Newbie needs some advise

[butcher]

Thanks Harold, You are right.
I did not know what all he added here, and was trying to cover the bases, both cementing and eliminating nitric, and I wasn't sure of the conditions of his solution, I was actually trying to suggest an overkill to make sure he recovered all his value's and start over, knowing he would also have more base metals in his incenerated powders.
from what I understood he could already have had a thick solution,
maybe I did not read it carefully enough, it sounded like a mess to me mud from other batches, computer electronic parts, possibly plated costume jewelery, I had no idea what base metals and then how thick after crock pot. and all the other chemicals added.
I figured he may have a hard time getting anything to precipitate easily and half way clean.

 

[Harold_V]

In a situation such as you're describing, I think I'd do my best to get things to settle, incinerate, screen, do a dilute nitric wash, rinsing well, incinerate once again, then do a wash with HCl. I never encountered a batch that didn't respond to that kind of treatment, and, in the end, would filter without issues. One must use good judgment, and test along the way, using stannous chloride, to insure that values are not being lost.

Assuming there was considerable waste material, including silver chloride, it might be a good idea to process the entire lot in the furnace, using a good flux, one with a thinner. A reasonable soak interval, plus the use of a collector (if necessary) would eliminate a great deal of the unwanted material. The resulting material is best poured to a cone mold. If there are sulfates present, the introduction of some scrap iron during the heat is a good idea. That liberates any values that may be bound as a sulfide. If that be the case, a center portion of the slag will be present, and look very much like gray cast iron.

It can't be stressed enough, that materials that are to be processed should be clean, and absent unwanted materials. The entire process of refining is eliminating unwanted substances. The earlier they can be eliminated, the easier the process. Which method to use is often dependent on the nature of the material. There is no one way to deal with these things.

Harold

 

[michelemalatesta]

Ok I started over with new materials, I had some computer pins and 14k gold rings. I started with the peroxide and hcl. I did that process twice. I then proceeded with the muriatic acid and subzero. I boiled the solution several times to evaporate the nitric. I then added the precipitate, I used stump out. The solution was an emerald green. A bunch of crystals formed and I now have black in the bottom of the solution with crystals and the solution in a pale green color. Does anyone know what i may have done wrong? And what do you sugest I do from here. I haven't poured any of the solution off yet. This is the 4th time and each time I get a new problem.

 

[Oz]

I did not go back over this thread but it sounds like a gold precipitation from a dirty solution is all, perhaps with too much precipitant. Did you filter your solution before precipitating? I do not know what subzero is but it sounds like you made a home brew AR with it. If so you will have lead and silver chloride sediment based on your source materials.

Test your solution with stannic acid to be sure you have all the gold then you will need to clean up your precipitation. Your black stuff is your gold if you followed a reasonable procedure to get to this point. I do not know what else is in stump out but it may be your crystals or the lead and silver chloride I mentioned if you did not filter first. Buy some clean SMB, it is cheap.

 

[butcher]

Michel,
where do we start?
it is obvious you have not read Hoke's book or much on the forum.
get Hoke's and read.

you started with copper pins (gold plated) any solder?
mixing these with karat gold was not a good idea.

peroxide and HCl will have a hard time doing much good here. as karat golds will hardly be attacked, pins would also have a hard time, unless cut to small pieces and heat and time was involved.

did these dissolve and how?

then you say muriatic and subzero (which I am asumming a nitrate fertilizer), which would make an aqua regia, I would be suprised the karat gold dissolved with out inquarting, (and you have salts as by product of subzero), and then your gold and base metals dissolved together,
the gold and copper, silver mostly chlorides, dissolving gold with base metals in homade aqua regia is not a good idea.
then you added stumpout, what type of stump remover? some more pottasium nitrate or was it sodium metabisulfite?
when did you evaporate off the NOx? the nitric will never let you have your gold as long as it has it dissolved in solution.

first thing I would try is denox, slowly evaporating down to syrup (keep an eye on it so you dont loose the gold in a foam over).
then add HCl to wet, do this three times total the last time add couple drops of sulfuric acid if the pins had solder (to make lead sulfate), add more than three times volume in water to dilute, let silver chloride settle overnight and in morning add a little Hcl to see if more forms, when all settled decant powders, filter solution, check with stannous chloride if possitive try more sodium metibisulfite.
(you also could have gold precipitated with the silver powders ?)

if gold still won't precipitate I would cement values with copper, put them in a jar (these will need reprocessed later). set jar in safe place, and get out hokes book and read it before I lost all my money and gold, get the understanding under your belt first, start with small expieriments, learn one process at a time. come on now you can do this, don't just jump into it without study, (if you do you might as well take your gold and put it back into the river, were some other miner has a chance of finding it, because processing gold without an understanding it you will lose it anyway. good luck & get Hokes and a cup of coffee.

 

[michelemalatesta]

I filtered the solution 3 times with coffee filters and then twice with filter paper. I may have used to much stump out. I read on here that stump out is metabysulfate, if I spelled that right. I will check in the morning to see if there is any gold left in the solution. The solution has a very strong odor.

If there is no gold in the solution do you suggest I pour it off?
how do I separate the crystals from the black sediment?
Do I need to start over?
How do I know what the pale green solution is? I'm asking because I need to know how to properly dispose of it when i'm done.

Thank you for your reply.
Michele

 

[butcher]

dilute see if crystals dissolve may be salt, green is probably copper chloride,maybe some nickel, test all solutions with stannous chloride, to see if gold dissolved in solution,
only one brand of stump remover is sodium metabisulfite, also called pyrosulfite, Bonide brand I believe,

after all gold out of solution Iron will dissplace metals below it in series, then a base will neutralize solution, read up on dealing with waste,

the most important thing you need, is to read up on processing.
we need to learn to walk before we run., reading will remove the blindfolds you have tied around your eyes, and then you will be able to see, these trees you keep bumping into while you are running through this forest.

 

[michelemalatesta]

Thank you for your replies, I did read hokes, watched videos bought and watched steves dvd on pgms. Ive been so concerned with the chemical process and making sure I use the correct amout of each chemical that I havent been paying much attention to the other part of the process, the metals.

I did heat the solution when I did the muriatic acid and peroxide. I did that process several times thinking that the heated process would get rid of all the base metals.

I then moved to the aqua regia process and when I did that, there were very few pins left. The rings were all still in tact, I did hammer them before I started and they were very thin and flat. This process was also heated several times. I did this whole process over 3 days. All the metals were dissolved.

I then went on to filter, several times.

I do think I added to much stump out, which is bonide, i got it off the chemical substitude list.

Thank you for your patients, it may be taking me a little longer to understand this whole process...there is alot to learn.

Michele

 

[butcher]

you'll get it, there is alot to learn, reading Harolds posts, and Hokes, one day the light will come on and will just blind you, from the reflection of your gold bar.

 

[Harold_V]

I noticed a comment that may be a serious part of your problem. You said "I did heat the solution when I did the muriatic acid and peroxide. I did that process several times thinking that the heated process would get rid of all the base metals."

Red flag time.

Is it safe to assume that what you are saying is that you repeated the process, decanting the base metal solutions each time? Please tell me you didn't evaporate the solution time and again without discarding the dissolved base metals.

When you undertake this operation, it's very important that you test the solution with stannous chloride, to insure you are not discarding any values.

As far as base metals go, the purpose in dissolving them is to eliminate them. Before you put any of the values in solution, the base metal solutions should be decanted, with the remaining solids rinsed well a few times to remove all residual traces. Tap water is perfectly acceptable for the rinse operation, assuming it is fit for culinary purposes. You may be told time and again that you must use distilled water, but I refined for better than 20 years and never used distilled water in my gold refining processes. My quality was superb.

Harold

 

[michelemalatesta]

Hi Harold,

I did rinse the remaining metals before going to the next step, I also tested the solution as well. I also saved all of my solutions. (just in case) I did learn something that I read and saving the solutions keeps sticking in my head at least until I have a solid understanding of what I am doing. I have a cooler full of them. Thank you for your concern. I havent thrown anything out yet....waiting for the perfect time and the way i'm going it may be later than sooner. That was also stressed in the book as well.

I will be working on all of your much appreciated suggestions in the morning and I will keep you posted on what I have.

Thank you again
Michele

 

[Harold_V]

I will be working on all of your much appreciated suggestions in the morning and I will keep you posted on what I have.

I'll keep watch, and offer suggestions if you'd like.

Harold

 

[michelemalatesta]

Ok, I checked the solution and it still tests for gold. The test turns a light brown. I turned the heat on as you suggested. I'm going to let it heat for a while. I'm not sure if you understood that I did not decant any of the solution. This is what I have. I have a black substance in the bottom covered by a white substance and the solution on top is a light greenish blue.

My plan is to let it heat up for a while and then add a little hcl? Then let the solutin evaporate and add more hcl? Then let it settle and add some smb to see if I can retrieve the rest of the gold.

If I understand correctly, the black on the bottom is gold and the white is silver?

When I am sure that all of the gold is out of the solution with the test, I am going to decant and then heat up the black and white substance on the bottom adding a little hcl?

Then I will need to hit it with a torch to bring the metals to a solid and start over?

Let me know how I did?

Thanks guys, This forumn has been very helpful and it is very generous of you all to share your knowledge.

Michele

 

[butcher]

Harold will also help here.
don't let my help get in the way of his, as Harold advise would be best. being patient and waiting for his help would also be a good idea.
don't use torch yet!
you possibly have base metals in solution with gold.
and metal powders in bottom possible gold,silver, base metals.
I would decant what has precipitated thus far, wash it for retreatment, adding wash solutions together,after a wash using Harolds instruction,( later these powders can be re-treated with HCl/bleach, it is easier to rid oxidizer, lead and silver can be filtered out in this process, wait before treating them Harold may have another suggestion).
solution, that tested positive for gold. which may still contain oxidizer, using the evaporation process to rid possible oxidizer.
Harolds trick if you have a little piece of gold to add, it can help use up any nitric that may be left in this solution,this can save time and amount of evaporations needed.
I would also keep forum posted of steps taken and wait for more help before going further with other steps.

 

[michelemalatesta]

This is what I did,

I let it sit today on heat, not a boil, I was afraid of boiling off my precious metals. I checked the solutin and after the test it did not show any gold. I decanted off the solution and let the mud at the bottom heat a little to get rid of excess acid. I added some hcl and let it heat a little again. I have brown mud in the bottom. I'm going to let that sit for the night and then rinse the mud in the morning as Harold suggested. If you think I missed something please feel free to let me know.

Thanks again
Michele

 

[Harold_V]

This is what I did,

I let it sit today on heat, not a boil, I was afraid of boiling off my precious metals. I checked the solutin and after the test it did not show any gold. I decanted off the solution and let the mud at the bottom heat a little to get rid of excess acid. I added some hcl and let it heat a little again. I have brown mud in the bottom. I'm going to let that sit for the night and then rinse the mud in the morning as Harold suggested. If you think I missed something please feel free to let me know.

Thanks again
Michele

Assuming you have recovered all of the values, the next step, even if you intend to re-refine the yield, is to wash the resulting powder. I recommend you do that at a full boil, so the agitation keeps the material moving. Your objective is to eliminate traces of dissolved base metals that don't readily leave the material. I expect you have a beaker and a watch glass. Use HCl and tap water for the wash cycles. Boil the material for several minutes, than add more water, to cool and dilute the solution. Allow to settle, then decant. Make sure that you have clear solution (it may be colored, but there should be NO gold in suspension). If the gold is quite dirty, which I expect to be the case, the gold may not settle quickly. Rinse once with tap water, bringing the material to a boil once again. After a brief boil, fill the container with tap water, stir, then allow to settle. Decant (siphoning using a 3/8" vinyl hose works very well. You can control the speed of discharge by varying the height of the discharge end. As long as it is below the intake, it will flow, faster as you lower the discharge end). Now repeat the wash operation, using ammonium hydroxide. This is an important step, for it will eliminate any traces of silver that may have hitched a ride as silver chloride, plus it will help eliminate traces of copper. Boil hard, take up with water, stir, and allow to settle. Decant, rinse with water once again, then repeat the HCl wash and rinse cycles. Sounds like a lot of work, but it's routine and will improve the quality of your gold immensely.

If, after you have completed the wash and rinse cycles, the color of your gold is still quite dark, I highly recommend you re-refine. If you feel you'd like to do that, maybe you can post a question in that regard. Unless you are satisfied with the end result, you should not melt the powder. It's very easy to re-dissolve precipitated gold for re-refining, so it should remain as a powder for convenience.

Luck.

Harold

 

[glorycloud]

What great moderators and mentors we have here!

Let's not take them for granted!! 8)

 

[michelemalatesta]

I agree glorycloud...I appreciate all of the help and support here...I hope one day I will be able to return the generosity.

Harold, I will do as you advised. I first have to go purhase a new burner...Mine gave out on me. I will keep you posted.

Thank you again )
Michele

 

[michelemalatesta]

Hi Harold,

You said that the wash with ammonium hydroxide is very important, can I use 3% ammonia? I cant seem to find ammonium hydroxide.

Thank you Michele

 

[Harold_V]

Use what ever you can find, although I think I'd recommend against using anything scented. I used to buy it in plastic gallons from a chemcial distributor. Don't recall the concentration.
That which comes from the local grocery store should be acceptable.

Harold