Old A/P solution. Yellow wash water?

[Charlesncharg]

Got some old Acid peroxide solution. Think it was the first and second times i attempted gold recovery. 1st time went great. Second time i'm quite certain i added to much peroxide. Its been sitting for a few months uncovered. Threw some copper in it to try and push any gold out of solution. Seemed to work well. Started rinsing to get acid out. 1st 2 rinses came out blue. Which i expected. 3rd rinse after sitting overnight is yellowish green and has fine brown powder floating on top. Is the yellow color normal? Is the fine brown powder my gold or possibly rust? Filter it off and put some nitric on it to figure out whether its of value or not?

 

[butcher]

Why nitric?

If you had Copper II chloride with excess oxidizer, just adding copper would cement out any gold and use up the oxidizer, making a browner copper II chloride/ copper I chloride solution, cementing out the gold as a brown to black dirty gold powder.
Yellow solution can be gold in solution, even a slight ring in the upper rim of a green solution can be a slight indications of gold in solution. iron can also make yellow solutions and can be confused as being a gold solution in some instances, here is where testing for gold or iron in solution can be important. See Hokes book for details.

You mention possible iron, if you had iron your CuCl2 solution then it is no longer just a copper chloride solution your mistakenly calling an A P solution. but a combination of Iron and copper chlorides or just iron chloride which will act somewhat differently than just the copper chlorides, it can still be used to recover gold but the techniques for doing so are different.

Iron can be in solution as a green or even yellow solution, and can make red oxides,redish rust looking which are not hardly touched by HCl.

Even after rinsing out acid (your not rinsing out the salts of chlorides), by adding nitric you started another problem to deal with, now you have a form of aqua regia to deal with and its oxidizer which is much stronger and takes more to deal with...

The red rouge iron is also not attacked by aqua regia, although other salts of iron or copper will be along with any possible gold.

 

[Charlesncharg]

I havent added nitric. I am asking for advice before i take any further action. I have read so many posts about people going through the entire process incorrectly and then asking for help. I noticed something i wasnt sure of and stopped. I am a good deal through Hoke's book and understand why i see it in pretty much every post on here. I have taken the old copper chloride solution which did have sold salt like chunks at the bottom along with black powder, put it into a bucket and began rinsing with water to remove any acid or chloride. At the third rinse after it sat over night to settle i came back to a brown powder floating on top of the water and sticking to the sides and the wash water a yellow color. I stopped there andhave been referencing Hoke and asking for advice.I appreciate all the wise words gentlemen. I am a fairly patient person so i've been told. So i have been trying not to jump the gun, any more so, and get myself in a steadily increasing mess before looking for guidence.

 

[Charlesncharg]

I siphoned some out and put it into something transparent and this is what it did after sitting. Picture below.

 

[Topher_osAUrus]

Second time i'm quite certain i added to much peroxide.

Stannous test the solution of questionable value?

 

[butcher]

The copper will displace any gold in solution as long as the solution remains acidic. I do not see any visible sign of gold in solution (the faint yellow ring at the top rim of the solution), a stannous chloride test will tell the tale.
The solution does look like it may contain iron, the color does not look like pure copper chloride, looks more like iron chloride mix, if it is acidic and a clean bar of copper will not cement out anything, and the stannous chloride tests negative for gold let it settle well and decant any settled powders for possible values, filter solution after decanting save filter (it can be incinerated with other powders in later steps, the paper acts as a carbon source and can aid in drying the wet powders during that roasting process).

Adding iron will cement out any copper from the solution, decant the solution from the copper.

Treat the solution for waste, bring the pH to 10 or 11, let the metal hydroxides settle, decant salt solution, and dry the powders for disposal, bring the salt water to pH 7, again let any metal powders settle for drying and waste, the salt water can be disposed of if you have the facilities or dried to salts and disposed of.

Any values will be in powder form after cementing on copper, these can be dried heated to powder and crushed and roasted for further treatment ...

 

[butcher]

The copper will displace any gold in solution as long as the solution remains acidic. I do not see any visible sign of gold in the solution (the faint yellow ring at the top rim of the solution), a stannous chloride test will tell the tale for sure.
The solution does look like it may contain iron, the color does not look like pure copper chloride, looks more like iron chloride mix, if it is acidic and a clean bar of copper will not cement out anything, and the stannous chloride tests negative for gold.

A spray bottle misting water will help to sink anything floating.
Let it settle well overnight and decant the solution from any settled powders, save these for possible values, filter the solution after decanting save filter.

Adding iron will cement out any copper from the solution, decant the solution from the copper.

Treat the solution for waste, bring the pH to 10 or 11, let the metal hydroxides settle, decant salt solution, and dry the powders for disposal, bring the salt water to pH 7, again let any metal powders settle for drying and waste, the salt water can be disposed of if you have the facilities to do so safely, or they can be evaporated and dried to salts for disposal.

Any values will be in powder form after cementing on copper. adding fresh HCl will put any CuCl back into solution as CuCl2 green or brown solution, the gold will not go into solution without the oxidizer.

If you need an oxidizer (dark brown solution), use air bubbled into solution this will not be a strong enough oxidizer to redissolve gold powders but can turn the brown copper chloride back green which will also help to dissolve any copper powders in the mix then you can let solution sit and settle again to see if you have any black powders...

Any gold powders recovered will be dirty and will need refined.

 

[Charlesncharg]

Thank you immensely butcher and everyone else for your guidance. The solution in the pictures was one of 2. The other bucket i have fits your description to the "T" thickish brown syrup lots of black powder at the bottom. I put clean copper in the bucket after eating up some of the copper it started turning black. I have been rinsing the copper off back into the bucket. It has stopped turning black and hasnt dissolved any further. I do not have any stannous chloride ATM. Waiting on the chloride before i proceed. The previous solution did yield some black powder. That i filtered and it is soaking in clean hcl now.

 

[rickbb]

I do not have any stannous chloride ATM. Waiting on the chloride before i proceed.

Take a small piece of 96/4 tin/silver solder and dissolve it in a small bottle of HCL, viola stannous chloride.

 

[Topher_osAUrus]

I do not have any stannous chloride ATM. Waiting on the chloride before i proceed.

Take a small piece of 96/4 tin/silver solder and dissolve it in a small bottle of HCL, viola stannous chloride.

It doesn't even need to be that kind of solder.
Literally anything with tin can be used... Lead tin solder, tin antimony, pewter bowl, tin traces on a pcb... Anything!