Need help with brown "ice"

[TJ607]

Hello all, a year ago I tried my first and only gold recovery attempt. I dissolved the gold plated copper tracings, fingers and 600g of heavily plated (tested at 22k) pins from a 1965 computer. I added MB until I ran out and stopped.
Fast forward a year and I realized I made a mess. Too much nitric. Overpowering smell. I bought Sulfamic acid to de-nox, then I read the posts to cement out the values with clean copper bars.
What you see is 2 weeks of 2000ml of dark liquid that had no particulates after 2 copper bars were submerged.
I did not heat or agitate the liquid or de-nox. I decided to filter the liquid and I found these salts that I thought were ice. I dissolved a small piece in water with no problem. It turned light brown.
My year old stannous chloride solution showed no color change. I bought 2oz of powder and mixed it 1.5g/ml. I put a smudge of the brown mud from the filter on a Q-tip and a drop of SC and the brown dissapeared completely. Same with the filtered solution. The 2 copper bars were clean when I pulled them out a week ago. The oxidation occured after.
I dont know where to go from here.
I have nitric, sulfamic, MB. I would like not to spend any more money.
Although you have heard this a thousands times, there is a lot of gold here, I just dont know where.
Thanks for any help.
TJ

 

[FrugalRefiner]

Since the solution tested negative with your fresh stannous chloride, it is reasonable to assume any gold is with the solids.

Since the solids, or at least part of them, are soluble in water, I would start with that. Add water to the solids, stir, and get everything that will dissolve in water to dissolve. Decant and/or filter that solution off and see if there is anything left that does not dissolve. Repeat if necessary.

Let us know what happens and we'll take it from there.

Don't throw anything away till we find your gold.

Dave

 

[eaglekeeper]

Hard to tell from that picture....If that's a stainless steel bowl, it will cement out any base metals and PM's that's in that solution/crystals. So collect any residues that are on inside of that bowl.

My guess on the crystals is from the SMB/sulfamic acid that crashed out of solution.

I'm assuming MB, you mean SMB...?

 

[TJ607]

Yes SMB. I didn't add any sulfamic acid yet. The bowls are clear pyrex.
I dissolved, rinsed and repeated with room temperature filtered rain water. I ended up with coffee grounds (last pic) and lots of fine brown sludge. The filtered water from yesterday is still very dark and acidic smelling. The brown sediment is in all the beaker bottoms also.
The filters are from yesterday as is the dry powder from a filter.
No color on dark or brown sediment when tested with SC. I ordered another pre-mixed bottle.
Any ideas as to whats next?
Thanks, TJ

 

[Yggdrasil]

Yes SMB. I didn't add any sulfamic acid yet. The bowls are clear pyrex.
I dissolved, rinsed and repeated with room temperature filtered rain water. I ended up with coffee grounds (last pic) and lots of fine brown sludge. The filtered water from yesterday is still very dark and acidic smelling. The brown View attachment 52797View attachment 52798View attachment 52799View attachment 52800View attachment 52801sediment is in all the beaker bottoms also.
The filters are from yesterday as is the dry powder from a filter.
No color on dark or brown sediment when tested with SC. I ordered another pre-mixed bottle.
Any ideas as to whats next?
Thanks, TJ

Stannos can only be used on solutions, not solids.

 

[TJ607]

I am confident that there is no gold left in the solution, as Frugalrefiner has said.
The last filtered solution from the redesolved brown ice, left me a large glob of brown sediment and the dark grounds.
Since i didnt add any additional SMB and only cemented with copper, is this brown sediment on the filters gold?

 

[TJ607]

 

[FrugalRefiner]

No color on dark or brown sediment when tested with SC. I ordered another pre-mixed bottle.
Any ideas as to whats next?

As Yggdrasil said, stannous is used to test for gold in solution. It does not work on solids.

Take a small sample of your sludge or the dried powder, dissolve it in a tiny amount of HCl and either bleack or hydrogen peroxide. Warm it for a while to drive off any excess oxidizer. Then thest the resulting solution with stannous.

You really need to download and read the book in my signature line. It explains how to use stannous chloride, along with a great deal about refining. It will answer many of the questions you'll have in the future.

Dave

 

[eaglekeeper]

I would collect all the solids and put them in a beaker.....filters also. Add Hcl and heat.... then add nitric acid 1 Mil at a time. Wait for the reaction to stop then add 1 more Mil, continue those additions until you get no reaction after adding nitric acid.

Stop the additions of nitric if there is no reaction......even if you see a little solids at the bottom. Test the solution with stannous to confirm if there is PM's in solution. If so, filter off any solids and drop with SMB.
As far as any solids still left over, you can always AR those again later. I just don't want you to over shoot the nitric franticly trying to dissolve worthless solids.

You could AR the brown stuff and black stuff separately if you want too.

 

[TJ607]

I tried the suggested tests.
Heated a small amount of hcl and bleach with a small amount of dried filter sediment. No color on sc test.
Secondly, I heated 50ml of hcl to 150F with a pea sized piece of filter sediment. Immediately turned yellow-green. Added nitric drop by drop. Slight reaction. Tested on coffee filter. Blackish brown color.
Interestingly, I put some heated solution in a bowl and added 1 drop of sc. Turned ink black on both test liquid samples. Was this a positive sign?

 

[Yggdrasil]

I tried the suggested tests.
Heated a small amount of hcl and bleach with a small amount of dried filter sediment. No color on sc test.
Secondly, I heated 50ml of hcl to 150F with a pea sized piece of filter sediment. Immediately turned yellow-green. Added nitric drop by drop. Slight reaction. Tested on coffee filter. Blackish brown color.
Interestingly, I put some heated solution in a bowl and added 1 drop of sc. Turned ink black on both test liquid samples. Was this a positive sign?View attachment 52827

So what happened when you heated with HCl bleach (This should not be heated due to loss of Chlorine which is the oxidizer.)
Did it all dissolve?
When you heated the pea sized sediment in HCl what happened besides becoming yellowish green?
Did it all dissolve?

 

[TJ607]

Yes. I was told to heat it to drive off any excess oxidizer. Both dissolved very quickly.

 

[Yggdrasil]

Yes. I was told to heat it to drive off any excess oxidizer. Both dissolved very quickly.

That is correct but not until all has dissolved.

What puzzles me is that you added Nitric to the heated HCl, and that was why I asked.
If the HCl dissolved all, there is no need for Nitric.
Next, if the Stannous is blackish in color, dilute the solution and test again until it is less black.
If there is Gold in solution there should be a beautiful Purple/Violet color.

 

[TJ607]

Well, after many mistakes and mishaps, I found my gold.