This will come in time for me, I feel as you do. Why waste the money just to satisfy a curiosity. I have already spent money on lab equipment that I don't think I will ever use and don't want to do that anymore. 
Thanks again Butcher, I hope you have a restful night. I myself am turning in early tonight. Got to take care of some business tomorrow morning early.
Butcher, you are appreciated old Buddy. You are *not* taken for granted!
I just needed to say that. I feel that you could get that feeling after sooo long, I am old school Butcher, I realize the time/work involved in answering all these questions for people like me. You are made out of pretty special stuff Butcher! As all the members on this forum who helps for nothing more than a thanks. Without even knowing if the (thanks) was sincere or not? What was it that the older members called the new guys, (NOOBS)?
Just remember, when I say thanks, I really do mean it, it is not an empty thanks, it will always be a sincere one.
Oneal


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## Oneal58

Hi Butcher, I have got a question.
I have got down to my last batch of gold filled jewelry. I threw everything in this last batch but the kitchen sink. Usually the solution I would decant after the Nitric had stopped working would have a greenish blue color to it. 
This last batch I am running has a black color to it? Very dark, I don't see any green or blue, just black. When I went to drop what silver was in solution I got no reaction, on the copper coil, none? This solution is so dark I can't even see the copper coil in the solution? Thinking that I may have depleted the Nitric completely I added some nitric back to the 1.5 gallon container full. Still no reaction. I am afraid of putting any more Nitric in solution. I thought that the solution may be too cold to get the reaction to drop the silver. I warmed the solution up to room temperature. Still I get no reaction. Now with all the gold filled jewelry I put into this lot there had to have been silver in it. I know there was silver in some of this jewelry. We are talking a hundred pieces of gold filled Jewelry?
So, I have did all I know to do to get the silver to drop and am out of options. Have you ever experienced anything similar?
If I mistakenly put some white gold or platinum Jewelry in with this batch would this have caused this? I had a large piece of platinum jewelry. I put it up but now I can't find it. My wife use to help me clean up sometimes. She says no, but that piece of platinum is gone or lost? It is possible I put some white gold in this lot. Well, not me but my wife when she was helping me. I stopped her from helping now. She has that OCD thing and everything has to be somewhere, so she drives me crazy sometimes! I incinerate everything to a red glow before desolving the jewelry. Sometimes the white will look like the yellow after you incinerate it. 
But do you have any ideas on why this has happened or what is going on? Why the silver will not drop? Did I do the right thing when I added a little Nitric to solution? 
Thanks Butcher,
Puzzled, Again
Oneal


----------



## Oz

Take a small sample of your solution and add a couple of drops of HCl. If no white curd forms (silver chloride) then there is no silver in your solution.


----------



## Oneal58

Thanks Oz, 
I will go try that now. I remember reading about that now, but I had completely forgotten about it? I had to shut everything down and go to N.C. this afternoon. It's still pretty cold here but I will warm a little solution up and try this. 
Thanks,
Oneal


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## Oneal58

Hi Oz, I got a 25ml sample of the solution. I then warmed to room temp. I then droped several drops of HCL into solution. No white cloud? I went ahead and dropped 3 more drops of HCL, no white cloud. 
I probably done this backwards but I had some solution I knew that there was silver in. I took a 25 ml sample. I then dropped 3 drops of HCL into the beaker. I saw the white cloud in the solution you were talking about. 
This tells me *NO* Silver is in solution, right? I also tested solution for PM's with Stannous. No precious metals. So I will just pour solution into big barrel and cover for now. Once I get a 30 gallon drum full of solution I will recover the copper that I know has got to be in it. Normally, is this what most refiners do? 
Do I need to neutralize the solution with Urea before I put it up in storage? 
I still can't figure out why the solution had no silver in it when all the other lots of gold filled had silver. Don't have a clue why the solution is black, any ideas?
I made some homemade Nitric, could it be that the salts left in the homemade nitric has anything to do with this?
Thanks, Oneal


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## Oneal58

Butcher, where did you go buddy, did you take a vacation? I have missed you. 
Butcher, I have been fighting the process of making my home made nitric for about 2 weeks now. I did the process over and over and would always do good to come up with 200ml of nitric on each attempt. I tried everything imaginable to improve the amount of nitric I would end up with, nothing worked? 
I weighed the nitric I was getting and it weighs 131g per 100ml. By the scale you sent me, this is about 50% Nitric. 
* I did this just to see what would happen*, I
Instead of putting 600ml distilled water in the batch, I put 900ml of distilled water in the batch. I came up with a little less than 500ml of Nitric. I weighed the Nitric and it weighs 129g per 100ml. So, that is still almost 50% Nitric and I have 500ml of Nitric for my effort. I would much rather evaporate it down a little than to do the steps involved to only get 200ml of Nitric. 
Could the problem possibly be that I am using a Potassium Nitriate Fertilizer with different concentrations than you are? I will check on the bag to see what the ratio of Potassim is to the Nitrates and let you know. 
I just can't figure why sooo much salts form. I also do everything in the recipe exactly and I still end up with salts in my Nitric when using it to dissolve with. I double check my temperatures, always bringing entire mixture down to -5 degree Centigrade. Heck, I even tried bringing the solution down to -10 degree centigrade. What happened was even more salts formed and I had almost noting left in liquid in the container, just a 12 cup coffee pot full of salts? It has to be in the fertilizer, don't you think?
Thanks Butcher,
Oneal
Thanks, Oneal


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## qst42know

Have you tried pouring off the solution after some of the salts have formed?

You might also try keeping the salts broken up as they form and vacuum filtering the nitric from it. Your nitric is there it's just trapped as water would be in sand.


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## butcher

Oneal,
Potassium salts form much easier and they are more insoluble, they also hold nitric acid easily in the crystals formed potassium salts are also better for the environment, as compared to the sodium salts.

Lets look at some of these salts, which we may get from making nitric acid,

Potassium sulfate K2SO4 (potash of sulfur), 
This salt is formed if you add water when making nitric acid from KNO3 potassium nitrate and (diluted) sulfuric acid.
K2SO4 solubility in water is about 
8g/100ml @ 0 deg C
80g/Liter @ 0 deg C
111g/Liter @ 20 deg C
240g/Liter @ 100 deg C
Can be used as fertilizer for tobacco, fruits and vegetables, (good if your watering the garden with city water that forms chloride salts from chlorinated water).

Potassium bisulfate KHSO4,
This salt is formed if you use concentrated sulfuric acid (no water), with potassium nitrate to make nitric acid.
KHSO4 solubility in water
36g/100ml @ 0 deg C
360g/ liter @ 0 deg C
480g/ liter @ 20 deg C
1220g/ liter @ 100 deg C
can be used in reactions that normally use sulfuric acid, it acts like sulfuric acid when fusing salts with heat, can be used to make ferrous sulfate (gold precipitant), or for fusing Rhodium to dissolve it in water, or other reactions you would need sulfuric acid, note it acts like K2SO4 and H2SO4 in these reactions.

Sodium sulfate Na2SO4 (Glaubers salt),
This salt is formed when making nitric acid with sodium nitrate and Dilute (added water) sulfuric acid.
Na2SO4 solubility in water
4.9g/100ml @0 deg C
49g/ Liter @ 0 deg C
195g/ liter @ 20 deg C
425g/ liter @ 100deg C
Notice this salt is more soluble in water than compared to potassium sulfate, but also the salts will not trap as much nitric acid, when making nitric acid from sodium salts, also notice by freezing we can remove much of these salts of (sodium or potassium sulfate), at 0 degrees centigrade the solubility of these is similar

Sodium sulfate salt seems to form finer crystals than potassium salts, so it does not seem to trap nitric acid as bad.


Sodium bisulfate NaHSO4 (sodium hydrogen sulfate)
Formed when making nitric acid with concentrated sulfuric acid and sodium nitrate fertilizers

NaHSO4 solubility in water
50g /100ml @ 0 deg C
100g/100ml @ 100 deg C
NaHSO4 is easily soluble in hot water. Also NHSO4 is soluble in cold water. Soluble in 2 parts cold water or soluble in 1 part boiling water. Decomposed by
Alcohol into sodium sulfate and free H2SO4.

Oneal, 
I would make the first batch more concentrated (as normal), the add water, then heat salts and re-crystallize for a second batch shooting for about 30 to 40% nitric acid, this would be strong enough to add to solution dissolving base metals with heat that also concentrates as it is reacting with metals, this more dilute nitric can also be used with aqua regia dissolving gold with heating, I would not be too concerned with just concentrating the acid by itself, but use it with heat and metals to get the best use out of it while it is concentrating and dissolving the metals in same reaction..

My byproduct metal-salts get reused (or saved), so I am not as concerned about some nitric acid trapped in potassium salts, although I use more sodium nitrate salts, and prefer them for cold reaction of making nitric acid, and if distilling stronger nitric acid I prefer the potassium nitrate salts.


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## Oneal58

Thanks Butcher, qst42know. 
I have tried breaking the salts up while forming. The salts that form are rock hard almost. I broke 2 of my coffee pots trying to break up the salts. I finally got my drill and drilled holes all around in the salts. This did help some, I got a little more Nitric out of doing this but nothing to brag about. I haven't tried vacuuming the salts to extract the locked up Nitric. I have thought about it, but I am concerned that while working on the salts, (trying to get them broke up) to vacuum the Nitric will dissolve some of the salts back into it. I am having some trouble with salts in my solution, when dissolving base metals. One time I let the solution sit a while without stirring. I was left with a mass almost as hard as metal in the bottom of the vessel. I had to cut it up with side cutters and crush each piece with pliers to break the mass back up. Fresh Nitric would not dissolve this mass untill I broke it up? I tried all day to dissolve this mass with no success.
Butcher, I haven't tried your last suggestion. I will try that and let you know how it comes out. I have been keeping the first decant of Nitric seperated from the last decants in seperate containers. 
After first decant, I would add just enough water and a little sulfuric and a touch of peroxide and heat (slowly) to get the salts to break up. Then I would go back through the process again. The last decant I would get would be about 30% Nitric after weighing it and comparing to the scale you sent me. 
But I will try your last recommendation and let you know what happens.
*OH, the bags of Potassium Nitrate I have are marked, (Krista-K /13.7-0-46) Soluable KN03 * Is this the concentration that everyone uses with this type method?
Thanks Everyone, 
Oneal


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## qst42know

> Potassium Nitrate I have are marked, (Krista-K /13.7-0-46) Soluable KN03



This is 5.3% higher nitrogen and 4.5% higher potassium than the numbers I have seen for potassium nitrate. You could try a single batch using 5.3% less nitrate and see if this helps. 

13-0-44


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## Oneal58

Hi qst42know, Butcher
Thank you for your post, qst42know I will try this to see if this is causing the problem? I made another batch today, got the same results as always. Poured off the concentrated first batch and followed Butcher's advice on the remaining salts. The salvage of the remaining Nitric in the salts are in the freezer now. A lot of work, Potassium Nitrate and time for 200ml of concentrated Nitric though. Butcher, I will let you know what concentration I come out with on this second run on the salts.
Qst42know, I will decrease the amount per your directions and try that to see if that's the culprit. The Farmer's Supply I bought the KN03 from asked me what type I wanted. I told him that it (KN03) had to be soluable and I wanted the cleanest, best grade that he could get me. I guess that's why I ended up with what I did. The Potassium Nitrate cost me $38.00 per bag? I thought this was kind of expensive for 60 pound bags? I have used 80% of 1 bag, so I have been at this for a while trying to get good Nitric to work with. 
*Question, If I take the temperature lower than -5 degree Centigrade will more salts form? Or has all the salts formed that will form at that temp? I can't tell because I used some of the lower strength Nitric that I know had salts in it on the last couple of batches of gold filled I have ran. Just to see if I would get the brown gas when I added the diluted Nitric. When I was (evaporating) driving off the Nitric I got a (whiff) smelled the salts in the solution. *
Thanks, Oneal


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## Oneal58

Hi Everyone, 
I have been refining gold filled Jewelry lots plus Sulphuric Cell lots, now for a couple of months. I have small buttons, medium size buttons, and want to make 1 large button. I went to the extra work on each lot following Butcher's and Harold's advice on Making Gold Pure. 
*Each button looks good but my question is,* 
Should I take this opportunity to re-refine all the buttons while putting them all together?
When I do the re-refine will I lose any weight (gold) during the process? I know I will lose a little weight but what can I expect to lose percentage wise just through handling losses? Even if all the gold is near .995 or better, with a re-refine are there losses due to just handling the gold again? Should I use a new melting dish for the final melt? I have a melting dish that I use to melt gold only. 
How often do you need to put more Borax on the melting dish? 
On each melt of values I have not used any Borax on the gold buttons. I could see no particulate on top of the buttons so I didn't use any borax. 
Would you suggest using borax on the final button?
What has been your experience in this area as far as losses? 
What would be your recommendation here? 
Thanks, Oneal


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## butcher

Others may give better advice on this.

Here are my thoughts.
but I would probably, just re-refine them, (depending on percentage of gold to base metal involved in-quartering with silver, then parting, could be needed), but from your description that is probably not the case, it sounds as though they may already be of very high karat gold, if they are fairly pure already in this case they will dissolve in aqua regia or the HCl/bleach methods (without in-quartering or pretreatment of nitric), melting and pouring shot, or flattening with a clean hammer and anvil will help them to dissolve into acid faster.

You will loose some weight in acid treatments (base metals left in solutions) when re-refining your gold, but you should not loose any gold if your careful with procedures, you will bring the quality up on the gold, possibly to the point a buyer will not have to refine it and then he can give you a better price it, also a jeweler may be interested in high quality shot.

If dish is clean, gold is fairly pure, just enough borax to wet the dish is all that is needed.
Also base metal contamination in a dish melting pure gold would lower purity of your gold, the dishes do not cost much (compared to the price of gold and the chance of lowering its purity), considering all the work you put into refining just get a new dish to melt the re-refined gold in.

The color of the precipitated gold can be somewhat of an indicator of its purity, if it is black or dark brown I would refine it again before melting, did you have any dimple pipe, or crystals on the gold button.


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## Oneal58

Hi Butcher,
Thank you so much for your post, I really appreciate you. I have called on you so often that I feel guilty sometimes. I don't want you to ever think that what you have done for me since the beginning isn't appreciated. I keep needing to say this to you, just so you know how big of an impact you have had on me. I just don't want you to feel like (he is overstaying his welcome)? Like company that comes to see you and then will not go home, If you know what I mean? :lol: 
But, I guess until you do tire of me I will just keep aggravating you. :lol: 
Butcher, I have a dimple/pipe on every button. Each button is consistent in color. I haven't noticed any crystals on the buttons. I have seen 24K gold before and I declare my buttons are the same color. My brother in law has a 5 oz. bar. I compared the color of my buttons to it. Same color. I went through the extra steps (Making Gold Pure) that you guided me through to turn out high purity buttons. I did this on each and every refine. I am hoping I am in the range of .995 at least?
1- Butcher, I will refine a couple buttons at the time instead of throwing all in one pot, just to be safe. Will this be best to do? 
2-I will order a few new melting dishes and use new ones. 
3-I will drill one out for making shot.
4-I will try to dissolve in AR after making small shot/*not *using the pre-Nitric treatment. Or would you do the pre-Nitic/could it hurt?
5-I will check for Indicator colors/Black or Dk. Brown to see if a new refine is needed?
6-Borax, just enough to wet dishes.
7-Do I need to Borax the one that I use to make shot with?
8-What does the crystals on the button mean? How should they look? Would they just glisten/shine when light hits them or is there a better way of determining if crystals are there?
Thank you Butcher, if you see where I made a mistake please let me know. 
Thanks Butcher,
Oneal


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## Harold_V

If you have a buyer that intends to use your gold when it's sold, he may prefer shot (jewelers often do, for it's much easier for them to alloy a specific amount of gold), but if you intend to sell it to an unknown buyer, you would be far better served to sell it as a button. Follow butcher's advice---use a clean dish, one that has been properly seasoned, and remove the gold the moment it freezes. That way it won't get trapped in the flux as it cools. Clean the button with heated dilute sulfuric to remove traces of flux. 

When gold freezes, the surface should be shiny. If it has a complex series of tiny crystals (or a general frosty surface), that's a pretty good sign it is contaminated. A shiny surface broken up by a large crystal structure is very good, as is a deep pipe. Any discoloration, regardless of color, is not a good sign. The melting dish should have, at the worst, a hint of pink through purple after melting. If the flux is discolored (brown, green, black, blue), that's a sure sign your gold was contaminated. 

Assuming you do choose to pour shot, yes, the dish should be prepared in the same way a dish is prepared to melt pure gold. It should have a 1/8" hole drilled in the center, then it should be warmed slowly to dry it fully. At that point it can be heated to redness, then sprinkled with borax. Borax glass or anhydrous borax are the best choices because they melt without issue, but any borax will serve. Coat the dish sparingly. Too much borax and it combines with the shot. Should that happen, boil the shot in dilute sulfuric until the borax has been dissolved. Rinse the gold well, otherwise traces of borax will remain, coating the shot making it white when it dries. 

Harold


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## Oneal58

Thanks Harold for your post.
After reading your post I went out and checked my melting dish that I used to melt all the the gold buttons in. But just the buttons in. My melting dish has a blue/blackish tint to it in the bottom and pink on the higher edges. The buttons must not be as pure as I thought and I guess I do have some contamination in one, two or more of the buttons? I can't remember or could I tell if all the buttons contributed to the coIor of the melting dish or just 1 did the discoloring? Just to be sure I guess I will just take the buttons back through a new refine, just to be sure I have the gold as pure as I can possible get it. Thank you Harold for your post and your guidance. 
*UPDATE, *
Harold, I went back out and took a picture of the melting dish I have been using. I have melted 7 buttons in this dish. You tell me what you think? Do I need to refine all the buttons again. I looked closely at the buttons again and it looks as though 1 of them has a tint of purple on it. This one could very well be the culprit of what you are seeing in the image below. But I am not sure of this? I see the pink you mentioned earlier and the purple, but how bad does it really look. The picture is true of condition of melting dish. What would you do if you were me?





Thanks, 
Oneal


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## Oneal58

Butcher,
I have another problem. I had at least 1, maybe 2 large pieces of Platinum Jewelry that tested to be Platinum. These were large brooches so there was a good bit of Platinum in these pieces. I think my wife added them in my last refine when she helped me clean up (one) day. When I decanted the first couple of times my decant solution was black, not greenish blue but black. I have read on the forum that Harold says that Platinum will dissolve in Nitric if the solution has silver in it. I know I had silver in the solution and I feel sure that my large Platinum pieces went into this last batch I ran. I have tried to get the silver to drop out of solution but I can't get the silver to drop? I know I have silver in it but it will not drop. I put a couple of drops of this black solution into a little HCL. I did see a little white cloud like appear this time. The first time I didn't see it, but I did the steps again and watched more closely. I believe I have dissolved my Platinum pieces in this black solution as well. I don't know how to go about recovering my Platinum out of these black decants that I feel my Platinum is in as well as silver? I have about 6 gallons of this blackish solution? Nothing that I have read addresses this particular circumstance? Can you give me any help with this? 
Thanks Butcher,
Oneal


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## butcher

If I understand you correctly this is a nitric acid solution used to dissolve the silver, but I would need more detail of conditions before this point to answer the question. Was this an alloy of gold and silver you in-quartered and shot that you believe you may have added platinum to by mistake, or what was the source and treatments prior to nitric acid?

Let’s look at some things while I wait for more detail.

Platinum will not dissolve in nitric acid.

Very little to no platinum will dissolve in cold aqua regia (a small amount fine platinum powder May somewhat).

Platinum is even difficult to dissolve in hot concentrated nitric acid but will go into solution slowly (powders would be somewhat faster).

If platinum is alloyed with (melted with) ten times its weight in silver then it can be dissolved into nitric acid.

So from the above your platinum would normally remain as powders if they were alloyed with gold and silver as quartered gold and silver, when being parted in the nitric acid solution, this would mean the gold powder (gold powders, also platinum powders mixed) which is insoluble in nitric acid would be left.

Lets look at the nitric solution for a second, unless you melted the platinum with a very high content of silver then it most likely contains no platinum, and you said you had a reaction (adding HCl of milky solution) indicating you still have silver in solution, which means to me, until you get all of the silver out of this solution (replaced by copper, or converted to insoluble silver chloride) you will not get the platinum out of solution if it is dissolved into solution, lets look at it as if we cemented out silver onto copper (too much free nitric acid may keep our silver dissolving back into solution until the copper nitrate uses it up, then silver will cement out first, if we did have platinum in solution it would cement using the copper buss bar after the silver was out of solution, this may be a very slow reaction, so it could take days. (It sounds like you still have silver but I am not convinced of platinum at this point).

Ok now thius solution of silver nitrate what if we had added NaCl table salt, or HCl to convert the silver in this silver nitrate solution to the insoluble white silver chloride, and what would happen to the platinum (if any was in solution), well some may be dragged down, but also we added HCl or chloride to this nitric solution so we now have made aqua regia, which would help to keep the platinum in this dilute solution, until we concentrated the solution and precipitated it with ammonium chloride or some other chemical reaction.

Now let see what would happen with our gold powders from above (for the sake of argument were mixed with platinum powders.

If we treated these gold and platinum powders, with cold aqua regia, platinum powders would not dissolve for the most part and would be left after gold was dissolved into solution as black platinum powders.
.
If we treated these gold and platinum powders in very hot aqua regia gold would go into solution first and then platinum would slowly dissolve also.

Lets say for sake of argument we had gold and platinum in this aqua regia solution, and we precipitated gold from a dilute solution after evaporation of free nitric acid, the platinum salts in this solution are water soluble, and would not precipitate using SO2 gas from SMB to precipitate the gold, if we did have platinum (after removing gold) in this solution we could concentrate it (to rid much water that platinum salts would re-dissolve in), and we could use ammonium chloride to precipitate the platinum.

We can also test solutions to see if we have platinum dissolved into solution.

There are several tests a person could perform on these solutions depending on what they were or what other metals may be involved in these solutions.

Aqua regia alone with platinum dissolved into solution the stannous chloride test.

Platinum with gold dissolved in aqua regia, a spot plate, precipitate gold with ferrous sulfate crystal, then move gold barren liquid to another clean spot in plate and test with stannous chloride.

The nitric solution I would cement out silver with copper buss bar (after removing silver) leave buss bar in solution and see if I did not get a black valuable cement from solution {possible platinum}.

I may also try to test this nitrate solution, in a spot plate some nitrate solution adding a few drops HCl, heat to evaporate and then test with stannous chloride, (other’s may have a better solution)


I have not worked with platinum, beside very small traces, I hope I will recover from my silver later, so my knowledge in this area is fuzzy, if someone see’s where I may be wrong, or if they can give Oneal better advice please speak up.

Oneal I hope you can follow my thinking, and please fill in some of the details needed here, so if your platinum did go into solution we can find it, but for some reason I do not think that it did, hope you keep stock pots, and your solutions (including waste)until you find it.

On second thought your platinum is probably the last place you left it, and the last place you will look for it. (Joking around), I hope you do find it soon.

Edit to add my thought on the melting dish, looks good, you have been doing something right, I will let Harold, give the advice on gold purity, as I am still learning too.


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## Harold_V

Oneal58 said:


> I went back out and took a picture of the melting dish I have been using. I have melted 7 buttons in this dish. You tell me what you think?


The dish shows the characteristics of gold that is slightly contaminated. The color in the bottom, green/blue is typical. The pink/purple color around the rim is typical of colloidal gold that has been deposited in the melting process. It's not a bad sign, aside from the fact that traces of gold are lost from the melting process. Just traces, understand, and there's not much you can do about the minimal loss. The values will be recovered in due time, assuming you process discarded melting dishes. 



> Do I need to refine all the buttons again.


That's a judgment call, Oneal. If the gold goes to a refiner, it likely will get refined again, even if you do it twice yourself. If your buyer is an end user, I'd suggest re-refining, in particular if there's even a hint of a chance that your gold has traces of lead included. If it hammers well, without splitting, it's probably fine, though. Traces of lead make gold very brittle. 



> I looked closely at the buttons again and it looks as though 1 of them has a tint of purple on it. This one could very well be the culprit of what you are seeing in the image below.


If you find a trace of purple on your button, it's likely encased in a trace of flux. I don't recall ever finding purple on my gold, although if it's contaminated bad enough, the entire surface could be discolored. What to look for is a shiny surface, one that looks gold in color, and has no rainbow effect anywhere. I've already mentioned a deep pipe. Gold that is contaminated won't pull a pipe, so anyone that sees your gold that knows anything about gold will recognize the pipe as an indication of quality. The novice may not understand that, so don't be discouraged if someone makes a less than flattering comment about the presence of a pipe. 

My advice here? If you hope to produce fine quality, yeah, refine it again. I did that with all my gold, and did it routinely for years. There was often no need, but by running it a second time, traces that are less than desirable are eliminated. I never claimed 4 nines gold, but I felt comfortable offering a guarantee of no less than industry standard quality (9995) because of the second refining. It served me well for years. 

If, by chance, your objective is strictly to recover gold for resale, and your buyer is not an end user, refine once, melt, then sell. That will minimize the amount of work and offer the best possible profit. If you do your work well, eliminating base metals before dissolving values, and introducing traces of sulfuric to eliminate lead, then follow a good washing procedure, you should be able to come quite close to 9995 quality. Your melting dish will tell you if you aren't getting the job done, as will the surface condition of the button. 

Here's one thing to remember when melting gold. In the pure state, it's perfectly tranquil. It will melt peacefully, with a yellow green luminescence, and a bright, shiny surface. If you see any type of oxide developing from the center of the button, moving towards the edge, where it is absorbed by the trace of flux in the dish, you'll know your gold isn't pure. The dirtier it is, the greater will be the oxide I speak of. You should be able to melt your gold without flux and have it remain bright and shiny if it's pure. That's assuming you use clean equipment, of course. Do not use anything that's dirty when handling pure gold. 

Harold


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## Oneal58

Hi Butcher, I am just getting in and reading your post. By the way thank you for your post. I have read over this post a couple of times, I will read back over the post with a fresh mind tomorrow a couple of times. It's after 2:00A.M. here and I been going all day. 
Butcher, this was the largest refine, by my standards that I had tried. This was almost 4 pounds of gold filled/Scrap Jewelry. Broke Hoke's rule, beginners start with too large of lots! 
This was a Nitric refine, evporate down, add more nitric, and do again, time after time. This went on for a couple of days? I finally ran out of 70% Nitric and started making my own. Finally, I figured out something was wrong, (using too much nitric to dissolve this gold filled compared to other lots). What caused this I believe is that I let the solution evaporate too long 1 time. I had too many Irons in the fire at one time and lost track of time. Due to this I had a nearly 2" thick brick of what I will call a (metal salt brick) form on the bottom of the 1800ml beaker. The Nitric would only work on the outside edges of this brick. It (The Brick) had all the gold and all the undissolved metals locked up in it? The Nitric could not get to the metals to dissolve them but this brick would use up the Nitric but not getting any work done? I decanted, I had to break the beaker to get the brick out. I cut the brick apart with a large pair of side cutters and then crushed the pieces up with another set of large linemans pliers.
I finally got the Nitric back to doing the work it's suppose to. This is where the black decants came into play. The first 2 decants I had were black? Then they turned the common greenish color. 
If I understand you correctly and please corrrect me if I am wrong but the first thing I need to do is check to see if in fact the platinum is even in the solutions. 
1-I will use spot plate to test nitrate solution/add few drops HCL/heat to evaporate/then test with stannous chloride, if barren, do the following.
2-Aqua Regia solution with values, a spot plate, precipitate gold with ferrous sulfate crystal, then move gold barren liquid to another clean spot in plate and test with stannous chloride.
If no positives for Platinum shows up here, I can stop worrying and start looking where my wife put those Platinum Brooches. I might have to let her back in the house long enough to find them. :lol: 
Butcher, it's got to be the last place my wife left it, she is getting blamed for it regardless of who misplaced the pieces. It's too late to beg off now if I am wrong, the damage is already done. :lol: 
Let me know if I am going about this wrong Butcher, I am really tired tonight and very well could be off base. 
Thank you for your post. 
Oneal


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## Oneal58

Hi Harold, thank you for your post and directions. 
Harold I believe I will get into the habbit of doing a re-refine on each button lot I produce. I have to melt it again anyway to get buttons into a bar so I think I will just go ahead and re-refine each button lot each time I have enough to pour a bar. I am not on production as you were in your business and can work on the lots I refine at leisure. But I am finding I spend more time on the refining than I did when I was working a job full time. I feel as you do though, the re-refining is not a bad habit to develope. 
I have always followed your instructions on Making Gold Pure on every lot I have refined. I did not use any flux on any of the buttons I have refined. Reason was, when I was melting the buttons I did not see any foreign material or particulate on top of any of the buttons. 
So, my decision is to just re-refine every lot I produce. If for nothing else but just self gratification and feeling good and confident about the lots I turn out. The Gold Filled Jewelry lots, dirty watch band tops, Etc;, have human skin, hair and oils on all the lots I refine. It is really rewarding to see what these beautiful pieces of gold were at one time and what they are now. It makes you feel really good inside. Hopefully without sounding arrogant, kind of proud of yourself. 
* I must note*, without this forum and the free hearted individuals on this forum this would have been *IMPOSSIBLE *to accomplish on my own. And I must note also, especially one individual, who has been my tutor, just about every single day from the beginning, he knows who I am talking about. 
Thank you Harold for your advice, This advice has aided me in making the right decision.
Oneal


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## butcher

Oneal


I would test solutions for the platinum.
If this broach was platinum I feel you would have noted it as something very hard to dissolve, if it did get put into solutions.

You could also check stock pot sediments, you would have to put some powders into solution most likely to test it,(as any metals higher in series would cement the Pt from solution in the stock pot).

Someone else may be able to give better advice, and have a better method to test the solutions.

If you did not melt the platinum with high volumes of silver, it would more than likely not be in the nitric solution, (no harm in testing, it would be better than my guess).

Oneal,
About the only thing I can give you advice on is, your wife is always right, I thought you have been married long enough to learn that by now. (I know I have been stubborn learning that lesson also).

It is much easier to re-refine the powders, (at final stage’s of the first refining process), before you melt them back into metals, (they go into solution with ease), this way it is not like doing a whole process over again, but is more like repeating final stages of the original process. 

Also some suggest using a different precipitant the second time around.
Paying attention to Harold’s advice of trying to get out any lead that may have followed through the first refining, I would make a note of that, re-refining your gold will give you a chance to see how higher quality gold acts in solutions, and also it could show you how much impurity you may have missed the first round, although it does sound like you done a very good job with the first refining.


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## qst42know

Have you tested your solution for palladium? 

If these broaches were palladium instead they could be in your nitric solution.


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## Oneal58

Hi Butcher, Thanks for your post.
I Acid tested the brooch and pendant probably 6 months ago. When I was just getting interested in refining.
*First*, I noticed that this material was much harder than any of the gold pieces I tested. I first tested the pieces for 14K and the deposit on the testing stone never did dissolve. I tested for 18K, same thing.
I then used the Platinum Test Acid on the pieces. The deposit did not dissolve, at all, or change color, that I noticed?
So I figured they were Platinum. I had already accidently put the pieces into a Nitric refine once before. They did not dissolve any that I noticed. I then put them back up in a seperate location for later. 
Then this time they may have been put back into another Nitric refine, I had a good bit of alloyed silver that I put into this Nitric Bath this time thinking it was alloyed with gold. Came from an old Jewelry Store Auction, years ago. So there was a lot of Silver in with the pieces this time, not like the first time where just a very little silver was in solution. Then trying to research what to do, I found a post that said if you have a high silver content in the Nitric Solution, it (Nitric Solution) will try to dissolve Platinum. I ran this lot many times, for days. So, if they (Platinum Pieces) were in there, (Nitric Solution) they had plenty of time to dissolve this time around with all the silver in the solution as well. 
I will do the test that you have previously recommended next week on stock pots to see if they test positive. 
Question 1-Is Platinum noticeably mcuh harder than gold would be? 
Question 2- Qst42know asked me if I had tested for Palladium, I haven't. Would these pieces have behaved the same way under the acid test that I ran if they were Palladium? Does Platinum and Palladium behave similar when being refined? I must admit I haven't had time yet to study the behavior of the Platinum group metals, yet. That's why I was saving these pieces until I finished up the gold I have. I have an old packhouse I used to put auction purchases in/and to get auction items together in. I keep running across Jewelry all the time I packed up years ago. So I have had more Gold Filled/Gold Jewelry to refine than I first thought I had. But anyway, I was going to study this group of metals in more detail when I got to the point of being able to refine them. I have all my used solutions, every last bit of them. I know I have made mistakes and I expected to make mistakes so I continue to save all my decants. So, I have the PM's somewhere, it's just that I got to find it. 
I am going to sneak back over to the old house (while wife if gone) and give one more good search for the pieces. It would be good experience to go through the testing for the Platinum, but I am not quiet ready yet. I still have other refines ahead of this. So, I am going to make sure that I am not overlooking the pieces so my testing would not be in vain. 
And yes Butcher, I have had to beg off and accept the responsibility of misplacing the pieces. She (wife) was only trying to help me. And as you said, she is always right, no matter what I think???
Thanks Butcher,
Oneal


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## Oneal58

Hi qst42know, thank you for your post. 
Qst42know I haven't tested for Palladium yet? I am at the point of having done a HCL Boil on material. I must admit I haven't studied the Platinum group metals behaviors yet? Been too busy with gold refines.
Question 1- If these pieces were Palladium, would Palladium have dissolved the first trip through a Nitric refine? The pieces I had already survied a Nitric bath previously by mistake. Would Palladium have dissolved in the first Nitric solution if very little silver was present in solution. The difference in this time is that I had a lot of silver in this refine. I dissolved some sliver that was alloyed with gold in this refine? So there was a lot of silver present in the nitric solution this time verses very little silver in the trip through the Nitric Bath the first time? 
Thanks Qst42know,
Oneal


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## qst42know

Platinum must be alloyed with silver to dissolve in nitric. Silver in solution won't change that.

I have encountered a very old piece of gold over silver that tarnished so bad from co-migration you couldn't tell what it was. It looked like gold but survived an AR bath. If you hit one of these with AR (like platinum test acid) you would have produced silver chloride and may have drawn the wrong conclusion.

There are some side effects from poormans nitric that don't resolve easily.


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## butcher

I agree if these were silver, they may have dissolved in nitric, they also would not test for gold in chloride solution. 
They may not have been platinum, but unless you find them we will not know for sure.

Like qst42know, says unless the platinum and 10 parts silver were melted together, nitric would not touch them (no matter how much other metal silver was dissolved with them in solution), unless they were silver or palladium (then nitric would attack them).

if you did not throw away any waste or material, if they valuable and were in the batch you can recover them no matter what valuable metal they were.


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## Harold_V

It should be noted that when palladium is a part of an alloy, unless it's present in miniscule amounts, it will discolor the solution badly. If it's present in a small amount, a solution that would have been blue would be green, and if it's present in volume, it may well turn out to be dark green through brown. So then, if palladium is present, it's usually very obvious. A quick test with stannous chloride is generally enough to reveal its presence, even in trace amounts. When all else fails, a test with DMG will usually be conclusive. 

Harold


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## Oneal58

Thanks everyone for your post, I have been down sick again for the last few days. I never did shake that flu entirely and working late in the cold/rainy weather it's (flu) tried to jump back on me again. I can't go out and play, I am having to stay inside. This is (wife's order's) until I am completely well this time. I will have to admit though, that's all I feel like doing. When I am able to go out and play again I will let everyone know what the status of this is. But one thing I know for sure, I will take the flu shot ahead of next flu season.
But thank you all for your post, they are appreciated. 
Oneal


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## Oneal58

Hi Butcher,
I have another problem that I just don't know what to do about. I follow your directions/instructions when doing a refine, I go through each and every step, sometimes an extra step or two depending on the condition ( how contaminated) that gold powders were in.
On this last refine while incinerating between HCL Boils, rinses before Nitric Treatment I over incinerated the powders and made some small balls of Gold. I have been trying to get the AR to dissolve these little balls of gold. After 3 treatments with AR I still have not dissolved them? 
I feel that they (gold balls) have contaminates in them. I was going to run Harold's (Making Gold Pure) method as usual on the droped gold to clean out the impurities. 
Would you inquart these little balls of gold and re-refine or hammer them really thin and treat with pure homemade Nitric or other? Or just put them in the dropped gold and re-refine the whole lot together?
One more thing, will I need to evaporate (strengthen) my homemade Nitric to treat these little balls of gold with if that's the best method to go with? I have been sick and am not thinking too clearly yet. Thank you for any advice.
Thanks Butcher,
Oneal


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## butcher

Oneal, 
If these balls do not dissolve in aqua regia, will they dissolve in nitric? (I do not know the source of this gold, but could it have had some silver in these powders?

If your nitric is very dilute I would just heat it with metals the heat will help the metals to dissolve into solution and will concentrate the nitric at the same time.


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## Oneal58

Hi Butcher, thank you for your post. 
This is another Gold Filled Jewelry lot that I am refining and this lot did have a good bit of silver in it. This is another one of the lots that came from a Jewelry Store sell out. There was a package that was marked (Alloyed with Silver). I did assume that this material was alloyed with gold but it could have been alloyed with something else? I have treated this Gold Filled Jewelry lot multiple times with Nitric, multiple HCl Boils also. I also went through the HCL Boils/Rinses with hot water, also added about 10 drops of sulphiric, then concentrated solution, dried, washed and incinerated again to make sure to drive off any acids. I got the powders too hot when incinerating the last time, resulting in making little balls of gold that will not dissolve in AR Treatments? I am just letting the AR solution sit until I can find out the best way to tackle this refine with the small balls of gold that I accidently ended up with due to gettig the powders too hot when incinerating the last time. The little balls of gold are in with powders that would not dissolve for some reason? 
Butcher, I had a small amount of gold powders that I added to this lot.* I had already dropped a previous lot of gold with Stump Out and washed several times. *
*I guess it is possible that I didn't get all the Sodium Metabisulfite completely out of this gold powder. If I did not get all the sodium Metabisulfite out of the powders that I added to this refine what would the indicators be if added gold powders contaminated with Sodium Metabisulfite to this refine before a HCL Boil?*
Just wanted to know your thoughts on this refine before I move forward on the refine? Should I just drop the gold out of the AR now and then treat the little balls of gold in a seperate refine by inquarting or try and dissolve in pure Nitric. I will have to concentrate my Nitric and the salts that are left from Homemade KN03 is a concern for me and I wanted to ask you about it. 
One more question, if you leave a container open to the air, will Nitric slowly work it'self out of a solution or do you have to drive the Nitric out of solution by evaporation or neutralize the Nitric? I guess what I am asking is, will HCL, H2S04, HN03, Etc;, slowly become neutral in a solution if you leave it open to the room temperature or will acids stay in a solution for extended periods of time until it is either driven off by heat or neutralized? 
An important lesson I have learned on this refine is that you do not try and work when you are sick with the flu!!
Thanks Butcher for any guidance,
Oneal


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## kadriver

Oneal58:

Howdy, I tried to dissolve two tiny pieces of platinum to make a standard solution. It took me over 8 hours to dissolve .1 gram of pure platinum!

Even then I did not get it completely dissolved - there was a tiny piece left over about 1/10 the thickness of a hair (approximately).

I added multiple doses of hot concentrated aqua regia.

Platinum if very difficult to dissolve!

Also, I harvested my first platinum metal today from two catalytic converters, please see:

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=51&t=12455

Thanks - kadriver


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## butcher

I would treat these small balls, separate from the rest of the powders, if they would not go into solution (aqua regia).

I do not know what they are, much would depend on what metals these powders being incinerated contained, but if they would not dissolve in aqua regia, I suspect they could be high in silver or lead or some other metal insoluble as a chloride or that would passivate in the aqua regia solution. The platinum group can be very hard to dissolve in aqua regia (some of them will not dissolve in aqua regia), but from your descriptions I kind of doubt that is the problem, first of all considering the source, (unless this is your missing broaches), and secondly I would think that other metals would melt into balls long before this more noble metal like platinum would. 

If these small balls were high karat gold they would dissolve into aqua regia.
If they were silver and gold melted together they may form a passive layer of silver chloride and not dissolve further. (And also may not dissolve in nitric because of gold), in this case inquartation would help.

There are very few metals or combinations of metals that would not dissolve into aqua regia.



I would wash these balls well and try nitric, if no luck there then, inquarter them with your next melt.

As far as acids evaporating in open air if stored in open air. 
Much would depend on the concentration of the acid (water involved), the temperature, and what acid.

Many of these acids are made from gasses dissolved in water.

NO2 nitrogen dioxide gas dissolved in water forms nitric acid, (one of the more volatile acids), if it was concentrated it would fume off strongly we also call it fuming acid, even at 68% concentrations it will decompose slowly (again depending on temperature) gassing of NOx gases, nitric acid will also decompose in light. if the acid contains more water (more dilute), these gasses can dissolve back into solution easier as the acid decomposes, so less would be lost to fumes, storing in direct light would still try and decompose even a dilute solution.

HCl hydrochloric gas dissolved in water to form hydrochloric acid if the acid is concentrated say 32 % and the bottle is open it will release fumes of HCl gas, again temperature can have an effect on how fast the gas fumes off, a very dilute HCl these gases would mix back into water easier and not leave the jug so easily.


Sulfuric acid is usually SO2 sulfur dioxide dissolved in a water and H2SO4.
Sulfuric acid is not very volatile and would need a very high temperature before the SO2 gas would evolve, so mainly water would evaporate from the acid and it would concentrate further.


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## Oneal58

Hi Kadriver, thank you for our post. I have been down in bed with something I can't seem to shake. I haven't been doing any refining this week at all. Kadriver I haven't felt like following your post on your Platinum recovery but I hope to feel better in a couple of days and I will go through it. Did you find it was much more involved than the gold filled lots you have refined. Do you plan on pursuing the catalytic converter refining? 
Thanks, Kadriver
Oneal


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## Oneal58

Hi Butcher, hope you are doing well. Been down this past week in bed entirely with a touch of pneumonia. I decided the best thing to do was to wait untill I am over this stuff before I go back into the cold and wet again. 
Butcher, 1 thing I wanted to ask you, IF I accidently added some Sodium Metabisulfite between HCL washes what effect would this have had on the gold I was refinning? I added some gold powders that I had already dropped. I had washed the gold several times to get the Sodium Metabisulfite out. But after adding the gold I could smell the Sodium MetaBisulfite very strongly in the vessel that I used to add the gold to the larger lot. The reason I ask this is because it seemed like the looks of the refine I was working on changed. This happened between 2 HCL washes.
One other question Butcher, do some refiners use .925 sterling to inquart with? Or does that just add .075 other metals in with the gold you are inquating?
Thanks Butcher
Oneal


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## butcher

Oneal, I sure hope you get to feeling better, be careful about laying in bed too much with pneumonia, your lungs need exercise to keep fluids in the lungs from buildingup. if this is so bad for so long maybe seeing a doctor, is not a bad Idea.

I would think that the sodium metabisulfite would wash out with hot water and dilute HCl.
If gold was already reduced to metal, (brown gold powders), I cannot see the SMB chemically reacting with the gold.

Using sterling silver to in-quarter the gold with is great, it helps me get my silver purity up and helps me in first steps of refining my gold.

Get better soon.


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## Oneal58

Hi Butcher, thank you for your concern and advice. I will take it. I have been at the Dr. twice this past week and at the hospital having X-Rays done. I only have it in 1 lung so I am fortunate or blessed I meant to say. I just got to be more careful with my health, working in the cold rain just isn't going to cut it anymore with the condition of my body.
Question 1-Butcher, if hot Nitric will not dissolve these powders in the vessel after several tries can't I safely assume I found my missing Platinum brooches. I haven't tested to see if the powders are platinum yet but is there anything else these powders could be? Because boiling in Nitric several times for hours does not faze the powders? 
Question 2 Butcher, if these powders are in fact platinum will I have a small amount of platinum in my gold drop from this material? 
Question 3-And if so, do I have to inquart and re-refine to seperate the platinum and gold or is there another way to seperate the two PM's before inquarting? Going through Harold's (Making Gold Pure) process will not help any here, will it?
I can't wait to get back on this lot, I feel I will learn a lot here. But the weather is nasty and I have learned my lesson. I have been house bound for almost 9 days now. This is getting old, I have watched enough news these past 10 days to make anyone sick. Especially watching the politicians who do nothing but waste good air time. We could have Larry the cable guy as President and he could get as much done with this congress we have running this country! Just rediculous, just rediculous. No common sense to be found in them, anywhere!
Thanks Butcher in advance for your answers,
Oneal


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## butcher

Oneal, 
I will answer the best I can; some of our other members could give much better advice.

I try not to assume what a powder is, but I may try different methods and try to get a good idea as to what it is, for all we know these could be silver chloride, although right now I do not remember what these powders were from (gold fill or plated) and what they have been exposed to up until this point without going back and reading all of the posts up until this question, and we have discussed so many things and with my pea brain memory I will just post some things.

I am supposing if your trying to dissolve these powders in nitric acid you have already eliminated any chlorides, (chloride salts of previous acid treatments using HCl), or (have not used chlorides), and you had no trouble filtering nitric (tin problems), if any of these we would need to change our approach here.

These powders will not dissolve in nitric (without considering silver chloride), or very few other metals, this is a good indication of possible gold and platinum group metals.

(Some palladium may show up in our earlier nitric digest as well as silver, (and base metals) the solution can be tested to see, or these can both be cemented from nitric solution with copper)

Gold dissolves easily in cold Aqua regia, platinum will not as far as practical purposes, (some traces of these metals may go into solutions or stay behind, so this is always taken into consideration), so we can dissolve gold from the platinum (if this is what we have), with cold Aqua Regia, leaving possible platinum group and other insoluble substances as powders, this gold solution decanted, denoxxed, diluted, and let sit 24 hours for anything to settle before decanting and filtering then to our precipitation vessel to retrieve gold (traces of values to stock pot). (Using your stannous chloride tests you can follow your values in solution, your eyes as to what you have where),

Now we can dissolve platinum in boiling hot aqua regia. Powders go into solution easier than solid metals, but it may take some time even for the platinum powders to dissolve, so adding some water, or acids (with their water content a little at a time while heating), can let you heat strongly without concentrating off the acid into fume’s before it has a chance to dissolve the metal powders. (A few drops of this solution can be denoxxed in test tube using hot air heat gun or other heat source, or using small glass vessel jar on electric coffee mug warmer or Mr., Coffee hot plate, in white spoon, or spot plate with ferrous sulfate for gold, letting brown gold precipitate in test and move remaining liquid to next spot on spot plate or to another white spoon (or Q-tip) to test with stannous for platinum looking for orange), depending on tests, gold can be precipitated with ferrous sulfate (copperas), or sodium metabisulfate, after separating liquid from any brown gold powders, the platinum can be precipitated using Ammonium Chloride.

I still find it hard to believe you would have broken any platinum down to powders, during your processes, I have not worked with platinum except for traces, but from my understanding if in metal form of much volume it is close to impossible to get it to dissolve to any extent with out working hard at it. So I would use testing solutions, and these test can be preformed on very small amounts of powder before processing whole batch, this can also help you to decide what steps to take before you begin.

Oneal, sometimes trying to help someone who is not familiar with all of the processes or variables one can encounter can be very hard, because many times when I work my processes are determined in steps usually governed by my tests or what is needed at that time, it is hard to say do step 1234, as when I work I may find that after a test or some other factor, that steps 1231 then 23423 would work better in the process I am working on, it is also very hard for me to know or remember what you’ve done or where your at in a process, or to be able to give advice of the next steps unless I am doing the work,

I hope your spending some of your rest time in bed with a good Hokes book.
Take good care buddy I worked today and am very tired so I really do not know if anything I wrote here is worth a dime, its about 4 hours past bedtime good night, 


your friend butcher


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## Geo

Oneal, 

i have COPD bad,and if i even get a whiff of chlorine or NOx i cant breathe good for days on end. i get a pneumococcal vaccine every five years and a flu shoot every year. you may ask your doctor about getting vaccinated for both when you get better.


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## Oneal58

Thanks Butcher, Geo. That is something I will ask my Dr. about when I go back tomorrow for more antibiotics. 
Butcher the sun came out today and it warmed up nicely. Though still feeling terrible I did walk over to the old house just to check on things. 
I had dropped the gold out of the last refine of gold filled jewelry before I got really sick. The gold drop was just sitting there in Sodium Metabisulfite. I stuck a Q-tip into the sodium metabisulfite and then put a drop of stannous on the wet Q-Tip. The cotton turned a black color, not purple but black? I didn't do anything else with the solution, just covered it back up and came back in the house. 
Butcher do you know what could have caused the cotton swab to turn black when stannous was added? If the metabisulfite wasn't holding any metals shouldn't I have gotten a negative test result? The gold had settled nicely on the bottom of the pot and the solution was clear but had a bluish tint to it?
I might had stumped my toe with the stump-out when dropping the gold. I usually dissolve the metabisulfite and then add to drop the gold. This was the first time I just used the stump-out straight out of the container and had far less control on the amount I put in. I will not do that again though. If I had an excess of sodium metabisulfite would this have caused the cotton swab to turn black? I just made a fresh batch of stannous right before I got sick so the stannous is fresh. Any ideas?
It seems that my thinking is not clear enough yet to mess with anything, especially these acids. The cough medicine I am taking must have something in it, makes me woozy! :?: 
Thanks My Buddy,
Oneal


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## Geo

false positives are brown and are mottled and not uniform. sounds like you have a positive for gold. take a small sample (just a drop really) and dilute with about three drops of water and test again. this diluted solution should give the purple color you are used to seeing.


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## Oneal58

Hi Geo, tried that but got the brown color???? Thanks Geo, Oneal


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## Geo

I've seen AR do that when the solution runs out of hcl first before the nitric is spent. this may not be the solution to your problem but if the dilute sample showed negative then its pretty safe to say you have dropped all the gold.


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## Oneal58

Thanks Geo, got the brown color on the swab like you said was a false positive. I didn't take the solution down as far as I normally do when I was evaporating the Nitric off this last time. I very well could have had a little nitric left in solution. I broke my container last time I took the solution down to a thick syrup so I didn't take it down as far this time. I guess I depended to heavily on the HCL to drive off the Nitric if any was there. Short cuts, but I see now there are no short cuts. 
Thanks Geo,
Oneal


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## Oneal58

Hi Butcher or anyone who knows the answer to this. 
Can I use a large stainless steel container to cool my homemade nitric in? Instead of cooling the nitric in a closed container, such as a coffee pot I thought I might have less nitric locked up in salts if I used a large round open bowl that is made of stainless steel. How quickly will the acids attack the stainless? It will have to be left in the bowl for hours while bringing the temperature down in the freezer. I thought I would make the Nitric as usual in the coffee pots but then pour into the large open stainless steel bowl. Thinking a lot less nitric will get locked up in the salts this way. I am losing a lot of Nitric from fluid being locked up in the salts after making it. This large bowl is open and flatter and maybe the salts will not be able to lock up as much nitric. I thought I would give it a try? Or how about a thick plastic bowl, tupperware maybe? Will tupperware hold up? Haven't made it back to work yet but feeling better today. I know I have to make some new batches of Nitric first though. Maybe in a couple of days or so?
Thanks Butcher,
Oneal


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## Geo

if the stainless is the ordinary kitchen stainless it will attack it immediately on contact. stainless series 300 or better is used for nitric.


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## Oneal58

Hi Geo, thanks for your reply. 
Is there a way of telling what series stainless you have? My sister works for this School District. She makes the purchases to keep the kitchens in the schools supplied and running. She also gets (for me) the old stainless steel items that get bent up, mixer funnels, Old Hobart Mixers, grinders, slicers, such stuff, that has worn out or needs repair. I will fix what I can and sometimes get lucky and make a few dollars. I have just got back from her house and she says that the school buys the high grade stainless but doesn't know what series the stainless would be? Says she doesn't ever remember seeing what grade of stainless it is she purchases on her paperwork. But what the school pays for these pots, pans, Etc;, is rediculously high! The pieces I have are thick and heavy, much thicker and heavier than anything you would see in a retail store that I have found. 
Can I assume that this stainless is a high grade stainless because of the thickness and weight? If not, is there a way to test it to see what grade it is other than putting the acid in there and waiting to see what happens? 
Thanks Geo,
Oneal


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## butcher

The way I understand concentrated will not attack higher grades of stainless steel.
But dilute nitric acid may attack it.
The concentrated acid will oxidize and passivate a layer, so the acid is blocked from further attacking the article.

I would study this more as I may be mistaken if dilute nitric will attack it.

I usually use glass, although I have bought nitric 70% in some white plastic jugs it looks like thick walled (HDPE), I really did not check the type of plastic and can be wrong of the type, I will look tonight and see what letters are on them.

I have let my potassium nitrate cool in empty brown 3% hydrogen peroxide bottles, these worked good as the brown plastic kept light from decomposing the acid, after decanting (or pouring off) the chilled nitric solution, I could bang the bottle to break up the salt brick in the bottom, sometimes adding some water and a little peroxide to these salts would free a little dilute nitric from the potassium sulfate salt.

The higher grades of stainless are non-magnetic.

Thickness of the metal will not give any clue to its composition or type.

Harold has posted some information about stainless; he also understands these metals well, a search of stainless steel and Harold, as author would be an interesting read.


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## Oneal58

Hi Butcher, bigger problems now. I mentioned a couple of weeks ago about me not being able to get some powders to dissolve in the last batch I ran, (lost brooches). I also had some gold that the first run with AR didn't dissolve so I put the batch back through another AR treatment. Then I got sick, from time to time I would walk out to the old building and heat up the AR just to try and get the remaining gold to dissolve. One day I left the batch on heat most of the afternoon. I felt good enough today to go back out and inspect this batch. *This batch is nearly 3 weeks old now*. Has been sitting in either hot or cold AR for nearly 3 weeks. I tested the batch to see if the gold had made it to solution. What I found is below. Powders are still in the vessel also that will not dissolve. But I am suspicious I found my missing platinum brooches. But now it is mixed in with the gold. I don't have a clue where to go from here? Platinum and Gold mixed in AR. How in the world do I seperate the two.
Thanks for any help here Butcher. 
Oneal


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## Geo

Oneal, 

Hoke tells us to precipitate the gold first with ferrous sulfate (copperas). it will selectively react to the gold, it may drag down a trace amount of other metal but its only a trace.


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## freechemist

Hey Oneal58,

If you really have platinum and gold as a mixed solution in AR, you can separate them by precipitating gold with oxalic acid:

1.) Eliminate HNO3 by repeated evaporation and addition of fresh HCl the usual way.
2.) Dilute the residual concentrated "denoxxed" solution with water and a few ml of HCl.
3.) Add a 10%(weight)-solution of oxalic acid dihydrate; 12 ml per gram of dissolved gold.
4.) Mix well and let the loosely covered beaker stand on a nearly boiling waterbath, at least over night.

After this time of hot digestion, precipitation of metallic gold usually is complete. Platinum will not be much affected and remains in solution, from which it can be recovered by cementation.

Good luck and regards, freechemist


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## butcher

Decant solution from well-settled powders, siphon aqua regia with suction bulb, solutions can be tested after small sample denoxxed. use the spot plate test we discussed earlier in the thread, with ferrous sulfate for gold, and then testing barren(for gold), solution tested for platinum.

The aqua regia solution if tests show a positive for values.

You can de-NOx solution using evaporation methods, (dilute to precipitate silver), the values in solutions precipitated from the aqua regia solution, ferrous sulfate for gold, from dilute solution then concentrating and ammonium chloride for platinum (only if these show up in your tests), if only traces (stockpot).
I did not go into detail about letting settle overnight, decanting solutions from precipitated powders and filtering before using the next reagent to precipitate the next batch of metals.

Another alternative is cement values from aqua regia using copper buss bar.

Which of these two methods I would decide to use, depends on test results and how much base metals I had in the aqua regia solution, and value content of metals in solution.

The powders I would wash well with boiling hot water, noting color of water washes, and letting decanted water cool in jar to see if lead compounds formed when hot water wash cooled (depending on what I see would give me clues as if I would need to remove other base metals from these powders. (Also how well the aqua regia filtered can give me clues of tin content)

If powders were just pretty much values (low in base metals), dissolve the gold in cold aqua regia, leaving insoluble powders (possible platinum), treat normally as you would gold in solution, after precipitating gold using ferrous sulfate take small sample of dilute solution and test for platinum if hardly any in solution it can be retrieved in stock pot.

To the remaining powders use very hot aqua regia to dissolve platinum. 

(This could be done with only a small portion of powders and aqua regia for testing purpose so if these powders did not contain values you would not be wasting time and trouble working on the whole batch).

Since we think these powders are mostly platinum I would probably just keep solution fairly concentrated while putting powders in solution adding small amounts of acids as needed, once in solution, denox any free nitric, keeping solution concentrated precipitate platinum using ammonium chloride, (test solution), traces of gold to stock pot.


I can write a process that may or may not work, as in recovery or refining each step taken depends much on what you have, and test results, so following a procedure as step one two three may not work as well, as if you understand the tests and clues you have while working, and the understanding of what step you may need to take when and why, by using your eyes and just seeing which way to go, that way you may not trip on something I cannot see from where I am.

Read Hokes here is where you will learn which steps you may need to take and when and why.

Now is the time to study Hoke's book, while you cannot be out in your cold lab.

Hokes book and some bed rest and fluids and you will be back on your feet in the lab with a whole new insight.

freechemist gives good advice, we each may go about a chore in some different mthod.
Oneal get well.


----------



## Oneal58

Thanks so much Butcher, Geo for your help. I have a general idea of what direction I need to go now. I will get back into Hoke's over the next few days and do some more studying while down and out. I am still prescribed bed rest but I feel good enough to sneak out a few minutes here and there while the wife is in the shower or gone shopping. Will try and get the spot test done and post the results over the next few days. 
Thank you all for your help, this is a wonderful site to say the least. Thanks to all of you who guide and direct me through this undertaking. But for me, this endeavor has proved to be somewhat more difficult than I first expected and has gained my respect, as you all have? But everyone knows that anything worth having deserves your best efforts, at least. Will let you know what I find out.
Thanks again,
Oneal


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## kadriver

Oneal58:

I just did this procedure. I used ferrous sulfate (copperas) to drop the gold out of the solution containing my PGMs.

I added 1 gram of copperas and the gold precipitated out perfectly.

I allowed it to settle overnight, then drew off the clear golden liquid containing PGMs.

I poured the gold into a filter paper in my vacuum filter and trapped the gold in the filter paper.

I then incinereated the filter paper until it disintigrated in a melt dish with lots of borax to keep the ashes in the dish (otherwise they fly out all over the place - causing lose of values).

I recovered a small bead of gold from theis process!

Here is the post with pictures:

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=51&t=12477&start=40

kadriver


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## Oneal58

Thanks Kadriver, I appreciate your post. Kadriver, how did you end up with gold in your platinum, as I did? Was the platinum really hard to get into solution with the AR for you? 
Also was your gold/platinum mixed solution a light red color. My solution I put my platinum brooches in has a redish tint but it is not a dark red? It's sort of a yellowish red? What are you going to cement out your Platinum with? 
Kadriver, tell me, if you will, what did you think about your Platinum Recovery? Was it worth the trouble it put you through? Do you plan on continuing on the converter's? I have been following your post on your recovery. I see it takes much longer than it does to refine Karat Gold. So I am just curious as to whether you are going to continue with the platinum recoveries.
I bought a bag of Ferrous Sulfate a while back I haven't even opened yet. I will try and drop the gold with that, as you said hopefully monday. I have 2 batches of this solution with platinum mixed in with the gold.* I was caught by surprise on the first one and have already added Metabisulfite.* The Gold did not drop well at all. I was wondering how do I go about getting the Metabisulfite out of the gold in solution or visa-versa, that I could not get to drop. I get a positive test on both Platinum and gold in these solutions. And now it is mixed with Metabisulfite and still in solution? I shouldn't have tried to mess with refining at all while I have been sick, that was a big mistake and I would advise anyone to never do that. I thought it was my homemade nitric causing the problem about not dissolving the powders in solution. So I boiled and boiled and added AR and boiled and boiled some more, for days. I was bound and determined to dissolve those powders with AR. I never did get them to dissolve completely and they are still in the bottom of the bowl, still. I had blamed my homemade nitric for all these problems but I think it's been the platinum all along. Hopefully I will be able to get back on this monday to try and sort it out. One thing I have learned from this experience, if you are not really sure what is going into the pot to dissolve, don't put it in there to begin with. If done by accident the way mine was, get a safe (that locks) to keep those pieces in. And not tell the wife the combination. I am in Hoke's again now trying to get this sorted out in my head, but I don't think anything is sticking right now, but I will keep trying. 
Thanks Kadriver,
Oneal


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## butcher

Oneal, 
keep reading Hoke's book, you will never know when the light comes on, sometimes it comes on and we did not even realize when it did, You have really learned alot in a very short time.


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## Oneal58

Hi Butcher, thanks for those words of encouragement. They were surely needed at absolutely the perfect time, appreciate it buddy. 
When things fall into place, as my first half-dozen refines did you get the big head, as I did. This aspired me to move onto bigger goals before I was ready to make that jump. 
This last refine or 2 has put me back in my place and made me realize how little I still know. How much more time I need to spend studying and reading instead of counting my nuggets. 
As we say in the South, these last 2 refines have beat me as you would a Red Headed Step Child. 
Beaten right now, but not broken. I will get this sorted out!
Thanks Butcher,
Oneal


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## Oneal58

Well, I must be losing my mind here? I finally got back out to the old house today and try and get some work done. I had 2 lots of refined gold, one sitting in AR and the other I had tried to cement with Metabisulfite and no drop took place. I have one lot sitting in Metabisulfite and the other solution in AR. I had tested both these lots last week just to see how strong a reaction I got. I even loaded a picture of the postive test on both the Platinum and Gold mix in an earlier post. This was my largest refines so far. I expected at least half an ounce out of these last 2 lots. 
I go back out today and test with stannous again, no results/negative. I made up some new Stannous and tested again, same results, negative? I made up another batch of Stannous while scratching my head and tested the lots again. Both test negative now for gold or either platinum. 
What in the world could this be? What could be causing this? I don't remember reading in Hoke's anything about results such as this. I know for a fact I had gold in these lots and now I get negative test results on both lots? I am going to try and drop the last lot with Ferrous Sulfate, the one that has the redish color tonight. Even though the solution is testing negative for PM's. I know I had PM's in the lots only 4-5 days ago. 
I am at a lose here. Has anyone ever heard of such a thing happening with their refines. I know that the gold is in these solutions but my test tell me it's not there anymore. 
Does anyone know what could have happened to the PM's in these lots. I know that there still in solution. I just get a negative result when I test for PM's. 
Any help would be appreciated.
Oneal58


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## butcher

Oneal,

Lets just stand back and look at this, sometimes when we get up too close we cannot see something right in our face.

Some of the chemical reactions take time, many times we may mix A chemical and B chemical and think we should get a reaction in a few minutes, when actually it can sometimes take time for these reactions to complete (depending on condition) minutes, hours, days, weeks, or more, also sometimes we may not have enough of chemical B or too much of chemical B, this can also change conditions of our reactions,
I have neutralized, chloride metal salts and got fairly close to neutral, expecting to see a clear salt water, only to see a colored solution that would not settle for day's, then I would add just a few drops of HCl, and watch what sit for days, precipitate in just a few minutes.


Do we have gold in solution, our stannous test say's none we can detect, are there powders maybe gold precipitated? Maybe we still have nitric in solution (or oxidizer)? Maybe there is gold and our stannous is not working?

Lets start to try some things.

Take a tiny piece of gold we do not need much at all (memory finger, filings off old gold ring, or chain, could be used), put this in small jar or test tube and dissolve some gold into solution, I would use HCl and bleach, (but aqua regia would also work), we will need heat to evaporate the oxidizer bleach or (nitric) whichever we used (bleach is just easier).

Now we have some gold in solution we can check our stannous with, while we are at it we can use a white spoon or spot plate and add a few drops of this solution to a crystal of ferrous sulfate to see if we get a brown ring in the spoon around the crystal, if these show up the gold, we have proved our test solutions will work.

We can repeat these test with the solutions you are scratching your head over, now is our stannous working? Maybe it works on the test solution from the test tube above, but not the solutions in the little house (your lab) we suspect have gold, but we still think these solutions may have gold in solutions, and we know our stannous chloride is good, lets take a small sample of the solutions we think have gold and put these in a test tube's one tube for each one of our solution's we wish to test, now lets heat these just incase we still have an oxidizer like nitric acid that may be re-dissolving our gold when we try and test them, (here is also where I may use a prill of urea, I know I always say urea is not needed, but that does not mean it can not be useful in a few places), now that we have de-noxed we can try and retest these solutions, lets try both stannous and ferrous sulfate.

If we find gold in solution we can take the liquid from the white spoon that ferrous sulfate crystal precipitated the brown gold out around the crystal, dip a Q-tip into the liquid and test it with our stannous to see if we may have Pt or another reaction to stannous chloride.

If our gold was there It is still there, we just need to find it, if these tests do not show us where it is, we may just have to stand back and look at this again.

It is good to see you feeling good enough to get out some, try and not to over do it, do not stress about the gold, these little gold Ion’s are just sneaky, sometimes they just want to play hide and seek with us, we just have to get the right tools to find them.


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## Oneal58

Hi Butcher, thank you for your post. I will do just what you suggested, spot plate and also test tube test. I am headed back over now to start on it. When I have results I will let you know what they were. More than likely be tomorrow, it will be too late when I finish up tonight to post results. 
I have thought this through many times, step by step, and just can't figure what happened. In my earlier post, the lot that I posted the picture of earlier that showed red mixed in with purple. I added the Ferrous Sulphate, about 2 grams of (fresh) Ferrous Sulphate to drop the gold and leave the Platinum which I strongly believe is mixed in with it. Again, nothing happened, negative drop, negative test with stannous. Take a look at the picture I loaded a few post back. This is the very same solution, same corningware dish, I changed nothing other than wait another 3-4 days. 
The first gold drop attempt on the lot I put the metabisulfite in, I tested it after I attempted to drop the gold. The results on the solution back about 4 days ago was so purple it was almost black. But now I get a negative when I test? 
I haven't been back but just a few minutes. I went to Ace Hardware and bought fresh HCL and fresh Rooto Sulphuric. I had used a few drops of another sulphuric, (different brand) on these last 2 lots but that was the only change I made. The sulphuric is professional brand (pure sulphuric) but it is a dark color, not like the Rooto brand I have been using which is clear in color. But that is the only change I can think of verses the previous 7 refines. 
But, it's just like you said, do the test, back off and see what the results are and what needs to be done to correct it, then proceed. 
One thing I do remember that was different than the others was when solution was being filtered. I had a build up of white powder in the filter paper that I hadn't seen before. I will load a picture of this later. I assumed the very white powder was lead. It came after I added a few drops of the dark sulphuric? It floated to the top of the solution and when poured off to filter turned white in the filter paper. It was not sticky or gel like, more like a paste or regular paint.
Wait a second, I will run out there now and get a picture of the white powder before I start the test. I will post it now. 
The paste was very white like paint, when I folded the filter paper I believe the tin, copper, Etc;. dust covered it. But it was very white, just like dried white paint. But it was the very first time I have seen it before in any of my refines. Picture is below.
Thanks Butcher,
Oneal


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## ryan6342

hi everyone this may not exactly be on topic, first time posting here. if you burn your leftover filters and notice green flames, is that the gold leaving to go play with the atmosphere? or is my gold all still in the bottom of this ash pile?


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## Geo

green flames are normally copper.


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## ryan6342

Geo said:


> green flames are normally copper.


 thanks  whew. 
so would the gold burn away as a color?


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## butcher

copper will give green flames to a fire.

Many metals will color flames, this is one way metals can be identified, with flame tests seeing colors in the fire.

Gold if it is a chloride salt can burn into the chlorine gases formed (I never noticed a color to the fire or smoke but have noticed yellow on surfaces that cooled, and when tin involved noticed it condensed to a violet purple color.

Silver chloride salts are also volatile, and your silver will burn up in the white smoke.

Gold is hard to oxidize, so if it is a metal it will not go up into smoke as far as I know, silver also does not oxidize easily (it will actually absorb quite a bit of oxygen into the melt and can spit it out on cooling.

many base metals can put off vapors of metals in the gases, almost all in our lungs are not good for us, some are especially dangerous, or deadly never breath any fumes of these metals, especially from electronic scrap, not only the metals but there are many toxic chemicals in circuit boards and things like heat sink greases, and materials the components are made from, also many metals we do not normally discuss.

Ore can also be a very dangerous material to incinerate or roast; these rocks contain some dangerous acidic fumes or other toxins like arsenic.


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## Oneal58

Hello Butcher and Everyone, just back on line. Been in hospital for a while, severe (diverticulitis infection). I thought I was a gonner for sure? 
I did get my testing done on my solutions though as Butcher advised. Found that my solutions were barron. Just a little gold in one of them but just a dusting. 
Anyway I had a lot of material left in my reactin vessel that just would not dissolve. By reading here on the site and Hoke's I finally figured out that my gold was still in the reaction vessel locked up with a heavy coating of silver chloride. I really did try and kill 2 birds with one stone and put a silver alloy in with this lot. So there was a lot of silver in this refine. I guess that's why this was my first experience with this problem. 
Anyway, I boiled the material in ammonia hydroxide for a while and low and behold there it was. All my work was revealed to me! This sure has been a learning experience for me and I have learned a ton from this. 
I want to thank all of you for your help. 
Has anyone ever experienced this? Am I right to think that too much silver in the refine caused this? Or did it have to do with the prolonged boilings with nitric that played a part in this? Or did the homemade Nitric play a part as well?
I did my very best to dissolve this material and I am hard headed but I couldn't get it to dissolve. So, I don't know why this happened for sure and would love to know if anyone has the answer? 
One more question, I contacted a Refinner today that said if my gold was .999 he would pay me 99% of spot. He also said if the gold was in Karat form he would pay me 98% of spot? This refining is sure a lot of work for 1% profit to refine it. Is this the going price or is this just because he doesn't know me. I even offered to shot it but he said that wouldn't help the price even if it was .999 pure. He would just put all the shot back together and refine it again to assay it? 
But, I have to remember, most of what I have has came from gold filled, gold plated, rolled gold Etc;. Just wanting to check in with everyone to see if this is the going rate for .999 pure gold?
Thank everyone for their guidance in advance. 
Oneal58


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## nickvc

I'll leave a full answer to Butcher who has been advising you all the way on your material and may I say doing an excellent job, only a fool would ignore his comments in my opinion.
The reason your material didn't dissolve is I fear down to your unexpected illness when you couldn't get back to work quickly or remember what was what. The silver had not digested fully in the nitric so when you put it into AR you got the hard silver chloride covering which prevented the acids working on your gold, go back to the nitric dissolution now you have removed the chloride and finish off that part and you should be good to go.
Terms for gold scrap or refined scrap are pretty good these days so the offers you had do not surprise me but remember much karat scrap isn't plum so an offer of 98% is one I'd take if he will accept the marks as 10 , 14 or 18 karat although I expect the payout will be based on a melt and assay, this is where some doubt can start to creep in as to actual returns...
With your gold filled again I'm sure the only way he will buy is on melt and assay again a grey area and in this case a big one, not all refiners or buyers cheat but many will and do, so unless you melt the material yourself and have an assay done how do you know what exactly your trading...


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## Oneal58

Thanks nickvc, 
I completely understand. Years ago I was selling to a refiner. I would test each one of my pieces of karat gold and knew what I had. When the check came it would not be what I had figured it should be? This happened time after time after time. I am not accusing, I know their are honest refiners out there who wouldn't be able to sleep at night if they did anyone wrong. But I can also see the reasoning why a refiner would prefer the karat gold in raw form and refining it himself. Look at the countless thousands of people who send in their gold in not having a clue as to what they have to begin with. It would take a refiner who was saved, sanctified and filled with the Holy Ghost not to be tempted to stump their toe every now and then. And then it would tempt the best of us not to watch the filtering real close, Etc.
So, I am like you, I would rather refine it, knowing what it weighs exactly, and also what karat I am near. I can say then, hey, I know better. I have told the refiner not to melt my gold, just to drill them if he has to assay the gold. 
It just doesn't make sense to pay $1 more spot price for refined pure gold than raw karat gold. Look at the time and expenses, labor, acids, utilities, and all the other overhead, The list goes on and on that's involved to refine the karat gold. So, you have to ask the question, WHY? I am open here for someone to give me their opinions on this. Maybe it will help me understand better, why this is? 
Thanks nickvc for your post. 
Oneal58


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## Oneal58

Butcher, where are you at Buddy, my friend. I need and would appreciate a little help if you have time.
I came across about 86 grams of karat gold, some 10K some 14K. For some reason I wanted to try a different method of refining than the nitric, inquartration method. I guess because of all the trouble I had on the last refine. 
I used (AR) from the start with my homemade nitric and HCL on the karat gold. I figured the amount of nitric and HCL to use and put the lots on low heat. The karat gold dissolved completely in about 1.5 hours with constant agitation. The 14K dissolving before the 10K did, that surprised me? The solutions came off the burner jet black, I diluted with distilled water and the solutions turned a dark green color. I tested the ph and both lots came in around 2 on my litmus paper. From what I have read I think I need to take this down to less than 1ph? These refines ended up being a large amount of solution. I iced the solutions down good, covered and left overnight. White powder has settled on the bottom of containers. This suppose to be mostly silver if I have read correctly. I know you are not a supporter of UREA to neutralize a solution. So would you drive off the excess nitric from solutions by heating and condensing the solutions down? Then using your method of evaporations, adding several HCL additions, few drops of Sulfuric additions. Also, to drop the gold, the solutions are a deep green color, tells me that it contains copper for sure. Would you use ferrous sulfate or sodium metabisulfite to do my drop since I processed with (AR) this time? 
Butcher, this process has went far too easy and quickly. Would you tell me why this approach isn't used more on karat gold than the nitric/inquartration method? Up until this point and this refine I thought (AR) suppose to have a hard time dissolving karat gold? I am confused now and am waiting on the other shoe to drop on this refine also. On the 14K material, rings, necklaces, pendants, etc:, was dissolved in less than an hour, took longer on the 10K? I thought it would be the other way around? I have read that I could use a little UREA to lower the ph and drop the gold through the green solutions with ferrous sulfate without dragging the copper, lead, etc; down with it? Then that would be the end of it after the use of Harold's making gold pure process. Why not sodium metabisulfite, would that drag down other metals as well in the green solutions? That sounds far too easy and I know there is a reason why not to do this?
I know I am missing something here, but I just can't put my finger on it? Why isn't this supposeably easier quicker method used to process karat gold, I know there are good reasons. I kind of hate to hear them but I need to understand, why? I know you don't use this method for good reasons, that's what has me concerned, what you are going to tell me?
Can you give me a hand old friend?
Oneal


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## jimdoc

Oneal58 said:


> Why isn't this supposeably easier quicker method used to process karat gold, I know there are good reasons. I kind of hate to hear them but I need to understand, why?
> Oneal



Because getting rid of the base metals should be your first step. Now you have everything in your solution to contend with.

Jim


----------



## Oneal58

Hi Jim, thanks for your post. 
I am under the impression that by using ferrous sulphate I can drop the gold through the green solution witout dragging down too much of these other metals? Then by using Harold's making gold pure process get rid of the metals I did drag down? Is this right or wrong? 
Thanks, Oneal


jimdoc said:


> Oneal58 said:
> 
> 
> 
> Why isn't this supposeably easier quicker method used to process karat gold, I know there are good reasons. I kind of hate to hear them but I need to understand, why?
> Oneal
> 
> 
> 
> 
> Because getting rid of the base metals should be your first step. Now you have everything in your solution to contend with.
> 
> Jim
Click to expand...


----------



## jimdoc

jimdoc said:


> Oneal58 said:
> 
> 
> 
> Why isn't this supposeably easier quicker method used to process karat gold, I know there are good reasons. I kind of hate to hear them but I need to understand, why?
> Oneal
> 
> 
> 
> 
> Because getting rid of the base metals should be your first step. Now you have everything in your solution to contend with.
> 
> Jim
Click to expand...



I failed to mention the problems that silver will cause with your new method.

Jim


----------



## goldsilverpro

Oneal58 said:


> Butcher, where are you at Buddy, my friend. I need and would appreciate a little help if you have time.
> I came across about 86 grams of karat gold, some 10K some 14K. For some reason I wanted to try a different method of refining than the nitric, inquartration method. I guess because of all the trouble I had on the last refine.
> I used (AR) from the start with my homemade nitric and HCL on the karat gold. I figured the amount of nitric and HCL to use and put the lots on low heat. The karat gold dissolved completely in about 1.5 hours with constant agitation. The 14K dissolving before the 10K did, that surprised me? The solutions came off the burner jet black, I diluted with distilled water and the solutions turned a dark green color. I tested the ph and both lots came in around 2 on my litmus paper. From what I have read I think I need to take this down to less than 1ph? These refines ended up being a large amount of solution. I iced the solutions down good, covered and left overnight. White powder has settled on the bottom of containers. This suppose to be mostly silver if I have read correctly. I know you are not a supporter of UREA to neutralize a solution. So would you drive off the excess nitric from solutions by heating and condensing the solutions down? Then using your method of evaporations, adding several HCL additions, few drops of Sulfuric additions. Also, to drop the gold, the solutions are a deep green color, tells me that it contains copper for sure. Would you use ferrous sulfate or sodium metabisulfite to do my drop since I processed with (AR) this time?
> Butcher, this process has went far too easy and quickly. Would you tell me why this approach isn't used more on karat gold than the nitric/inquartration method? Up until this point and this refine I thought (AR) suppose to have a hard time dissolving karat gold? I am confused now and am waiting on the other shoe to drop on this refine also. On the 14K material, rings, necklaces, pendants, etc:, was dissolved in less than an hour, took longer on the 10K? I thought it would be the other way around? I have read that I could use a little UREA to lower the ph and drop the gold through the green solutions with ferrous sulfate without dragging the copper, lead, etc; down with it? Then that would be the end of it after the use of Harold's making gold pure process. Why not sodium metabisulfite, would that drag down other metals as well in the green solutions? That sounds far too easy and I know there is a reason why not to do this?
> I know I am missing something here, but I just can't put my finger on it? Why isn't this supposeably easier quicker method used to process karat gold, I know there are good reasons. I kind of hate to hear them but I need to understand, why? I know you don't use this method for good reasons, that's what has me concerned, what you are going to tell me?
> Can you give me a hand old friend?
> Oneal



Most of my life I haven't inquarted unless absolutely necessary. Instead, I dissolved the jewelry directly in aqua regia. Even with keeping it near boiling, it took at least 3 to 4 hours and often longer. From several things you said, it sounds like you didn't have karat gold to start with. It just doesn't go nearly that easily or that fast. One reason people inquart is that direct dissolving. Are you seeing a strong yellow color within the green color? Use a stir rod and drag some solution up along the glass above the solution. If this doesn't appear yellow, you have a problem.


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## Oneal58

Hi goldsilverpro, thank you for your post. 
You are the reason I tried this refine with (AR). I follow your post and spend time on your site and see you use this method. 
Goldsilverpro I tested each and every piece of this karat gold. Unless my chemicals are giving me a false reading each and every piece was either 10K or 14K? I have been testing gold for many years the same way so I am pretty sure that it was karat gold I dissolved. 
I may have mislead you on the condition of the gold before it went into the (AR). I cut each and every piece up into tiny pieces with my lineman's pliers. I also took my anvil and flattened each and every piece of it, so it was very thin. I then cut into even smaller pieces and made bends in the pieces that were big enough so they would not lie flat on the bottom of the vessel. The (AR) tore into these pieces with a vengeance. 
With me standing beside the two heating elements agitating vessels constantly. I guess that's why it only took around 1.5 hours to dissolve the gold. 
I do have the yellow color in the solution, it's just masked by the green color. When the solutions came off the burners it was black, it turned green only when I added distilled water to dilute and cool it. 
Goldsilverpro, I have a couple of thousand $ in these refines so I am nervous and want to be cautious. I am just at the point that I am not sure as whether to use ferrous sulfate or sodium metabisulfite or some other method to drop the gold. 
I see you offer a book on refining. Does your book have this process in it? Since you have been using this process for years any guidance would be appreciated from you here. It seems you are one of a very few that does this process. 
In the meantime if this process is in your book I could purchase it as well. 
I need to finish these refines up the right way. It's just that I don't know what the right way is right now. I have looked for a couple of days on the web and can't find the last steps. I have trouble watching videos with my computer for some reason I haven't figured out yet.
Would you give me the link to the book that has this process in it, it would very much appreciated. 
Thank you for your post and any guidance you could give me from here. 
Thank you, Oneal


Most of my life I haven't inquarted unless absolutely necessary. Instead, I dissolved the jewelry directly in aqua regia. Even with keeping it near boiling, it took at least 3 to 4 hours and often longer. From several things you said, it sounds like you didn't have karat gold to start with. It just doesn't go nearly that easily or that fast. One reason people inquart is that direct dissolving. Are you seeing a strong yellow color within the green color? Use a stir rod and drag some solution up along the glass above the solution. If this doesn't appear yellow, you have a problem.[/quote]


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## goldsilverpro

Oneal,

My book does cover that process.

If you haven't thrown anything away, you still have all the gold and there is always a way to get it - Always! I'll help but I have to first absorb your posts. You write very well but, in the future, please break stuff into more paragraphs with spaces between them. To me, this is very important when you have a lot of details. On one long paragraph and no spaces, my eyes glaze over after about 8 lines. Need some white area.

The way you prepared that stuff, I will agree that 1.5 hours is very possible.


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## Oneal58

Thanks Goldsilverpro, will do. I just get in a hurry sometimes and take my mind off what little communication skills I do have. 

Thank You in advance for any guidance. 
Oneal



goldsilverpro said:


> Oneal,
> 
> I'll help you but I have to first absorb your posts. You write well but, in the future, please break stuff into more paragraphs with spaces between them. To me, this is very important when you have a lot of details. On one long paragraph, my eyes glaze over after about 8 lines.


----------



## Oneal58

Hi Goldsilverpro, 
Believe me when I say I haven't thrown anything away. I have a lot invested in this lot and am being very careful with it. 

I have 2 coffee pots full of green solution sitting in cabinets, covered.

Yes, it took me a couple of days working on and off to prepare the gold for the refine. I did this in the house while watching the news. Drove my wife crazy with all the hammering. Had a big piece of plastic under the chair and in front of where I was working to catch all the pieces that got away from me from time to time. I spent a lot of time on my knees also. 

I will get the book you offer on this process. 

Thanks Goldsilverpro for your post and help with this. 

Goldsilverpro, is the book the item that is offered on the GoldRecovery.US site/Lazersteve's in the Store? When I type in Goldsilverpro Book I end up there. I see the item being offered but am not sure if this is the book that has the process in it? The one offered on this site says it's the *Gold Silverpro's Official Refining Guide*. I have also read on the forum that there's a Ebook you offer. Which one of these has the process of (AR) refining of karat gold in it we are talking about? 

Thanks Goldsilverpro, Oneal



goldsilverpro said:


> Oneal,
> 
> My book does cover that process.
> 
> If you haven't thrown anything away, you still have all the gold and there is always a way to get it - Always! I'll help but I have to first absorb your posts. You write very well but, in the future, please break stuff into more paragraphs with spaces between them. To me, this is very important when you have a lot of details. On one long paragraph and no spaces, my eyes glaze over after about 8 lines. Need some white area.
> 
> The way you prepared that stuff, I will agree that 1.5 hours is very possible.


----------



## goldsilverpro

It's item #30 on Steve's site, goldrecovery.us


----------



## Oneal58

Hi Chris,
I just paid for the item. What happens next? Please take note that this Paypal account I used is in my wifes name. If you need the email address or any other personal information just send me a PM and I will respond. 
Thanks, Oneal


----------



## butcher

Oneal. glad to see you back up and busy,and felling better.

I have Gold Silver Pro's book, it has an awful lot of good information in it, you should like it too.

I have been kind of busy lately.

I think many of us will learn, as GSP helps you with this lot.


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## Oneal58

Hi Butcher, it's really good to hear from you. I am glad to be up and around again and really thankful that I am still here. Butcher, It's 4:30 a.m. here and I am running on empty. But I just could not go to bed without saying It's really good to hear from you old buddy. I am not vearing off course here Butcher with this refine, I just think I need to try each and every one of the methods. I feel I will gain experience with each and every different one. I want to try the HCL/Cl and the AP Process next. I just feel I will be more rounded as a refinner if I have a somewhat limited knowledge on each method.
Call me crazy or just thick, but for some reason I seem to want to know how each different refining method works. 
Well I got to call it for tonight, so good night Butcher, my friend. 
Oneal


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## Oneal58

Hi Goldsilverpro, 
I received your PDF Book. I have read some of the material pretaining to the (AR) Refine. I have read in the book that you used Nitric first to dissolve the base metals before you put the karat gold into the (AR). 

I have probably goofed here because I put the Karat Gold straight into the (AR), no pre-treatment at all, just put the karat gold straight into the AR. Left in the (AR) untill all the gold had dissolved. 

I didn't see in either books where you used the (AR) method without any pre-treatment?

I also have probably got excess Nitric in with the gold bearing green solution. 

This is where I am at, 2 coffee pots full of the green solution with everything in it that was in the 10K and 14K gold. Other than what droped out of solution when I diluted and iced the solution down. 

I guess what I am asking is where do I go from here. I misunderstood you to begin with. I didn't think you used a pre-Nitric Treatment of the Karat Gold?

I am really pleased with the information in the book, it's going to take me a while to absorb all the information that's in it.
*From what I can gather my options are as follows.* *Any help here would be appreciated here. *

1-Filter all solutions to remove silver and etc;, combine solutions. 

2-Raise Ph with Urea dissolved in hot water then add to solution until foaming stops. When Urea is added bringing ph to at least 1.0.

3-Dissolve sodium metabisulfite in hot water and add slowly. With 2.5 ounces of gold expected I would use 2.5-3.0 ounces of metabisulfite. 

4-When gold starts to drop, keep testing solution with stannous until solution test barron for gold. 

5- Leave overnight at least for small gold particles to settle completely.

6-Pour off top portion of solution, filtering only the gold bearning last portion of solution. 

7-Use Harold's *Making Gold Pure Process* to clean up the gold before melting. 

This is what I have gathered so far. I am off base anywhere here please advise, it would be appreciated. 

Thank you Goldsilverpro for any guidance. Oneal


----------



## Oneal58

Hi Goldsilverpro,
After the gold drop would I process the powder with nitric and then use the Making Gold Pure Process. 
Thanks in advance for any guidance. 
Oneal


----------



## Harold_V

Oneal58 said:


> Hi Goldsilverpro,
> After the gold drop would I process the powder with nitric and then use the Making Gold Pure Process.
> Thanks in advance for any guidance.
> Oneal


Once you have precipitated gold from a chloride solution, the use of nitric acid is not suggested. Unless you heat the gold to the point of eliminating all of the chlorides, you risk dissolving some of the gold when you add nitric, and that's even after rinsing the gold several times. It's nearly impossible to remove all of the acid, as you'll discover when you melt your gold. Fumes come off upon heating, even if you've dried the gold well. That's the nature of the beast. 

That's not to say that washing with nitric can't be beneficial. It can be, but you're asking for unneeded complications when doing so. Stick to the HCl and ammonium hydroxide washes I discuss in the thread you mentioned. It works, and very well, and eliminates any worries of losing values from dissolution. 

Harold


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## Oneal58

Thank You Harold for your post. 
I am remaining in a holding pattern on this refine until I hear from Goldsilverpro. He had mentioned he would help me through this but he must have got tied up somehow. I hesitate to do anything with it (the solutions) fearing I could do something wrong.
As you just pointed out, losing values if I went with a Nitric treatment when it's not necessary. That's good important information to know. I sure wouldn't want to lose any values on this refine, I didn't find (buy) this karat lot at an auction as I did my gold filled, plated, rolled, Etc;, that I have been refining. So it will hit my pocket book pretty hard if I mess this refine up. 
So, I will just sit tight on this refine and read Goldsilverpro's Books he sent while waiting to hear from him. There's a lot of information in those books to digest. 
I (kind of) know what to do Harold, but just like the Nitric treatment, if I hadn't of asked and you answered I would have lost values. So, kind of knowing, just isn't good enough. 
That's why this site is so important, well the members are so important. I would have made a mess more times than I have if it hadn't of been for Butcher, you and others. It seemed everytime I didn't ask someone to hold my hand through a process, I would goof it up. 
I must say though, Butcher has held my hand through most all of this from the beginning. It was the times that I didn't want to bother him is the times I made a mess of things. He has spent so much time with me, I feel guilty sometimes asking him for help. I must make myself understand that the member's are here to help newbie's like myself. Or they would not offer the help. I am just not familiar with getting something for nothing, as a gift, and have a hard time with asking someone for help. I don't know why, it's just the way I am? 
I have been trying my hand at refining since the last of Nov., I think. I know I have a long, long way to go. If I can keep my old body up and going, hopefully in a year or two I will not have to bug anyone, as much. Then finally be able to start to return some of what I have been given. Hopefully to be able to maybe answer a question for someone like myself, with confidence. 
Thank you Harold for the information and taking time to post, I appreciate it. 
Oneal


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## Oneal58

Hi Butcher, I guess GSP has got tied up somewhere. 
While I am waiting I have a couple of questions I hope you can help me with.

I have accumulated maybe 45-50 gallons of spent Nitic soution sitting around. Some of this solution is when I first started as you know. I am sure I have some gold in there, silver that I couldn't get to drop and other things as well. When I first started I did make a mess of things for a while. The Spent Nitric looks to be starting to rust? Has a yellowish rusty sludge on the bottom of the drum? I can scrap down to the bottom and bring up the yellow looking material that looks sort of rusty? 

I was wondering what's the best way to go about recovering these metals in the Spent Nitric Solution. I have read that I can take angle Iron and put into the spent Nitric, but it acts like bird shot though and gets everything?

How would you go about getting the metals from this spent Nitric solution? I have no way of distiling a container this large and the only way I could do this is take maybe 1/2 gallon out at a time and distil down. That would take forever though.

I have all my HCL and Sulphuric as well saved. I thought I would just distill these 2 back down and reuse them. I have metals in the bottom of the HCL and Sulphuric. The metals in the HCL looks like silver but I am sure there are other metals in there as well.

In the sulphuric there is some gold that has settled out from the time I was running the sulphuric cell. I am going to try and get this gold and I thought I would just distill the sulphuric back down and reuse it as well. 

I don't have nearly as much HCL and Sulphuric as I do the Nitric Solution.

* I know you are the pro when it comes to recycling solutions* 
I would appreciate any directions and pointers you could give me Butcher to get these metals back out of these solutions. I know I have went through pounds and pounds of copper when I first began. Using way too much Nitric to begin with. All that copper is locked up in the Nitric solutions. I believe I have some gold in them as well. Well I know I have some gold in them from mistakes that I made at the beginning. 

I don't want the solutions to get any farther ahead of me and would like to get the ones I can resue back to usable condition and dispose of the ones that I can't recycle but recover the metals first. 

I forgot to mention all the sodium metabisulfite and ferrous sulphate solutions I have saved after my gold drops also?
Thank you Butcher for any help you could give me on this.

I realize this is a huge question but I would really appreciate your help on this if you have time. 
Thank you so much Butcher,
Oneal


----------



## butcher

Oneal, there are several ways to recycle your waste, much depends on how you collect the waste, if you have kept the nitric acid waste separate from chlorides, it would not have chloride involved, if you added chlorides then that should be considered if reusing the waste.

The 50 gallons of nitric is a large volume to have around, my guess is it is a dilute solution, the mud in the bottom of the storage vessel has a high potential of being valuable, leave this mud undisturbed.

What I am saying here next you will have to determine if the solution had added chlorides, and if so and solutions you get from this later should be tested for gold or other values.

One way is reuse this dilute solution concentrating it (for less waste to have to treat), and get some work done with it at same time.

Decant the solution and add to crock pot, add gold plated pins or other materials you wish to remove base metals (if the contain copper it will work, and will work better is base metals are above copper in the series of metals), put crock pot on low heat, this will concentrate solution and dissolve some base metals as the solution concentrates, cover pot, to keep out, rain and snow and dirt, also keep out of reach of children or pets, this is done outside as it will fume off some gases but mainly water at first, let this evaporate, and depending if the nitric had free nitric acid can determine how far you can let this evaporate (if too high of nitric acid content on evaporation it is possible for a boil-over if excess acid and greater than 68% concentration, and heat is too high), with low heat and not letting concentrate too far you should not have trouble with boil-over from the solution, every day check on it add some more of the used nitric as it evaporates off, let this dissolve the base metals, (if powder form let them, but after they build up you remove powders to a selling jar, also when solution gets very concentrated move it to this settling jar, (this could be a gallon jar, that after letting settle the concentrated solution from this selling jar decanted to 5gallon pail), when you get to the bottom of the 55 gallon drum you can add your powders to the settling jar, now you have 5 gallons of concentrated copper nitrate solution and some copper powder that can have values, these powders can be cleaned up with fresh acids, and the 5gallons of concentrated solution still has use, (you could use it as an electrolyte, or crystallize to salts and get some nitric from it or just cement the copper and other metals with iron and treat it for waste).

Chloride solutions you can treat similar, but also if you added a chemical or reagent to them like SMB or sodium sulfite or like ferrous sulfate the can form sulfate salts when concentrating, as the HCl fumes from these either make metal chloride salts or vaporize off in the evaporation process. So if your chloride solution does not contain sulfate’s you can use it like copper II chloride, or you can use it to dissolve copper in heated crock pot letting it get very thick and dissolving copper to powders, these powders again settled to be cleaned up later, this lowers the volume of waste to treat (concentrating it), and gets some use out of it at the same time, 

now these copper powders with some gold or gold flakes can be used in a new stock pot, as you refine add you solutions to them it will clean these powders up this way you do not have to waste new acids to clean them up, and the solution if values involved will replace the copper (or other base metal from these powders), your now solutions will be more concentrated as the pick up as much metal as they can from these powders……


As far as sulfates solutions these are still useful, even if they have some chlorides, as they can also dissolve base metals, and as they concentrate with metals, the HCl can be driven from them (as chloride metal salts, or fumes), and as you go you can remove the chloride salts, and eventually you will end up with sulfate metals salts, ferrous sulfate can be made this way or copper sulfate, again useful items in refining.

Some principles need to be understood doing this, like what the salts look like, so you have an idea as to which ones your making, these salts can also be re-crystallized for higher purity, also understanding what gases and acids leave the solutions first and which ones may not leave the solution is also important, also what temperatures or conditions these leave your solutions, or form metal salts.

Water is more volatile than nitric so it leaves first, then nitric, then chlorides, and sulfates will not leave unless temperature is extremely hot and salts are roasted,

So from this you can see if you had a mixture of all of these the end product would be a sulfate salt. (But the solution could be making salts of other metals as it was evaporating from this soup).

I will stop here as this is getting long and it gives you plenty to consider for now.
Hope I wrote this where it is understandable.


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## Oneal58

Hi Butcher, thank you for your post. I really appreciate it!
Butcher I have to admit that the Nitric soutions contain chlorides. At first I put some of my HCL in by mistake. I also have been making my home made Nitric from Potassium Nitrates and the solution contains a lot of sodium metabisulfie, and a little ferrous sulfate. Also, when I would open the container to decant into it I would get a rise of Nitric Brown fumes so I added Urea untill this stop happening, I added a lot of Urea, I just got tired of smelling it. 
To be completely honest with you, at first I put a little of everything in there. I also played around with the Ammonia Nitrate once and I have read that this will form Chlorides when exposed to certain metals as HCL does? So, I have a buffet of chemicals that to be honest with you I would love to get to a point of just getting it out the building where I am working. 
Do you think I will be OK to distil this solution down with all these chemicals in it, safely? Surely some where that the children, our pets or unsuspecting people would not be for sure. 
From what I am reading of your post I can expect a lot of salts from this distilled solution.
* So, where do I start?* 
Do I just get a crock pot and starting distilling and when the salts form let you know the color and crystal form and have you direct me from there. I sure don't know how to recognize the different salts yet. 
I had a large heavy piece of what I thought was 900 parts silver. I thought that Nitric would dissolve this silver (at first) when I started refining and put it into a jar and added 70% Nitric with just a little water to get reaction started. I put this on the back porch of the house and forgot about it. I opened it up the other day thinking I would try and recover the silver which was maybe 240 grams. To my surpirse there are beautiful blue salts crystal all in the bottom of the container the silver was in. Formed around a little of the metal that didn't dissolve. Most, if not all the silver is gone, the metal that the crystals are growing on looks more like tin or zinc than silver. These salt crystals remind me of the Ferrous Sulfate I have, looks just like them?
So, do I get started by starting up the crock pot and just keep you informed of my progress and the new situations that arise as I take on this project?
I know this is going to be a long drawn out project, but it has to be done for the experience of it as well as keeping the chemicals out of the enviorment. I sure would not dump them on this farm or any place else, I love my deer, coons, rabbits, Etc;, too much to do that to them. 
Thanks so much Butcher.
Oneal


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## butcher

Oneal, 
First thing to do is to read 4Metals post on dealing with waste, in the safety section, use his advice.

In your case of the soup, I would not try and reuse solution, in this case I would hang a piece of clean copper into the barrel, leave it there until it no longer reacts, you can brush it into a jar if it forms a black crust, and re-hang it inside solution, this will cement anything lower in reactivity series than copper (valuable metals) if the solution is at least slightly acidic (If the copper does not react check pH and make solution slightly acidic with some H2SO4 or other acid), or if it is too acidic already and the copper dissolves then hang in another piece of copper, until no more copper dissolves and when reaction is complete some copper bar is left, I would start with not too large a piece of cut and flattened out a copper pipe. Punch a hole to wire a solid copper wire to hang it with,(what I would try is a copper that might fit in a quart jar say a 1 1/2" copper pipe 6" long, so that if it does not dissolve you can use it for other cementing jobs, cut it length wise, large tin snips or hack saw, and unroll pipe and flatten it out, sand it off clean), hang in barrel, once all of the copper has cemented all it will (if it will), 

Then decant solution to another barrel, do not disturb settled powders (very likely valuable metals) save the powders in jar for processing later, mark jar as to contents.

The solution you can then hang in a piece of steel.

Or a faster method is a piece of steel for an anode (+), an old piece of flat computer case steel no paint. 

And a piece of non-magnetic stainless steel, for a cathode, I would also do this in 5 gallon bucket.
Large pieces of metals to fit bucket and give large flat surface area.

Take a battery charger I would use the 6volt scale. And an old truck 12volt head light, then wire this bulb in series with the 5gallon electrolytic sell.

Red positive of battery charger (+) to ------wire-----to light bulb one terminal of =(“O”)= other terminal of light bulb-------wire----to anode of cell (steel).

Then the black negative of terminal of the battery charger, wire it to the cathode (stainless steel plate).

The light will limit the current and also gases formed, it will also give an indication of the operation of the cell, (it gives me light when working at night), and it will drop some voltage to the cell, now the cell will change resistance as conditions change, this can be seen by how bright the lamp is, this light bulb also protects your power supply (battery charge) if the two plates or the cell shorts out (the light just gets bright).

Hang the two pieces of metal in bucket, up off of the bottom as copper powder that will fall to bottom of bucket would otherwise short them out, keep the anode and cathode from touching (on opposite sides inside of the bucket), the steel (iron will dissolve into solution, and the copper will plate as a mossy copper powder onto stainless steel (some copper will fluff off into bottom of bucket), 

This copper can be scrapped of the stainless into a pail I would keep the copper powder covered with a some-what acidic solution so copper does not oxidize in the air).

When all of the copper has been removed from solution, remove plates and turn off charger, let the bucket settle and decant solution to another five gallon bucket, put the copper powders in the jar with other copper powders mark this jar copper.

This Iron solution needs to be brought up (slowly) to about 9 pH, you can use sodium hydroxide (drain cleaner, or sodium carbonate (soda ash) automatic dishwashing soap, or screened hard wood stove ashes, or even baking soda, or garden lime, bringing up the will precipitate most all of the metals (too high of a pH will start to dissolve some of them back into solution), when solution gets closer to the right it will start to look clear (salt water), after powders settle well, sometimes I use Epsom salts to finish clearing the solution (you want clear salt water to dispose of, some time I may need to adjust ph with acid, or more caustic base) after powders settle decant clear solution to jugs for disposal (if you have a septic do not put it there as too much salt can kill your septic tanks bacteria), 

The metal powders need to be dried well, flat trays in the sun, some lime and cat liter can help some, once dry the powder oxides can be disposed of.

Please read 4Metals post, as I worked all day and this late at night I most likely left out some important detail.

Have a good night
ole friend take care.

Oh yea the blue crystals could be copper sulfate.


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## Oneal58

Hi Butcher, thank you so much for your post. 
Believe it or not I understand each and every part of your instructions? No problems that I can see right now to get this done. I will need to start on this next week though.
I have an Uncle who I am very close to, the only Uncle I really ever got close to who treated me like a nephew. He is failing fast (Lung Cancer), his wife called and said if I wanted to see him again I need to hurry up there. He Lives in Johnson City, Tn. I leave tomorrow morning to go up to his place. He is not doing well at all and Aunt Cathy has called the family in to him. 
I have been really busy the last couple of days trying to get lined up to leave. I think I will be staying through Monday, unless something comes up unexpected. 
Butcher I wanted to touch base with you before I left. It will probably be Tuesday before you hear from me again. I just want to say thank you Butcher for all your help and always being there for me. 
I went ahead with the refine that I was holding off until I heard from GSP. I have a couple of questions on this refine but they will wait until I get back from Tn. I am hoping that GSP is OK. I don't know why I haven't heard from him? 
But I studied and read all I could find on the process and went ahead with it. I ended up with nearly 4 grams missing/disappearing. The sodium metabisulfite I used to drop with tested negative with stannous. I know that the stannous is good because I have a test solution of gold I use to verify it each time. I have double checked my figures and they are right, but 4 grams of the gold went somewhere? I figured up what I should have had before the refine and tested each piece and the Karat's on each and every piece? What I should have had and what I ended up with was 4 grams short. I still haven't figured out what happened, I don't think I ever will? 
But I got to get some work finished up over at the old house tonight. 
Thank you again Butcher, I will get in touch with you when I get back from Tn.. It's about a 6 hour drive from here so I plan to leave around 9:00 a.m. and take my time going. Just want to miss that Charlotte, N.C. traffic from around 4:00 through about 6:30. Hit it wrong and it has taken me 1-1/2 hours before just to get across Charlotte. 
But anyway, I will see and talk to you when I get back. 
Thank you my friend,
Oneal


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## butcher

Oneal, take care on the road


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## Oneal58

Hi Butcher, Everyone. 
I have finally made it back home, again! I got home the first time and found out I had left my firearm I carry with me while I am on the road. My Uncle advised me to carry it anyway, he said something about someone who was killing people with an ax or something in Tn.
But to make a long story short I ended up having to make the trip again to retrieve my weapon. When I got to Tn. the second time, I ended up with a stomach virus that had me in the bathroom every few minutes so I had to wait until my stomach settled before I could get back on the road to come home. 
But anyway, I am going to start on the recovery and processing of my waste solutions next week Butcher. I am sure I will have plenty of questions. I just wanted to give you a heads up and say Hey. 
It sure is good to be sleeping in my bed again. 
Talk to you next week Butcher, I hope you and family have been doing well. 
Oneal


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## butcher

Glad your trip was safe, family is doing good, I guess I am going to have to study up on Hoke's book, as I bet you have alot of ideas saved up to discuss.


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## Oneal58

Hi Butcher old Buddy. 
Sorry to keep you hanging so long but a new developement came up and I have been very busy with that. I had to put the solution recovery we discussed on hold for a while to try and make a few dollars. 
But to make a long story short, I had a person who collected only gold plated items for years and wanted me to recover the gold from the gold plated for him. He had some high quality gold plated and I expected good returns form the cell. 
It was quiet a large lot and I have been working on it since I got back from the trips to Tn. 
I used the sulphuric celll to strip all the gold plated and was really impressed with the amount of powder I ended up with. Shorted the cell out one time and had to make another run on the plated items. Put everything together and I rinsed the powder many times in hot water boils/settle and decanted untill decant was clear. 
I then decided to use the Hydrochloric/Chlorox method to recover the values. This part of the process went perfectly resulting in a deep beautiful yellow liquid that I was really impressed with. I was only left with some white soluable salt in the bottom of the container. I let the solution set up open for a couple of days for the chlorox to precipitate out so I would have no trouble with it. 
I then added my sodium metabisulfite and watched as the solution turned a clean color indicating to me that I would soon be seeing the brown gold swirrling around next in the containter. I added another bit of sodium metabisulfite and nothing happened, added a little more nothing happened. 
Getting concerning I pulled a small amount of solution out of the main container and added a good bit of sodium metabisulfite, nothing happened? No gold drop. 
I am stuck here, I have a container which I know is full of gold (tested positive/fresh stannous) but cannot get it to drop with SMB. 
Butcher, do you have any ideas on what has happened to this refine? I just bought this container of Stump Out the other day so I feel it is fresh. 
Thank you Butcher for any help you could give me on this. The gentleman is comming around nearly every other day wanting to know how it's going with the gold filled. I am really worried about this now and I don't know what in the world I am going to tell him next? The truth is what I must tell him but he isn't going to like that, neither would I!
Thank You Butcher for any advice you could give me. Oneal


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## Oz

I’m not Butcher, but it seems you need help yesterday. Since you tested with stannous and you know the gold is there but not precipitating when you add SMB, I would guess that you still have free Cl gas in your solution. Take a couple hundred mL sample of your gold solution that you have added SMB to and put it on a hot plate taking it up close to a boil but not quite. You should see gold start coming out of solution.


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## Palladium

He mentioned some salts from the hcl Clorox process which might mean he has not diluted it enough also. After you heat it if you see any more salts which you probably will try diluting with water before you drop and see if that helps.


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## Oneal58

Thanks OZ, Palladium. 
I did as advised, I found that even after 2 days of sitting open, I still had some chlorine in solution, thank goodness. 
I added another 1/3 of distilled water to the main batch. I then put the vessel on low heat on the stove. Just enough I could see a little steam rising from solution. I left solution on the stove until the extra water I added was evaporated away. I started getting worried again but decided to let the vessel stay on heat a while longer. 
It didn't happen all at once but I started to see fine particles of gold accumulating on the bottom of the vessel. I would stir the solution and the little pile of fine gold in the center/bottom of the vessel would get bigger and bigger. 
As time went on I ended up with a complete and successful drop with solution testing negative. 
Thank you so much for your help, I feel much better now and a lot of worry is off of me. Thank goodness I didn't have to explain to the gentleman what had happened. He hasn't came around for the last few days but I expect him today. I have left the drop in the vessel to show him before I finish with the refine. 
It sure takes a lot of plated items to make any kind of show, I hope he will be happy with his returns. 
Thank you all again. 
Oneal


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## butcher

Oneal, explain to him how gold always looks like more than is actually there, if you melted the powders in front of him he could see the gold shrink into a button.

I am glad your back out and refining, I seen your post but you already had some great guy's helping with your question, so I did not chime in.

Are we going to get to see a picture of the melted gold?


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## Oneal58

Hi Butcher, it's good to hear from you old Buddy. 
Butcher, I wanted the gentleman there during the melt, just as you advised. It is very important to me not to have anyone think I would ever take from them. I know how easily it is for someone to become suspicious of a gold refiner when returns aren't what they expect them to be? 
And of course, as I expected, he was disappointed. *I have made a decision that I will never, ever refine gold plated again, ever, for someone other than myself.* I honestly believe the man walked away thinking I had in some way stolen from him. Something I would never do to anyone. I blame myself partly because I didn't warn him or fully explain to him how little gold is on gold plated items. His expectations were high and returns were low. So he was very disappointed, as I was also, for him. 
From now on it's just Karat Gold Refining for anyone who wants me to refine for them. The variables are just too complex to give someone a correct estimate on what returns will be on gold plated items. I know I could get close but it would just take too much time to get the estimate close. I even considered adding some of my own gold to his just so he would be satisfied and not suspicious of me having done something shady.
I can test, then estimate what returns should be on karat gold. Getting pretty close on what returns should be most times, if I don't mess up somewhere.
But I have to ask myself, do I want to even refine for the public. With my personality, I think I would lose too much sleep over it. I would probably end up working for nothing, as I did in this case. Not even considering the cost to me for chemicals, electricity, Etc;. 
I can understand this gentleman's feelings. He had been collecting these gold plated items for many years. He had developed a mind set that he really thought he had something of great value there over the years. I picked up on his feelings he had become attached to the material. But it was too late to back out of the refine by the time I felt I was in trouble with him, or his expectations.
I worry about what he may be saying within the community about this experience. 
But I know I did everything I possibly could to get the best returns for him I possibly could. I can rest and feel good about that. But it also worries me that after I seen how disappointed he was with the returns that he may be saying something negative about the experience to others? 
Oh well, nothing I can do about that now. I did the best I could for him. Hopefully, I will stop worrying about this eventually. 
Butcher, I have been really busy on other things for the last week or so. As soon as I can get to the stored up chemicals project I will get with you seeking your help. 
Thanks Butcher, as always your insight and advice is spot on. It is always appreciated and respected. 
Thank You, 
Oneal
Oh, almost forgot to post a picture of the button that has caused all the worrying. I am pretty sure I did get close to at least .99 on this one, maybe a little better. It pulled a deep pipe and has the right color. I have had pretty good results with the sulphuric cell buttons turning out good, (Knock on Wood!).Worried about changing my luck, NOT ME???
But I have only ran a few with the cell. And this one will more than likely be the last one for a while? But I was impressed with the HCL/CL method I used on this one. But for the hickup with the left over CL I had on this one.


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## butcher

O’Neal, that is beautiful, a job well done, I would not worry much, you were honest, You know it, and he has pure gold in his hand, he probably would have had a hard time finding any one to sell the raw material to who would give him as much as you have given him, he just does not know how lucky he is,
Also if he Honestly understood how much trouble you went through to refine this for him he would probably not be able to pay you for all of it with that pretty button of gold, you have learned a lot, and that experience is worth more than that yellow metal.

O’Neal it has been a pleasure to help you with a few questions, and I feel I have gained a good friend while doing it.

Congratulations on a very fine job.


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## Oneal58

Butcher,
I am proud to call you my friend. My friend Butcher, even though I have never meet you face to face. I feel I know you better than if I would have lived next door to you most my life. 
Butcher without you, that little button of gold, which has caused me so much worry. But at the same time has put a sense of pride and self worth back in my life again. All would have been impossible without you holding my hand and showing me the way, from the very first here on the Forum. 
And let me just say this, when you say you have just helped/answered just a few questions for me? With that way of thinking I sure wish you owed me just a few dollars. I would be the richest man in town :lol: 
Of course we don't know each other's stories or where someone is at during a particular point in their walk through this life. 
It would take a Novel to explain to you what my story is. And maybe the same for you? But try to understand this, with me, it has never been truely just about the Gold Buttons. The reasons for this endeavor run much, much, deeper than the gold buttons. I am sure you understand what I am trying to say. 
But, I am just getting back in the house for tonight. I am getting too old to be doing this night owl stuff again this late in life. That's what the wife says anyway, and as you have always said, the wife always knows best. :shock: 
Thank you my friend and good night.
Your Friend,
Oneal


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## Oneal58

Butcher, hope you are doing well today. 
I have a question for you, hoping you can help me with. Of course I keep testing solutions on hand up to 22K Gold testing solutions and also Platinum testing solutions. I make my own solutions now but I would like to be able to tell what Karat Gold I have using the density measurement test. That's the only way I see right now for me to be able to see if I can determine if I have 24K without having a piece assayed. I have read up a little on Fire Assaying but only having a piece or 2 of Platinum now and then I need to spend most my time reading and studying the main subject, which of course is gold recovery right now. 
I would need to purchase a set of (Ohaus Cent-O-Gram scales) which would set me back over $100 to do the density test correctly. I have studied the density process and understand it but I was wondering if the investment in the scales is worth it, or not? Will using these scales for the density test tell you if you have 24K gold that's reliable, if test is done correctly? I guess what I am asking is how accurate is the density test? Or is the only ture way to determine if you have 24K is to have the piece assayed? Is there another way to check density without having to have the Ohaus scales? 
I have a couple of sets of small scales but only the smallest set that can be used for legal trade. This set will only test up to 20 grams. Plus they are not designed for use around water. I guess I could rig up a reverse weight measurement system (not knowing the correct name for the method) a (Jury Rig) and use the precision scales to weigh the piece while it's underwater. Or Is there another way of testing to see if your gold is 24K without sending it out to be assayed?
Oh, I have one more question Butcher. I have another ring that looks like Platinum. I have done a Platinum test with Platinum solution which the large ring passes. I also put the ring into pure Nitric and then into cold Aqua Regia for a couple of hours. Neither of these solutions had any effect on the ring, none. I didn't want to heat the AR due to the outside chance I could mess it (Ring) up if it turned out to be 800 parts platinum. 
I never did invest in a little pure platinum to make that testing solution, I didn't think I would be messing with Pt. so I didn't buy the pure pt. samples needed. 
I guess I could file enough filings off the ring to make a testing solution but I hate to do that. Also, if the ring turns out to be something else I would be wasting my time. What process do you use to test for Pt. without having it dissolved in solution? And, if you don't have any pure platinum on hand. Is there another process that I can use? Or I just need to order the Pure Platinum samples to make the testing solution?
Butcher, I read that I can submerge the ring in hydrogen peroxide and if I get hydrogen bubbles released it is Platinum.
I went ahead and did this test, the ring did bubble in the Hydrogen Peroxide. 
After all this I found a name on the Ring, I googled it and believe there's a possibility that it could be a metal that a manufacturer is calling Saladium? Says it has a lot of properties similar to stainless steel. Do you know if Stainless would bubble in Hydrogen Peroxide? I do know stainless will not dissolve on a scratch stone with 22K gold testing solution or Platinum testing solution. Just don't know if it will bubble in Hydrogen Peroxide or not?
So, I am stuck I guess, I guess what I will have to do is just put the item up or order the sample pieces of platinum? That is if (Saladium) test positive as Platinum would in the test I preformed on it? 
Thanks so much Butcher for your time and help. 
Oneal


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## nickvc

Try the ring in hot hydrochloric if it possesses the same or similar metals to stainless it should start to dissolve which platinum certainly will not.
Gold is never totally pure and in my opinion the only test is an assay but they do it in reverse for high purity metals, they look for impurities and deduct those from the result I believe.


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## goldsilverpro

Are you sure it isn't spelled Siladium? That's a stainless alloy used for cheap class rings. The specific gravity of that would be around 7.9.

http://www.google.com/search?q=siladium+alloy&ie=utf-8&oe=utf-8&aq=t&rls=org.mozilla:en-USfficial&client=firefox-a


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## Lobby

I just read this entire thread this morning. What a fascinating read.

As someone who's soon to process some GF jewelry, it's been quite enlightening.

Thanks to all who've posted.


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## butcher

Oneal, 
I really could not help with this question's, I am sure glad we have more knowledgeable professionals here who can help us.

I have never heard of siladium (stainless steel), besides the hot HCl Nickvc suggested, and the specific gravity test GSP suggested, I remember Irons and Lou talking about using a torch (if I remember correctly), PGM alloy's glow white hot in a reducing flame, other (white) metals oxidize in flame turning colors.

I also believe the specific gravity test would give an idea of the materials involved, but would be very inaccurate to tell how pure the gold button is, too many variables for that fine of a weight difference to be measured, a tiny air bubble, dust particles when gold measured in air, slight difference in temperature, type of setup apparatus, scale being able to measure such an extremely minute amount of difference in weight, (even the most expensive lab scales may have a hard time trying to tell impurity in the atoms of gold), and so on make this an impossible task to tell impurity in the atoms of gold that make up the button.

The pipe in your gold is a good indication of its purity.

I feel (but do not know) even an assay could not tell how many atoms of other metals are involved in contaminating the gold atoms, but give a general Idea of its purity.
I do not know but also believe even an assay can also be fairly inaccurate at telling the exact purity of the gold (but can give a good indication, and is a very good method), as it seems to me there can also be many variables in performing the assay, if we are thinking atoms of contamination of the pure gold.

Nick you mentioned you think they done the assay in reverse, for high purity gold, it would be interesting to learn more about that process.


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## nickvc

Butcher if I remember correctly it was in a post by one of our pros GSP, Lou or 4metals who described the process, I can't remember the details but I'm sure one of them can give details if my memory is correct, i'm far from an expert on assaying techniques I'm afraid but I think once a certain point in fineness is reached it becomes inaccurate after that point. My apologies if my memory is incorrect on this


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## Oneal58

Thanks Everyone for your time and your post, they are all appreciated. 
I guess the best thing to do is learn enough about refining and do enough refines so you will know when you have 24K. 
Then let the pro's who only assay worry about the fineness of the metal when and if they need to. Just do the very best job you possibly can on a refine and if it doesn't turn out right, do it again. Thanks everyone. 
Butcher, I will try the white hot glow heat test, just to see what happens. I am suspicious now it's Siladium since reading the information on Google that Goldsilverpro sent me. So, I am pretty sure we don't have to worry about it being Platinum. 
Butcher, I am going to do the read by (4Metals) you directed me to over the weekend. Butcher, I hope to start on the Soup of Chemicals next week. I sure hope nothing pops up, I am looking forward to it. I know, with your guidance, I will learn a ton. I have got to get a few things together per your instructions. So, I won't bother you buddy with my questions until I am on the project.
Oh well, I lied Butcher. I do have a question. You mentioned a while back that there are many different grades of stainless steel. What grade and thickness do I need to try and find for the project? Using the size bucket you recommended? 
Thanks Butcher. 
Nickvc, I will try the HCL boil to see what happens also. Thanks Nickvc
Goldsilverpro, the name on the ring is very hard to decipher but it very well could be spelled Siladium. I read the info. on Google you sent the URL to. I am thinking there's a *very good* chance that's exactly what I have. But I am going to do the suggested test, just to try and verify, as best I can.
Thanks, Goldsilverpro
*Question to Anyone who would know? Does or will stainless steel glow white if heated as Platinum will as Butcher mentioned trying? I guess I could round up a piece of stainless and try it. I got to have some stainless stock anyway, but it's always good for me to know someone else has seen the results before hand. *
Welcome aboard Lobby, I haven't been here long myself. You have literally found a Gold Mine of Knowledge here on this forum. Lobby, I still can't get over the fact that all this knowledge is given freely with no strings attached. Well, maybe 1 string, you will probably end up with some very good friends, as I have.
Thanks Everyone,
Oneal


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## butcher

Question : “You mentioned a while back that there are many different grades of stainless steel. What grade and thickness do I need to try and find for the project? Using the size bucket you recommended?”

Oneal, I must admit I do not remember what we were talking about when you mention a stainless steel bucket, or what purpose you intend to use it, some stainless steel is magnetic and will corrode easily, I really do not even consider these as stainless.

The non magnetic types hold up well to corrosion, like 304 and 316 although I would keep them away from HCL, here is some Google info on stainless steel:

http://www.google.com/search?hl=en&source=hp&q=nonmagnetic+grades+of+stainless+steel&gbv=2&oq=nonmagnetic+grades+of+stainless+steel&aq=f&aqi=&aql=&gs_l=hp.12...1469l19128l0l20987l39l39l0l24l0l0l156l1610l8j7l15l0.frgbld.

Sorry I do have a bad memory. What are you going to do with the stainless steel bucket?


“Question to anyone who would know? Does or will stainless steel glow white if heated as Platinum will as Butcher mentioned trying? I guess I could round up a piece of stainless and try it. I got to have some stainless stock anyway, but it's always good for me to know someone else has seen the results before hand.”

When I have heated nonmagnetic stainless steel with a torch it would turn a kind of rainbow bluish color, sorry never tried a torch on platinum, but I hope to one day.


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## Oneal58

Hi Butcher, it was in your post about recycling my waste solutions. Your quote was, 
*"And a piece of non-magnetic stainless steel, for a cathode, I would also do this in 5 gallon bucket.
Large pieces of metals to fit bucket and give large flat surface area."*
I was just wondering what series of stainless steel would work best for the cathode?
But anyway, It seems every time I get ready to start on this Butcher something else pops up. When I can get to the waste solutions I will just get with you again. 
*Here is what is pressing now,*
There is a friend of mine who owns a computer service in a nearby town. He asked me if I would be interested in refining his circuit boards, chips, Etc;, that he has accumulated. 
I told him I would give it a try to see how it goes. 
I wanted to do a test run on some fingers, trimmed close. I ran 200 grams of closely trimed double sided fingers in a batch of HCL/CL. About half of the fingers were small and the other half was medium sized. I got a good return on the foils out of the 200 grams, or so I thought, at first.
When I put HCL into the foils, the once fair amount of fingers seemed to disappear in front of my eyes. After 3 washes in HCL I ended up with about 1/2 of what I started with before the HCL washes. 
I wanted to see exactly what amount of gold was in the 200 grams so I went ahead and ran the making gold pure process. 
I ended up with a good looking nugget, trouble is, it's only a little over 1/2 gram. I remember you saying something about electronic scrap here a while back that lead me to believe you process electronic scrap. If I am wrong about this I guess I didn't remember correctly. 
*My second question for tonight Butcher is,
Is this return anywhere near normal for 200 grams of small and medium sized fingers lot? The little button looks as good as any I have turned out and I believe it's near 24K. But I am wondering If this is a normal return or I am definetly doing something wrong somewhere and losing gold? I did the stannous test after each wash and detected no gold lose in the decants?
[b]My last question is this[/b], 
I left a window open and it rained and messed up my copper sulfate. The store I bought the old bag from started getting in a new kind. I am going to load a picture of this copper sulfate, it is a bright blue color. No green color at all. The picture is below. On the bag it says it is (99.0% copper sulfate pentahydrate). I am wondering if this is OK to use to drop gold with? 
As always Butcher thank you for your help. It is very much appreciated. 
Thanks, Oneal 
[img]http://web.ftc-i.net/~danni1/sulfate1.JPG 



*


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## butcher

Oneal,

You mentioned processing memory fingers in HCl/Cl, did you remove the gold plating as foils with HCl/3% peroxide first. Which also removes copper from the foils, before dissolving the gold foils in HCl and bleach?

The gold foils are removed from the memory fingers circuit board with HCl and 3% peroxide, before dissolving gold with HCL/Bleach.

When I process electronic scrap I do not calculate yields, I believe other members state 1.6gram to 2.5grams per pound of close cut memory fingers, I cannot verify these figures.

Copper sulfate is not used to precipitate gold, copper sulfate could be used to refine copper in an electrolytic cell, and it is also used to kill roots in sewer lines. This is not used in refining gold, although I have made copper sulfate as a byproduct of recovering gold.


Copperas or also called Ferrous sulfate or iron sulfate (FeSO4) is made from iron and sulfuric acid, it is a green crystal when made fresh, green crystals will precipitate gold, or test for gold in solution.
If the ferrous sulfate is oxidized in air it turns brown and will no longer work to precipitate gold. The name copperas has nothing to do with copper. I believe this is what you’re thinking of in using to precipitate gold.

I think the name has you a bit confused here.


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## Oneal58

Hi Butcher, 
You are right on all counts, as usual. I didn't mention the first step on removing the foils with HCL/3% Peroxide first before the HCL/CL.
As far as when I went to the hardware to buy the Ferrous Sulfate, (SULFATE) was all I seen when I looked at the package. Glad the crystals were Blue and I asked you before I used any of the Copper Sulfate. I don't know what I was thinking, had a lot going on but that just lets me know to be very careful from now on. 
I can't forget, if I happen to make a mistake with different chemicals there could be a dangerous reaction. I need to keep this in the fore front of my mind at all times. 
Butcher I am now working the many different types of CPU Chips. I didn't realize that there were that many different kinds of chips. Some have the solder on them that I have read contains a high content of gold. Others have no solder that I can see on them. Some are made of ceramic which i busted up good, others are just made of fiber that has what looks to be a stainless steel cover over the internal silicon chip, others have gold lids, some have no covers at all on them. I have a broad selection of chips made all over the world? I don't think that I have enough of each to run them seperately.
Can I just take the ones that have the stainless steel covers off with my knife (pryed them off)? Is the silicon that is holding this lid/cover on have gold in it? I have taken all the processor chips off the boards and opened all of the chips up. some just have gold pins on them. Some of these chips have gold pins on them that are only 1/32 to maybe 1/16" of pins showing out of the fiber board. I was thinking to just process the pins and save the boards to sell once I have enough that a refinner would be interested in. I was thinking of taking my dremmel and cutting the very tops of the short pins off and then cutting the pins right on top of the fiber chip. This I am thinking, tell me if I am wrong, would keep the majority of the KOVAR out of the refining batch. Which would also allow the acids used to get inside of the pins to strip the gold. Or am I off base completely here. Or the pins even gold plated inside?
Maybe as time goes on I may become competent enough to try and recover the other PM's that are in the componets on the boards. 
This is my first try at this, other than my disappointing returns from the fingers I processed. I got a total of .5 grams of gold from196 grams of fingers trimmed very closely. Just too much work for too little return and then have to divide that up. Not even enough to cover the chemicals used? Now, if I had 10 times that amount trimmed fingers, that might be worth all the work involved?
Just wanted to hear what your thoughts on this would be before I make anymore mistakes.
*Oh, I have one more question.* There is a square looking piece of silicone on some of the chips under the cover. Do I want to break this silicone/glass like piece up before stripping? I don't see any gold under the lid, just a piece of what looks to be a glass like cover over a white metal foil that looks to be a platinum color? 
As always, thanks Butcher, Any direction here would be appreciated. 
Thanks Butcher, Oneal


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## butcher

It has been a long time since I have done any CPU's.

I would process ceramic and fiber type separately.

A propane torch will burn off oils; remove lids and can help to burn of heat-sink compound (that you did not get completely wiped of before-hand). The torch can also help to remove pins from the fiber CPU’s.

A pair of needle nose pliers to grab the heated CPU, a bang on the table to knock off unsoldered pins or lids, or a paint scrapper to push then off.

The pin and fiber chips I would use hydrochloric acid and 3% peroxide, to remove base metals (Kovar), this can be done in canning jars, the small pins take time as the tube of gold with the sealed end is hard for the acid to get inside with bubbles trying to escape the tube, make sure tubes are hollow (float or swirl easy in jar before trying to dissolve the gold foil, You can then use HCl and bleach for the gold, the fiber board I usually incinerated after the process and peeled apart the layers of fiberglass, and to gain access to and process the metal between them.

The ceramics can be processed in Hydrochloric acid with additions of sodium or potassium nitrate (poor mans aqua regia), or with nitric acid and then aqua regia, or even HCl and bleach, just make sure there are none of the lids or heat sinks added, I usually break them to small pieces and leach them, (I would later then powder the ceramic and re-leach them again, others say there is no benefit to powdering them) the powders settle so frequent stirring is needed, also they need good stirring and rinsing after leaching.


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## Oneal58

Active Member 


Posts: 202

Joined: November 4th, 2011, 1:16 am

Location: S.C.



April 23rd, 2012, 2:49 pm 

Re: Refining Gold from Gold Filled Jewelry

Hi Butcher, I messed up when I replied to you on my last post. I hit the quote button on the bottom of the page and I don't think my last post showed up as a new post so I am going to delete the post that I hit the quote button and post this reply again. Maybe you will find it this time, sorry, I don't know what I was thinking when I did what you asked about previously. 
But You are right on all counts, as usual. I didn't mention the first step on removing the foils with HCL/3% Peroxide first before the HCL/CL.
As far as when I went to the hardware to buy the Ferrous Sulfate, (SULFATE) was all I seen when I looked at the package. Glad the crystals were Blue and I asked you before I used any of the Copper Sulfate. I don't know what I was thinking, had a lot going on but that just lets me know to be very careful from now on. 
I can't forget, if I happen to make a mistake with different chemicals there will be consequences. I need to keep this in the forefront of my mind at all times. 
Butcher I am now working the many different types of CPU Chips. I didn't realize that there were that many different kinds of chips. Some have the solder on them that I have read contains a high content of gold. Others have no solder that I can see on them. Some are made of ceramic which i busted up good, others are just made of fiber that has what looks to be a stainless steel cover over the internal silicon chip that looks like it has a gold colored solder around the edges of the square piece, which I think is the silicon chip? Others have gold lids, some have no covers at all on them. I have a broad selection of chips made all over the world but not a lot of any of them? I don't think that I have enough of each to run them seperately.
I took the the ones that have the stainless steel covers off with my knife (pryed them off)? Is the silicon around the edges that is holding this lid/cover on have gold in it or is this the heat sink silicon that you are talking about? I have taken all the processor chips off the boards and opened all of the chips up. Some just have gold pins on them. Some of these chips have gold pins on them that are only 1/32 to maybe 1/16" of pins showing out of the fiber board. I was thinking to just process these pins and save the boards to sell once I have enough that a refiner would be interested in. I was thinking of taking my dremmel and cutting the very tops of the short pins off and then cutting the pins right on top of the fiber chip. This I am thinking, tell me if I am wrong, would keep the majority of the KOVAR out of the refining batch. Which would also allow the acids used to get inside of the pins to strip the gold plating? Or am I off base completely here. Or the pins even gold plated inside?
Maybe as time goes on I may become competent enough to try and recover the other PM's that are in the componets on the boards. 
This is my first try at this, other than my disappointing returns from the fingers I processed. I got a total of .5 grams of gold from196 grams of fingers trimmed very closely. Just too much work for too little return and then have to divide that up. Not even enough to cover the chemicals used? Now, if I had 20 times that amount trimmed fingers, that might be worth all the work involved?
Just wanted to hear what your thoughts on this would be before I make anymore mistakes.
Oh, I have one more question. There is a square looking piece of silicone on some of the chips under the cover. Do I want to break this silicone/glass like piece up before stripping? I don't see any gold under the lid, just a piece of what looks to be a glass like cover over a white metal foil that looks to be a platinum color? 
I need to ask another probably stupid question here. why can't I strip the gold off all the chips together with AR or HCl/Peroxide or a weak Nitric solution?
One more question Butcher and I will let you rest.
I read that I can take 2 pieces of iron pipe. One of the pieces is just a little smaller than the other. It will silde into the other piece of pipe but will be fairly tight. I have read I can take the boards, chips, Etc;, and put them into a stainless steel pot, drill holes at the bottom of the stainless steel pot and place it in a bed of charcoal. I can then take a fan, small fan and bring the heat up enough so that the internal electronics will bake to the point that when I take the two pieces of pipe that has been welded shut on each end with a thick steel base. Use this as a tool to crush up the material to a fine power. Then use several or more washes with water to pan off all the non metalics, run a good magnet through the metal and then after I am sure I have all the non metallic material and fibers, foreign materials out of PM.s use AR to recover the gold out of this material. 
Does this sound vialble to you or it this something that would be a waste of my time? 
Excuse me Butcher, I see where you directed me to powder the chips in your previous post. 
As always, thanks Butcher, Any direction here would be appreciated. 
Thanks Butcher, Oneal


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## butcher

I use about a 3" pipe about 12" long I welded a steel bottom on it, then a piece of pipe 11/4" 18" long with pipe caps on both ends, this homemade mortar and pestle to break the ceramic chips, I did not try heating them first, you can only break one at a time, they are hard and the surface are of the chip to hammer makes this a lot of work (and if you crush them to powder as I do after the first leach, it is a lot of work).


I would not strip the ceramic processors with the fiber board processors, the fiberboard CPU's have kovar pins this and the lead and tin solder would give you troubles, if you tried to process them with your ceramic CPU's in solutions to dissolve gold. 

The fiber chips I would remove base metals using HCl and 3% H2O2 first.
We Know how much trouble the tin is in our solutions.

There is a recent discussion of processing the fiber type CPU's,
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=39&t=9693

How is that Grandbaby doing growing like a weed I would bet.


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## Oneal58

Hi Butcher,She is here right now, she says Hey. I can hardly type most times with her sitting in my lap but that's OK, I manage. She pretty much hangs with her PaPa every single day she can. She doesn't like me working with the refining, she keeps walking over half-way to the old house and calling me until I have to stop what I am doing, step to the door and let her know I am OK. I guess this is my fault, I instilled in her and my grandson how dangerous what I do and how it will cause them harm. And never, no matter what to go over to where I am working. That it was just too dangerous to get close to where I am. Now she worries about me all the time. But, I will have to admit, it feels good and brings a smile to my face each time she does this. She doesn't give up, she will call me constantly until I step out and give her an answer. She is going to be a sharp little thing and is growing like a weed. 
I hope you and your family are doing well also, tell them I said Hey as well Butcher. 
But anyway, I could go on (bragging), Those but I need to get back to the refining. You say you haven't tried the heating method of the chips yet? From what I can find out (research) the ceramic chips break up really easily if first heated with the charcoal method. I will give it a try when I have time and let you know how it goes. If it works, it sure would save a lot of work.
Butcher do you think that this method would work with the fiber chips/boards as well. I know there will be some very toxic smoke that comes from doing this but it seems that if the process works what you would be left with would be just the metals that were in the fiber chips. Then process the remaining metals after they cool/ treat with the HCL/and H202 as you advised. Then go on with the refining from there. If this would work it sure would be better than trying to seperate all the crushed fiber material from the fiber chips by water and panning? I read a post of yours previously that you said you seperated the layers of the fiber chips to get at the metal between the layers of the fiber material. Do you think to burn all the fiberous material away would take so much heat that it would melt or fuse the remaining metals, or would it matter? Or just make one big mess? Holes were drilled all the way around the stainless steel vessel about 2 inches up from the bottom so the smoke would exit the bottom of the vessel.
I have even read that all the boards, chips, Etc;, incinerated and what metals that were left were then processed from there.
But I am going to follow your advice and if it works out that I have a lot of elecronic scrap from computers and if there is any money to be made I may look at some methods to process in bulk amounts? If It works out and I have bulk amounts of electronic scrap to process it sure would take a lot of the work out of processing a lot of material. 
Right off the top of your head do you know how the large bulk processers go about processing their chips, boards, Etc;? 
Let me know your thoughts on this Butcher. 
As always, thanks Butcher for any advice and insight. 
Oneal


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## butcher

I would not burn large amounts of circuit boards, but I have built a fire with a good bed of coals and put some of the fiber chips in the pan with a lid shoveled coals over the top and threw firewood on top of that, the flames were hot enough to burn the smoke from the pan, this was not large batch's, after they cooled the fiberglass sheets would separate and I could separate the metal from the fiberglass, my fire was not hot enough to melt the metals but incinerated the resin in the fiberglass.

Since then I have seen members like no Idea and patnor discussing Pyrolysis of the chips (I understood the theory from making my own charcoal), this was kind of what I was doing with the fiber chips in the pan, but if I done it again I would use some of the ideas these guys have brought to the forum.

if you can keep the smoke in the fire until it burns it up there is not much more smoke that the regular fire, smoke in wood besides water is un-burnt fuel. The smoke from resin would also be un-burnt resin (fuel).

Still these have a little lead solder I the pins, so I would not stand there and roast hot dogs over them.

I would not think of doing this for large batches without building afterburners.

I enjoy hearing how much you and your grand-baby enjoy each other.


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## Oneal58

Hi Butcher, just wanted to say hey, I have been back to the hospital again. Just getting back to feeling like sitting up again. I hope you and your family have been doing well. I want to get started on the solutions once I finish up this first batch of chips and fingers. I had to let the last refines sit for a while but hopefully I will be back on it again in a couple of days. 
Butcher, I just walked over to check on everything I had to leave as it was. While I was checking on everything I looked closely at the solutions that I have been accumulating. 
I did mix solutions at the begining but later on I did get to doing things (mostly) right and I would seperate solutions into 5 gallon jugs and mark. I paint the lids on the jugs also so what happened with the marking of the vessels with magic markers and have the markings disappear would not happen again. 
I have Nitrate's, HCL washes and Sulphuric solutions from my cell that (I Think??) that contain only those acids and aren't mixed with anything else. But I can't be absolutely sure? 
Since I can't be 100% positive that I didn't mix anything else with the earlier solutions that I think are pure, would you take the chance or just go ahead and process as you said in your previous post and not worry about saving/recovering any of the used acids that I can't be 100% sure about? 
For the last few months though I have got it together and do a good job on keeping everything seperated. I give this stage the attention it deserves, but I had to learn this the hard way I guess. 
I know for sure I have precious metals in the early waste solutions. I made a good many mistakes the first couple of months. This time period is when I refined all my good quality scrap. I probably have as much as 1/4 of the total gold in these waste solutions that I have already recovered and most my silver in these used solutions.
But I just wanted to touch base with you and let you know that I am still around. 
Thanks Butcher, as always, your help is very much appreciated. 
Oneal


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## butcher

Oneal, it is good your back up and about, sorry I do not remember what we were talking about with these used solutions so I will not try and answer something I am not sure of, It is good your up and wanting to get back to work, take it easy and do not overdue until the body strengthens and can take it.
Small steps and we will see some more of your beautiful gold.

Your friend Butcher


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## Oneal58

Hey my old Buddy Butcher, hope you and family are doing well. Have requested Dr. to test my blood for heavy metal poisoning. I have just been too sick for too long. I just want to know if I may be more sensitive to the whiff's I get from the chemicals from time to time than anyone anyone else would normally get. Such as taking off the tops of canisters, making homemade nitric, adding sulphuric upwind from batch but still getting a whiff sometimes. Such situations as that. I may be more sensitive to the vapors than most people. I need to know this before I mess with the recoveries anymore right now. I think most of this came from the last batch of silver I melted, caught a little of the smoke off the melt. If I am that sensitive to the vapors I am just going to get me a positive air flow mask/suit and that will take care of that problem. This is the first time I have been back up in days and days. Waiting on Blood test results. Will let you know when I find out something of what's going on with me. Haven't been doing anything at all with the Gold until I find out for sure what's going on with me. 
Will let you know Buddy when I find out something. My family Dr. had to send samples off to have tested. Says she will call me when results get back. Said that that type testing is something she has had to study up on herself, I guess no one else is doing what I am anywhere nearby or using my Dr. at least? Holiday slowed down everything down everwhere. It may be the first of the week before I know something for sure. Will let you know. 
Thanks, Butcher 
Your friend, Oneal


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## butcher

Oneal,

Sorry to hear your still having troubles with your health, I know it is not any fun.

I do believe some people can be more sensitive than others, to almost anything including metals an these vapors, if you have other health issues the immune system can also be weakened and I would guess make a persons system more agitated by these substances, also certain metals in certain states can be dangerous for a healthy man, and for someone having health trouble I believe can be much more dangerous (like melting zinc, these fumes from welding galvanized iron have made me sick with cold sweats for days after, (I know better know).

if your system is weakened by a cold, flue or pneumonia any fumes surely would not be good for the lungs or the health in general.

It is a good Idea to get your blood levels checked for these metals, Hopefully the level will be normal and the doctor can find some simple solution to get you back on your feet and hopping around like a spring chicken chasing June bugs.

Take care of yourself; all the gold in the world is no good without your health.
Your friend Butcher


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## Oneal58

Hello Butcher, and everyone. 
Well, I am back from the dead, literally. I will not bore everyone with my experience on the operating table but I thought I would just let you know I am still around and kicking. I was able to gather enough strength today just to post a note to you. Just to let my buddy know that all the work he has put into me wasn't all wasted. I am hoping in a couple of weeks I will be up and going once again. 
Butcher it would be good to hear from you. I have missed aggravating you this last couple of months.
Give me a shout to let me know you are still educating ones like me. 
Waiting to hear from you Butcher, 
Oneal


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## Palladium

Great to hear your doing alright Oneal. I been there brother! God wish you a speedy recovery.


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## butcher

Hey, it is great to hear from you, I was wondering how you were Oneal, thank goodness your still with us, I bet you holding your grandbaby close by, get strong so you can play with them they need you so much, I know your as stubborn as an ole mule so keep Kicking and build up your strength, I still try to help on the forum, although I have had a hard time reading everything everybody writes nowadays.

It is good to hear from my friend, and to hear he is getting back on his feet, take care.

Butcher


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## Oneal58

Thank you fellows, it has been a rough ride but hopefully in a few weeks I will be up and going again. Thank you for welcoming me back. I spent the long days in the bed studying and looking forward to getting back up and going. Hopefully it will not be too long, then I will be able to get back to doing what I have become to love. The longer I am here the more thankful I am for each day I am blessed with. 
I will be aggravating everyone in no time once again. 
Butcher, you are exactly right. Those Grands need me right now. I am the only one they trust to pull their teeth, so what would they do without me, :lol: 
Thanks Everyone,
Oneal


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## maynman1751

Oneal,it's great that they found what was ailing you. Hope you have a full recovery and can get back to business. John. 8)


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## Oneal58

Hi Butcher, 
I finally felt like going out to work place and taking a look at what was going on. I have many 5 gallon jugs of spent Nitric solution with copper bussbars that have been in the solution for probably 2 months now. I drained/filtered a couple of these jugs, (poured into a larger barrel). I found that I have a fair amount of silver in the bottom of all the jugs. I also can visually see gold mixed in with the silver that is in the bottom of these 5 gallon jugs. 
As you know I have been making my own Nitric. Most of this material is pure silver. My thoughts are that my homemade Nitric is not strong enough to dissolve the silver and leave the gold. Surprisingly when I first got started at this I was losing a lot of gold into my decants?? That has settled out over time into the silver in the bottom of the jugs, I guess when I mistakenly poured my metabisulfite into the jugs when I was first getting started? I have a condenser that I could make stronger nitric but it would take me a while to make enough to dissolve all the silver that's in these jugs, it's a fair amount. 
I have also thought about just dissolving the gold with Aqua Regia and leaving the silver to clean and process. I will rinse the silver bearing gold many times before attempting this making sure I have all the other chemicals that could be present still in the solution. 
Does it make sense to you to add some metabisulfite to the spent nitric solution to make sure and drop any gold that still may be in solution before I attempt this. 
Or is there a more simple way to go about recovering the gold out of the silver?
This would leave only Liquid which I will process with the method you gave me earlier before I got sick. 
Your thoughts would be very much appreciated on this Butcher. 
Thanks Butcher,
Oneal
P.S.
Thanks maynman for welcoming me back, it's appreciated. Oneal


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## butcher

Good your back at it.

I would look at using the silver to in-quarter my gold with, and recover the silver and gold in those processes, if this silver was cemented from copper then you could wash and then melt it and shot it for use.

Trying to dissolve the gold out of this is going to form some silver chlorides, all of the silver may not convert to chloride, I suppose you could do that, but then you would have silver chloride to deal with.

The homemade nitric could have some chlorides, (sulfates with homade nitric are also almost always involved) which the chloride if involved could have dissolved a little bit gold,(gold could also have been in fine powder or flakes especially if tin was involved and got carried over then), but if you cemented everything in this nitric with a copper buss bar,That gold would have also cemented with the silver and settled out of solution, I see no need for adding SMB to the nitric acid (it most likely would not work anyway), if you were concerned of any valuable metals in solution, you could take a cup of the solution, a very clean strip of thin copper and heat the solution with the copper see if and powders form (black powder for gold, PGM or gray cement for silver). I do not think the stannous test would work if any nitric was still active, if all of the solution was converted to copper nitrate solution with no free nitric (even when heated, then the reaction with stannous could show something (although if this was the case most likely all values would have been cemented before copper nitrate was saturated).

Take it easy and be careful.


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## Oneal58

Hi Butcher, 
I agree, that's the best way to go. I do have a problem though with using the silver to in-quarter with. I estimate that I am going to have 4 or more pounds of this gold bearing silver. That's getting up around a pound of Karat Gold that I would need, of which I do not have on hand?
I have been through most of what gold filled I had on hand, (80%) or so. I will more than likely end up with even more silver from the remainder of the Gold Filled I have on hand when I process it. So, I am spinning my wheels, as far as getting at what gold I have in the silver I have now. 
I did take the time to make up some new stannous and test each and every jug, all tested negative for gold. So, as you said, what gold was in the spent nitric has dropped out of solution.
I think I will do this, I have been wanting to build me a silver cell. When I get to feeling a little better I will build a silver cell, recover the pure silver bullion and collect the gold out of the filter bags. 
Do you think this would work Butcher?
Thanks Buddy, 
Oneal


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## butcher

silver cell would be a good option,

Since this batch was cemented silver from homemade nitric acid, it is likely you also have silver sulfate, or other metal sulfates in these powders, in this case I would try inceneration, with some iron metal in the mix, this can help to drive off any sulfate as SO2 gas, then use store bought nitric ( or distilled nitric) to dissolve the silver, clean up any iron, copper ect, and seperating most of the gold, then re-cement the silver on copper, wash the copper out of the cemented silver, melt silver into anodes.

You will ned good nitric for the silver cell.

You could try to incenerate (some iron in the powders) wash and melt and try running the impure silver several time's through a cell (similar to running sterling through the cell), but I do not see any advantage in this process as you would be using just as much nitric acid (constantly replacing contaminated nitric electrolyte, and silver purity would surely suffer with the process).

maybe another member has a better Idea on how to proceed with your batch.


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## goldenchild

If I've read the last few posts correctly Oneal has a batch of finely divided silver mixed with finely divided gold. In these forms the metals are easiest to deal with so I wouldn't try anything that involved melting the metals. So unfortunately I think the best route would be to rinse your silver/gold powders well and digest the silver in nitric. I know the downside to this is the amounts of nitric you'll need to use. Have you a distillation setup? This is something I've been wanting to try with gold filled and imagine it would work great with silver but... If you take your silver and put it in the reaction vessel of the distillation setup and digest with nitric, you will be able to capture all of your spent nitric and use it over and over again. Then you would simply decant the digested silver and leave the gold on the bottom of the reaction vessel. Add more silver powder and repeat. At the end you will have all of your silver in one container ready for cementing and all of your PM's on the bottom of the reaction vessel. A minimal amount of nitric would have been used. Just an idea.


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## butcher

goldenchild, I agree, but with this method I would watch for undissolved silver sulfate (sulfate from the homemade nitric used previously).


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## Oneal58

Thanks Butcher, Goldenchild, for your post, they are appreciated! 
I do have a distillation system. I bought it when I first considered refinning, never have used it though. I think that the method that goldenchild mentioned might work best for me since I have everything I need to get this job done. This method sounds like something I can already handle as well. 
BUTCHER, the comment you made about the sulfates in with the PM's from the homemade Nitric I have used? You mentioned incenerate with iron metal to drive off the sulfates as S02 gas with some iron metal in the mix. Can you give me an idea of how much iron to use per ounce and what form the iron needs to be in to use in the mix. Also, I know Iron comes in various qualities and my knowledge is very limited in this area. Can you recommend which type iron I would use for this and where I would find it? I have strong angle Iron, would that work? Do I use it like it is or take my grinder and finely grind it up into shavings?
One more question, how about the possible SMB Solution in with the solutions, MAYBE??? Will several rinses with distilled water take care of this?
Thanks Butcher, Goldenchild and Everyone.


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## butcher

Oneal, I would use small pieces of iron, like horse shoe nails, or transformer laminates, regular nails would probably work but they are steel, I would not worry about having more nails in there than you need they can be screened out later, I believe this is a contact process for iron to collect the sulfates from the silver and then heat to decompose them to SO2 gas, so you want the silver powder to come into contact with the iron stirring powders well while heating, not much iron would dissolve in the mix so here not much iron would be needed (except the contact with silver sulfates).
Iron powder or filings would work and get good contact, but would be harder to remove the undissolved iron later.

any SMB powders should wash out, but if much was in there and if base metals were involved it could have also made sulfate salts (the iron should help here also).


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## Oneal58

Butcher,
OK, I got some horse shoe nails I found in an old box from auction along with some horse shoes. My wife makes wind chinmes out of the horse shoes, maybe the luck will rub off of some of these nails. :lol: I guess I should not be depending on luck but I guess it never hurts? 
Anyway, from the way you are explaining it, there is not a count per ounce, it just has to be enough to make good contact with all the silver when I add the nails and stir? Cutting the nails into say (8), 1/2" pieces before adding may help, don't you think?
I will rinse several times with distilled water, let settle good between each rinse and make sure and sink the floaters. Add the nails, heat. 
Question, how long to heat and what to look for when the S02 has been removed? I don't see where you mentioned a (LENGTH OF TIME) either? Do I need to boil or just bring to just under boiling point. 
If there is not an indicator to look for, if not, how long would you say to heat 4 ounces per run of silver/gold with half-dozen or so horse shoe nails cut into 1/2 inch lengths? Do I need to use more nails per 4 ounce run of silver/gold material. Could I use more silver/gold or should I use less silver per batch and also how many 4 inch nails, (cut into 1/2" pieces) should I place in the Silver/Gold mixture to accomplish this? Would a indicator be when none of the nails are being dissolved?
Then, just go with the distilled Nitric, reclaim the Nitric by distillation and start on next batch? 
Butcher what would be the best way to get rid of the Nitric left in the solution, incenerate silver and gold mixture or do my best to rinse out the Nitric with several boils in hot water and decant, then incenerate? Since I will be using Nitric to dissolve the silver and leave the gold do I need to worry about the Nitric? Will the hot water rinses get rid of the iron that may be left in the solution?
BUTCHER, if you see where I need to make adjustments to this plan please let me know. 
As Always Butcher, THANK YOU. I don't know what I would have done without your guidance from the very start. Just let me say again, I really appreciate you and nothing/your help/and especially your friendship will ever be forgotten or is taken for granted!
Your Friend,
Oneal


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## lender

I'm trying to download Hoke's manual but scribd won't let me without paying for it. Is there something I need to know about the free download I keep seeing throughout the forum? I even tried the one day pass and I still could not get it to download.


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## jimdoc

lender said:


> I'm trying to download Hoke's manual but scribd won't let me without paying for it. Is there something I need to know about the free download I keep seeing throughout the forum? I even tried the one day pass and I still could not get it to download.



Try here;
http://goldrefiningforum.com/phpBB3/download/file.php?id=2480


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## Palladium

Yeah Scribd started doing that after i posted it there several years ago. Pisses me off! I though about linking it back to the forum. It's just that when they read it on scribd they also can see my other free downloads there also. If you open a scribd account and post something, anything it don't matter what, they will let you download for free anytime. It's easy to open one. They don't spam you or anything of that nature.


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## goldsilverpro

Unless it has changed recently, when you try to download a file on Scribd, they ask for either money or an upload. If you upload a file, they let you download free for 24 hours, I think. I usually upload some PM pdf file on my computer that I have downloaded from some other source.


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## Oneal58

HI Butcher, and Everyone.
I bought out a Jewelry Store many years ago. I sold or rather give away a lot of gold out of that purchase before realizing what I was doing. I started testing each and every piece when someone commented he had hit a bonanza that was mismarked, this material came from me too. 
Anyway, I have a lot of material left that does not test at 10K but I don't want to make a mistake again and sell material that is less than 10K for scrap iron prices. 
I have a lot of this material, fresh out of the molds, a lot of it still has the white material on it that wasn't cleaned off when taken out of the mold.
It would take a really large amount of Nitric to dissolve all this material up and it may end up not being gold at all! I have been looking at using the Muriatic and Soda of Nitrate process. 
IF ANYONE HAS TIME COULD THEY PLEASE TELL ME ABOUT THE PRO'S AND CON'S OF THIS METHOD, IT WOULD VERY MUCH BE APPRECIATED! The video's and information I seek seems to be left out OR I just can't find what I need to know. 
Question1, Like, how much Soda of Nitrate pellets to use per 1/2 gallon of Muriatic, or just the ratio's, metal, soda of nitrate, muriatic %. 
Question 2-This would give me how much of this mixture I need to use per pound of material. I have many of what I am calling trees, the things the Jeweler's used on each piece of jewelry to Gold Plate It, I HOPE. I also have a lot of material that I don't have a clue what it could be. Looks sort of like zinc, some of the pieces have Jewelry individual pieces still on them that wasn't cut off.
Question3- Would I put everything into the batch?
Question 3-How long do I need to treat (unassembled jewelry pieces) material or just keep treating until I get no more Brown Fumes?
Question 4-Do I need to pre-mix the Muriatic and Soda of Nitrate Pellets before I add it to material?
Question 5- What colors to look for in the solution. I know it should be yellow (since I am trying to dissolve gold, but I ran a test run on some material and the color of the solution was jet black?? Can anyone tell me why I ended up with black when I should be dissolving gold? 
ON MY FIRST TEST RUN I USED 1/2 POUND OF JEWELRY PIECES, 1/3 GALLON OF MURIATIC AND 1/4 CUP OF SODA OF NITRATE PELLETS?
If anyone can tell me if I am doing anything right or all the things I am doing wrong or anywhere IN-BETWEEN. The things I should be doing and what I should be doing, it would be appreciated. 
My reasoning for trying this method is I know that I will probably have a lot of material that does not contain gold. I just don't want to waste any NItric on metal that isn't gold or silver?
Oh, yes I do get a very strong positive for gold with the stannous test.
Thanks, Everyone
Oneal


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## butcher

Oneal,
I would test the material with drops of solution, sort it accordingly.

Nitric on a file spot can detect copper; it can be used to help detect silver and gold.
Nitric can also be helpful in determining gold plating on an object.
A scratch stone is also useful with a drop of nitric acid.
Many base metals would react with HCl alone, those above hydrogen in the reactivity series of metals.
Schwerters solution can test for silver, help to determine karat gold (other metals) and can test for some of the base metals.
The touch stone and using karat needles and comparing the marks of known and unknown scratch marks using nitric and different concentrations of aqua regia and known test needle scratches.
You can also get an idea if PGM may be involved with this test.
And then there is putting a small portion of the metal (drilling filling) into solution and testing with stannous chloride, DMG, and so on.

Pawn broker’s guide is an excellent source for these methods (you can find it in a search of the forum).

After determining if an object is plated base metal and possibly what base metal, or if the item was karate gold or silver, and separating these materials,

Then decide how to process, some material may be better to run in the concentrated sulfuric cell, very little chemicals or waste to deal with, some may be valuable enough to melt with silver dissolve silver and base metals in nitric and then refine the gold.

Testing can also help you to determine what material may be better off sold that messing with yourself.

As far as making a large batch of poor man’s with HCL and a nitrate fertilizer, I would hold off on that Idea for now, in my opinion it would not be good for large volumes of base metals Too much waste, and also small amounts of gold dissolved into solution with untold amounts of unknown base metals could just become a mess.

I would first get an Idea of what I had before making plans on how to process it.

I know I did not answer the questions you had but I hope this helps.

How have you been? we do not hear from you that often anymore, are you getting good hugs from the Grands?


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## Oneal58

HI Butcher and thanks. My daughter knows I am not up to my old self, yet. She sort of limits the visits from the kids, knowing they can be a handful at times. I have got to call her and tell her to let me be the one to say it's time for a break instead of the kids thinking it may be me that does not want them to visit. 
Butcher, I guess I was just trying to take the lazy man's way with this lot. If I had to sit down and count how many of these unassembled bracelet, necklace, pieces, I have, the count would more than likely run into the thousands. 
So that is why I was looking for a process to make it less involved. I guess this is telling me that I am not yet up to the job healthwise yet. I would not have hesitated to test each and every piece a few months back. Maybe I need to just take a little more time to get back to my old self and build my strength back up. 
 By the way, thanks for asking Buddy. 
Oneal


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## butcher

Oneal, can you sort some of the material which seems of higher quality that the others by looks?

A helper could also help with testing.

A long journey starts with one small step, a mountain can be moved one shovelful at a time, do not look at how far you have to walk, or how big the mountain is, just take a small step and one shovelful.

Oneal, you really do not want to overdue, but you also do not want to let the moss grow under your feet, take it easy, but do not give up, and build your strength.

Give those grand kids a big hug for me.
Your friend Butcher


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## Oneal58

Hi Butcher, everyone
Butcher, thank you so much for the encouraging words in your last post. I apoligize for being away so long and not contacting you. As good a friend as you have been to me I at least felt I needed to let you know I am still hanging around. Not so high anymore but still here. 
Not too many years ago you could not have convinced me it would take all the energy I could muster to make it to the computer room or the bathroom? 
I just want to take this opportunity to thank you. You are and always have been a willing, free hearted, very highly respected individual by me. What a great guy you must be and I only aspire to come somewhere close in this lifetime. Qualities in men are sometimes put there through hardships, successes, failures, etc;, experienced. But, of course for some, just being thankful for just the gift of life. Most importantly, let me not to forget and leave out our (Parent's), mentor's teacher's, Etc;, starting at birth and then throughout life. 
I am and always will be thankful for your guidance, your patience with me. But most of all, befriending me. I just wish I could have meet you sooner.
When I can get to going again, I have a thousand questions for you. 
Your Friend and devoted apprentice, forever.
Oneal, 
I hope I got that Etc; thing right, or is it "Etc", if I messed up Harold will have a fit, thanks Harold for all your help!!

P.S.
I also want to thank (KADRIVER) who has also went out his way to encourage and help me that few men would have done. I also want to thank everyone on the site for their support and guidance as well. I will talk to everyone again when I get to feeling better.


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## Palladium

Our prayers are with you.


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## maynman1751

Oneal, hang in there and gather your strength. You are in our thoughts and prayers. John.


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## butcher

Oneal, 
I have missed you on the forum, I also feel appreciative to be able to have met you and feel the bond of friendship, I also hate to hear your still struggling with your health, and at the same time glad you are looking to get back up and refining, that shows your fighting spirit, and you are not giving in, keep fighting to get back to the computer, and join in on the forum we miss you here, and the forum I believe can also be good medicine for the mind, and if we can help to keep our mind healthy it can also help our body healing.

I miss some of our discussions, you had a way of making the discussion very rewarding and full of detail, also I feel like even though I have not met you I know you, and I have a good friend in life I can count on (a rare thing in life), I also miss the discussions about the grand kids, I do not have any grandkids, maybe that is why I love to hear the stories about yours.

My good friend do not give up, and get better, so we can have some long chats, about gold and Grand kids, you have been missed here on the forum.

Get back to health

Your friend Butcher


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## nickvc

Oneal I too wish you well and hope your health and strength return to you soon. 
With Christmas coming perhaps ask for an I pad or similar device so accessing the forum isn't such a chore but one you can do from your armchair or bed if necessary, keeping your mind active is as important as every other treatment in regaining your health, as I know your are aware of how much information there is on the forum it will keep you busy for decades and work your mind continually and hopefully give you the needed impetus and even better the knowledge to return to your hobby with renewed enthusiasm.

Keep well and stay in touch with the forum even if you cant process at present I'm sure in time you will be back to it.


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## Oneal58

My sincere thanks goes out to each and every one of you for your support and concern. After reading everyone's post I have felt better today? After the first month I was a member here of the forum I knew this forum was much more than just a place to seek free knowledge for a new hobby. I found out very quickly that it was and is a place to meet and talk to wonderful individuals from here and around the world. 
Butcher, those grand's are growing like weeds, I think that there's something in the food the children eat anymore nowadays? They both just left the house, my grandson Dayton, has this golf cart that looks like a dragster. He also drives it like one. Thank goodness it will not run like one. He wanted a 4-wheeler but I stopped that in it's tracks. I caused a big fuss but I stood my ground! My Pastor, Son-in-Law finally came around, after showing him some statistics of how many young children gets killed or hurt badly on 4-Wheeler's. You know the reason I had to do that Butcher. After the lose of one of these precious gems given to us, I will not take the risk, ever! There are just too many accidents with the 4-wheeler's involving children that concerns me. Especially children who drive like I once did in my youth. Which my grandson only know's one speed, pedal to the metal!!! I guess it's in the gene's passed down from PAPA. It was sure in my blood, 440 Hemi Cuda, Super Sports Chevelle's that muscle car fever lasted for far too long in my life. Then came the Motor Cycle craze which did kill me for a short period of time until the Dr.s fried me with the paddles. I could not walk or move for days after that. Every muscle in my body turned into cement, that's what it felt like anyway. That is when Mrs. Parker put her foot down and I had to sell everything I had. 
Now, the little Angel, now she is 6 years old. Of course she has to see her Papa every single day. Even if just for a few minutes. If I am laying down she comes in to my bedroom and gives me a big hug and a kiss, and of course, (I love you PAPA). Crawls in beside me and says she wants to cuddle for a while. I looked out the window today and she was dragging a snow man in a snow sled. She drug it up on the front porch and plugged it in. She says, now Santa can see you Christmas Eve night. What wonderful magic memories she brought back to me by her actions today. I fear it will be her last magic Christmas, I think she already knows but just knows how to play along also? She has already asked why Santa only worked on her playhouse when she was gone or in bed? In a few years she will go as my Grandson is going, his own friends and things to do. Much more fun than hanging around with a broken down old man. But this is normal and I expected it, I even encouraged it, so no surprises there. 
Both of them are sharp as pins, I am so thankful for their good health, mentally and physically. When I get the time I will send you a picture of them. It makes me feel so sad for you to know you will never be able to experience grandchildren. For me personally, I am enjoying my grands more so than I did my own children. Reason being, that I don't feel the need to make them toe the line as I did my children. In my case, I really do enjoy my grand's more. Don't get me wrong, I am not saying I love them more than my own, but just as much as I did and do my own. What I am trying to say is, I can enjoy them more, but love them the same. 
How about I stick them in a box and mail them to you for a few days. After a few hours with both of them together, I may get them back, mailed by way of express overnight,Guaranteed delivery by 10:00 A.M.! 
Thank you so Much Everyone!
Oneal


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## Oz

Oneal,
Your attitude impresses me greatly. Both in how you are choosing to look at some of your health issues and family, as well as how you choose your friends. You have picked from the cream of the crop on the forum in noticing what a fine man Butcher is. Humble, educated, and well walked in many a man’s shoes. 
I will hold you and yours in my prayers and wish you a happy and healthful holidays.

PS; yes I have broken from forum rules in keeping religion out of general discussion.


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## Palladium

Glad to see you back to Dave!


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## Oneal58

Thanks Everyone for your encouragement. It is all appreciated and truely has helped. 
Butcher,
I caught the wife gone today to see her mother. I took your advice and just made myself walk over to the work building. I had to leave a couple of projects right in the middle of finishing them off. As I have mentioned before after the last operation my memory doesn't serve me well anymore. I normally keep notes on each process as to where I am on them, especially through the weekends so I don't make any mistakes due to not remembering where I was on a refine. 
I didn't have the note option this time , I had to drop everything and leave it. So when I walked back into the work room today I was surprised to find out I had left 4 different projects going while I have been unable to get out. I was able to figure out that 2 of the refines were left sitting in AR. Then on the other 2 refines I could not remember what had happened. I know that I have a very large corningware dish over 1 inch deep that has gold in it, it has dark regular colored silver that looks like it has just been dropped with copper after a Nitric bath, and on top of that I have areas of what I believe is Pure White Silver Chloride.I have at least 1-1/2 pound of this stuff. 
I was thinking of several different methods to try to get the Gold out and the Silver Chloride back to elemental silver? If I had to give % of white substance to the regular silver colored silver I would say that 30-35% of the white substance. I had left everthing covered with water before I left. 
I am pretty sure my homemade nitric caused this to begin with but that doesn't matter. What matters is how I get out of it without losing all the gold which is the most important for me to save. There is a good bit in the lot. I have read back over my previous post and in the building I see I was in the middle of setting up my condenser to make purer Nitric so I must have been going to try and dissolve the silver and then filter and drop. Then recover my gold, which should still be in the large corningware dish.
I did this today, I rinsed in cold water, let settle and repeated, repeated, then repeated again. So I have rinsed refine 3 times in cold water. Keeping all the decants. I will check for silver before decanting. I still have the insoluble white silver compound. I thought about adding heat tomorrow to see if I could get some of the white substance to dissolve? 
I thought about using the iron as you mentioned earlier but being mixed with that much elemental silver the chances of all the white substance contacting the iron would be minimal or would it Butcher?
Butcher, how about using (AR) to go after the gold first since the gold is really fine? If I drag some silver over I could take care of that just as I always have? What would keep me from doing that. Wouldn't I be able to get most of the gold with AR, then go after the Silver? 
Is there some properties that Silver Chloride has that would interfere with going after the gold first with AR? I realize I will have to rinse many times and end up with a large quantity of solution but I can evaporate all day if need be?
Or could I just incenerate (outside of course) a little at a time until I drive off the salts and then go with Nitric, to start over? Or just get outside somewhere, melt in small lots, make shot and then go with the Nitric?
Butcher your advice would be very much appreciated. If I feel as good tomorrow as I did today, I just may give it a try. 
If I am not thinking correctly here you let me know Buddy. 
Oneal


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## butcher

Oneal it is great to see you get up and get some fresh air.

Well let’s see we do not know what this is if it is a chloride or not or if any nitrates are involved.

First I would separate any larger pieces (I use a cheap plastic kitchen tool a cup with a handle and a plastic screen), screen the powders separating the larger pieces or un-dissolved metals, if all are powders you can skip this.

Let’s give these powders a boil in water and decant the water while still hot (let any white powders settle), decant the liquid int a jar let this jar cool ,we may have a colored liquid indicating copper, and if you see crystals form after it cools this can indicate lead chloride we dissolved in the hot water, if rinse is dark colored or lots of lead we may wish to do another boiling hot water wash, if only lightly colored we will go to next step. (check and see how the liquid filters this will give us a clue if tin may be involved for our later steps)

Cover powders in water adding sodium hydroxide NaOH (caustic lye), we want to make salts out of any chlorides and if we make silver oxide that is OK too, get close to pH 7 or neutral, stir powders well, let settle and decant the salt water that has formed, wash several time in hot water, this is to help remove chloride trying to convert then to salt water and washing out the NaCl salts.

Decant liquid, set heat to low to dry powders when dry raise heat then to high keeping powders crushed, they may fuse and seem to get wet again like syrup, you may have to lower heat to keep it from bubbling if this happens heat till dry again raise heat and re-crush powders roast red hot with good air contact stirring red hot powders (you may see powders darken as they oxidize.

If tin was indicated boil in HCl, lower heat, let powders settle add a very small amount of water then decant the wash hot, give several hot water washes, neutralize again NaOH, water rinses to remove salts, and incinerate to remove chlorides. If no tin was indicated you can skip this step.

Now this should leave your powders as metals powders and oxides, you can get silver palladium if any, and base metals with HNO3, and wash's in hot water in hot water letting powders settle before decanting liquid to a jar, hang a bar of copper in this nitrate solution to cement out silver and palladium. 

Here I would wash the powders using Harold's gold wash and then you can dissolve them to refine them as gold (PGM's if involved).
I would refine them twice with good washing techniques the gold should be very fine.

Do not forget to use your testing solutions.

Do not overdue or over work, but do try and get up and get some air.
I am glad you’re feeling good enough to get up.
Take it easy, and give those grand kids a big hug for me.
Your friend butcher


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## nickvc

Oneal I to am glad to see you back to better health and feeling like getting back to your refining but please go easy on yourself and don't overdo it, don't forget we are all messing with dangerous chemicals and reactions that can take some time, so don't start processes if your not feeling up to it, do some gentle tidying and clearing up of your already started processes and get back to your studies on the forum, as we say your values are going nowhere unless you throw them away.
Take it easy and enjoy your time in the lab don't make it a chore and be careful around any processes that involve strong heat and fumes or smoke.
Give the kids a hug from me, wishing you all the best.


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## Oneal58

Hi Everyone and thanks so much. I will give those grand's an extra hug for Everyone tomorrow, I promise. They get many hugs from me everday I see them. But I promise that I will designate one special hug from Everyone here on the forum!
Butcher, I wasn't able to get out this week yet, but hopefully tomorrow I will be able get out a while. It has been raining all day on and off. Also it's been turning colder here so I decided to stay in until it clears up. Weatherman says tomorrow we will see some sun. 
Butcher, all the powders are fine, no lumps at all. The only color is the dark particles of what I think is gold in with the white powders. You remember me telling you about the white substance that was on these pieces of jewelry before I started the refine?. I started to try and clean off this white substance but I was feeling so bad, weak and overwhelmed at the time I just said to myself the Nitric bath should just leave this substance in solution. I really don't know exactly what this white substance is since I have never poured or made any Jewelry? 
Could this possibly be some type of silica or porcelain type material that was possibly formed when the molds were fired during the process of making the Jewelry? I know you can fire clay hot enough for long enough time and you can end up with fine porcelain, even glass like material.
Anyway, I will get on with following your directions hopefully tomorrow, second guessing doesn't get anything done. Thank you so much Butcher for your help. I will let you know as soon as I find out something. 
Thanks,
Oneal


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## nickvc

Oneal I think I can help here if the white powder was on the castings and on the casting sprues it's almost certainly investment powder from the casting cans, it's what they use to burn out the waxes and leave the shapes to be filled with metal.


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## niteliteone

Has anyone heard from Oneal58 since his last post on this thread ???


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## maynman1751

niteliteone said:


> Has anyone heard from Oneal58 since his last post on this thread ???




Bump!!?????


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## butcher

I would like to know how my ole friend Oneal is doing also.


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## Palladium




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## Jobmustang

I always do it outside. Stay away from fumes and keep people away. Always use PPE. I use nitric and muriatic filter junk out after 24 hrs. Neutralize with urea. Less chemical waste. I was also told after I could also put baking soda to double neutralize? Anybody else here of this?


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