Solution still light brown after drop

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Alliedft

Active member
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Mar 1, 2020
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27
I am new to refining. I used ap for foils, dissolved with acid/bleach, heated slightly and let sit over night. The solution was clear and yellow, after I added I tsp dissolved smb I got a drop after 1-2 minutes, I allowed to settle 8 hours and solution is still light brown. I have checked with stannous and no gold is in solution so I filtered and refined 2 more times. Solution is still staying slightly brown. What would help to clear it up so I can get all the gold down to drain. Please help. Thanks
 
How much gold was in solution? If it was only a very small amount it may take time to settle. I would start by stirring it. Be carefully as gold powders seem to stick to everything. It may be the off gassing of the SMB that is keeping your powders suspended. A picture would be helpful.
 
I'm guessing maybe half a gram or a little better. It may be the gasses because I'm sure I used excessive smb for what I was planning on recovering. Would it help to heat the solution to help drive off the excess gas
 
I have added pictures of the before, after adding and then after sitting 6-8 hours
 

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I know those vases very well. I even use a few still for settling just such powders.

I will start by saying I don't like chlorine, bleach seems to drop very fine particles for me. I would guess that those slow settling powders are dirty, and will settle very slowly. What I do when I reach that point is pour off those into another container, and leave it to settle for how ever long it takes to clear it up. The heavier, faster settling powders are then ready to be washed, if you want higher quality gold. If not, you can melt them as is once dried. You could have reduced the volume before dropping the gold by low heat and letting some of the water steam off. Do not boil it, you will send gold up with the steam. Reducing the volume can aid a cleaner drop. Once the slow stuff settles, I decant off the clear stuff and leave those powders to sit. Next time I process more gold, I will add to those fluffy powders until I have a fair bit of them, then process them and collect what is there. If the gold belongs to someone else, I will process them sooner, so I can give a better return on the expected amount.
 
I thought this from butcher would fit well here, taken from this thread..https://goldrefiningforum.com/phpBB3/viewtopic.php?f=49&t=28744#p302988

The gold precipitant particle size will depend more on how easily the newly reduced gold atoms can come into contact with each other to form clumps of gold atoms heavy enough to sink to the bottom as they overcome the resistance of the solution to gravity.

precipitated gold is normally tan to brownish if precipitated from a solution loaded with base metals the gold is usually dark brown to black.

The color of the solution should be fairly clear after precipitating gold from a fairly pure gold chloride solution, when base metals like copper and some other metals are involved they can leave some color to the solution after precipitation.

GSP once said that the color of that solution at the very top, in the third picture, is an indicator that all the gold dropped from solution. When everything is near perfect, it will precipitate and settle in under one minute.
 
I cant get a clear picture inside solution but it is extremely fine particles. I think it is stating to settle more as I can watch them slowly falling with a back light. I'll leave it sit overnight and see how it looks in the am. Thank you for your help
 
I will try nitric on next drop and see if they drop better. I just used chlorine to save on nitric. Most of my nitric gets used for silver.
 
Yep, sometimes nitric cost is prohibitive. I think your doing pretty good, just give it time to clear. As I mentioned, that clear streak at the top is a pretty good sign.
 
Heating your solution can help speed up the settling process but make sure to use proper lab glass.
 
Yeah I didnt wanna take a chance trying to heat this vase, I only use for cementing silver usually, but it finally cleared up this morning and was able to decant and boil in hydrochloric and rinse and dry. I was actually surprised I ended with 1.93 grams total but it is very fine.
 
Based on the volume of powders in the picture, I thought it might be more than you expected. To heat those vases you can use a coffee maker hotplate, I use a handsaw and cut the upper portion off and keep water out of the bottom. Even then, only fill it 1/2 to 3/4 full as that is a tall, narrow cylinder and heat doesn't move up well through them with such low heat. In a pinch, you can heat a glass coffee pot in a Corningware pyrocyram dish, the vases will break pretty easy this way though.

Looking good!
 
It definately was. Now I have another question. After cleaning my stockpots and refining them I put this solution in a fresh clean stockpot with a new bright copper bar today I opened it to add some more solution and noticed more has dropped out of this solution than did with smb. Mainly brown precipitate. Would it be worth refining again to check or just wait till full again. It's a 5 gallon bucket with bubbler. Next question is what else would drop from solution with copper other than silver. Also why would their be gold in there if I got 2 negatives with stannous, 1 about 1 hour after drop and one the next day.
 
Copper will drop the PGM's (platinum group metals) as well. Not knowing exactly what all is in the stock pot, PGM's could be a possibility. If your stannous test showed a brown color, it could have been a false positive from excess SMB in the solution. You could take a small sample and put it into some AR and test it again. How do you do your stannous test, spot plate, q-tip, paper strip? If it is PGMs, a spot plate might give an easier to see coloration.
 
This was all from fingers and a few cell boards and sattelite lnb boards processed in ap. Stannous test was clear with no change at all on filter paper strip. What has dropped out is brown like gold not a black. I made the stannous solution and maybe I need to throw it away and start over with it, evidently I messed something up. Because all that is in the bucket is the clear solution after the drop and the rinses and boils.
 
Instead of throwing solution away...Take a plastic spoon and put a foil in it. Then a couple drops of hcl and a drop of bleach. Test it with said stannous that is already made.

How was the previous solutions decanted? We're they filtered or just clear to the naked eye and poured off. (Finest of powders can flow right through the filter too) Since the powder was so fine to begin with..the remaining particles could have had to become the whole gestalt to be more visible to the eye.
 
I took a pipette and gathered a small amount and dissolved and I get a strong positive for gold. It was filtered with a slow filter and several pour offs just by eye when settled. I agree with it being so fine I knew I would have a little loss but there is literally more in the bucket than I collected. And the solution and rinse water sat in a jar for a day while I processed old stock pot and made a new one with new copper, during the time it was in the jar th err re was no color once I added to copper it dropped out.
 
I would add any remaining used AR first. Might as well process all of it instead of repeating it over and over. Then allow everything to settle out, collect those powders then re run a sample in AR. Then from the drop use a vase to let the remaining solution settle more. Decant any remaining powders, then while in the vase add a piece of copper and see what happens. If you get more gold, then your missing a step somewhere.

This is how I do it when I run into a problem. It helps me find where my problem is and eliminate it. By testing at every step it allows you to identify possible PGM contamination as well.

Take a test sample from your stock pot, wash with hot water until the water remains clear and any acid is gone. PH tests will give your a confident answer if unsure of remaining acids. While testing like this I use good quality distilled water. Twice I have found tap water to be my problem.

1. Put everything into solution using minimal amounts of nitric/bleach and hydrochloric
test

2. Denox, eliminating any remaining nitric/chlorine
test

3. Add a few ml of sulfuric acid, helps remove any lead (may not be needed but I always use it just in case)
test

4. Add distilled water to raise the volume by 75%, allows potential silver to drop out as a chloride.
test

5. Filter until absolutely clear, remove anything that isn't dissolved. Check that filter close, any metals could be cementing some of your gold.
test

6. Drop your gold and allow to fully settle
test

7. Decant into another container (I prefer glass so I can see what is happening here), not your stock pot yet, then use copper to see if anything drops at this point.
test



At each step if your test isn't as expected, then you can identify possible problem areas and work towards fixing them. It isn't a perfect method, but it will greatly help towards identifying problem areas.
 

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