Refining Gold from Gold Filled Jewelry

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

edit: wow it worked, now if I can remember the instruction my buddy gave on how to do this.
 
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
 
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
discovery1.JPG

crucible1.JPG
 
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 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
 
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} :cry:

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.

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. :p
 
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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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
 
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
 
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
 
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
stump1.JPG

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?
hall1.JPG

hall2.JPG

oysterplate1.JPG


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:
 
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.
 
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
 
"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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