HELP! NO GOLD After addition of SMB

[Fariborz Razban]

So here is the issue, I washed the dust like powder I was given by a friend, sth like 60g(the gold is of ore source, probably river, he got it as a payment from somebody and I think the dude has even worked on it with cyanide). first with water, then nitric acid, then added the AR(I went slowly, first HCl then nitric, not much nitric was needed cause as soon as I poured in the HCL it started turning yellow then red was observed and when heat was applied and strong steering(65 C) for 16 hours dark red, I believe it to be super pure since without nitric it was going but I added in total maybe sth less than 30ml(65%) but a lot of HCl was used, sth like 250ml(30%) and 1.5ml of concentrated sulfuric acid(98%) was also added to deal with lead, the entire thing was 320ml on my beaker at the end I applied 120C heat and strong steering with magnetic steerfish for and hour then I let it cool before vacuum filtering it a couple of times over the same filter and washing the filter with distilled water) the damn thing was filtered(I got only silver in my filter paper) and the dark red solution was boiled down to almost half of its original amount, it was blackish red, then I diluted it with distilled water to twice its size(400 ml), which turned it to gold yellow and cooled it to about room temp. then SMB was directly added, first some red foam was observed so I assume my denox wasn't that good, anyway, I kept adding SMB till no brown fume was observed, some dust formed and disappeared before it settles, then the solution turned green, a pale greenish really cloudy solution and no gold, not even a microgram.
I doubled the amount of water, applied heat and kept steering to dissolved the undissolved SMB at the bottom and not much is happening and I'm clue less as to what to do next.
P.S. I added a milliliter of H2O2 and I can see the gold is still there + Stanious test is super positive
P.P.S: despite addition of More water to almost full my 1Lit beaker, there is a lot of SMB at the bottom and some sort of Crystals are forming on top of the solution(very tine and shallow for now).
I was thinking of adding more Hcl to kill the excess SMB maybe and turn it back to yellow then work my way from there again maybe take the NaOH route but I really am scared since in theory I didn't go side track from what I was supposed to get but if I go side track what could I get!!!!
anyway help is urgently required if anyone is kind enough to assist me, I really am clue less, I was thinking of adding some a dilute NaOH solution then H2O2 to let the gold oxide precipitate out and heat it till its pure but I Think I would ruin the whole thing and I know the reaction to be extremely delicate as it can foam like crazy and blow all over the fume hood.

I really would love to know where did I go wrong!!!!! I went by the book for this

update: the solution was neutral, I poured in some HCl and dissolved the remaining SMB in the vessel, the cloud is gone, but the green is still present and no gold still.

 

[Yggdrasil]

So here is the issue, I washed the dust like powder I was given by a friend, sth like 60g. first with water, then nitric acid, then added the AR(I went slowly, first HCl then nitric, not much nitric was needed cause as soon as I poured in the HCL it started turning yellow then red was observed and when heat was applied(60 C) for 16 hours dark red, I believe it to be super pure since without nitric it was going but I added in total maybe sth less than 30ml but a lot of HCl was used, sth like 250ml, the entire thing was 320ml on my beaker at the end I applied 120C heat for and hour then I let it cool before vacuum filtering it a couple of times over the same filter and washing the filter with distilled water) the damn thing was filtered(I got only silver in my filter paper) and the dark red solution was boiled down to almost half of its original amount, it was blackish red, then I diluted it with distilled water to twice its size(400 ml), which turned it to gold yellow and cooled it to about room temp. then smb was added, first some red foam was observed so I assume my denox wasn't that good, anyway, I kept adding smb but no brown was observed, some dust formed and disappeared, then green, a pale greenish cloudy solution and no gold, not even a microgram.
I doubled the amount of water, applied heat to redesolve the unresolved smb at the bottom and I'm clue less as to what to do next.
P.S. I added a milliliter of H2O2 and I can see the gold is still there + Stanious test is super positive
P.P.S: despite addition of More water to almost full my 1Lit beaker, there is a lot of SMB at the bottom and some sort of Crystals are forming on top of the solution(very tine and shallow for now).
I'm so dead, he is gonna kill me.
heap is urgently required if any is kind enough to assist me, I really am clue less, I was thinking of adding some a dilute NaOH solution then H2O2 to let the gold oxide precipitate out and heat it till its pure but I Think I would ruin the whole thing and I know the reaction to be extremely delicate as it can foam like crazy and blow all over the fume hood.

The easiest way out of this is to hang a piece if solid Copper in your solution.
This will cement out anything of value in your solution.
The take the powder/slime from this and redissolve it again with either if these methods.
HCl/Hydrogen-peroxide, HCl/bleach or HCl/pool chlorine.
Make sure the pH do not get too high.
Then there will be no need for deNOxing.
How much Nitric did you use in total?

 

[Fariborz Razban]

The easiest way out of this is to hang a piece if solid Copper in your solution.
This will cement out anything of value in your solution.
The take the powder/slime from this and redissolve it again with either if these methods.
HCl/Hydrogen-peroxide, HCl/bleach or HCl/pool chlorine.
Make sure the pH do not get too high.
Then there will be no need for deNOxing.
How much Nitric did you use in total?

30 ml HNO3 in total, will powder copper work?
I may have some rusty iron wires hanging around, would that work as well?
and what should I keep my ph in those methods? sth around 8 would work or higher?

 

[Fariborz Razban]

30 ml in total, will powder copper work?
and what should I keep my ph in those methods? sth around 8 would work or higher?

I was thinking of filtering this again before doing anything, since there is a layer of SMB or AgCl or both at the bottom, then do whatever I can do, maybe boiling it down again

 

[Golddigger76]

Copper will cement out the precious metals, iron will cement metals below silver so I would find some copper.

 

[Yggdrasil]

30 ml HNO3 in total, will powder copper work?
I may have some rusty iron wires hanging around, would that work as well?
and what should I keep my ph in those methods? sth around 8 would work or higher?

Powder will work, as long as you stir well.
Iron too but the drop will not as separated.

I missed the Cyanide part yesterday, NEVER touch any part of material you suspect has been processed with Cyanide with acid.
Not until after the Cyanide has been properly destroyed, it almost a death wish.

When dissolving Gold with HCl/Bleach do not let the pH get higher than 4.
and when dropping the Gold it should be in the 2-4 range.

30ml of Nitric should be good for somewhere around 30g of pure Gold.
I'm starting to doubt you powder since it started to dissolve in HCl alone.
If this was pure Gold about half would not be dissolved.

There might be less Gold than expected in there.

After you reclaim the powder with Copper, filter it and set aside.
This will contain "all" values.
Take a long talk with your friend and let him know this may take time.
Then set your stuff aside and start studying before you hurt yourself or others.

1. Read C.M. Hokes book on refining jewelers scrap, it gives an easy introduction to the most important chemistry regarding refining.
It is free here on the forum: Screen Readable Copy of Hoke's Book
2. Then read the safety section of the forum: Safety
3. And then read about "Dealing with waste" in the forum: Dealing with Waste

Suggested reading: The Library

Forum rules : https://goldrefiningforum.com/threads/board-policy-this-should-be-read-by-everyone.4646/

 

[Dreamer]

Excuse me for jumping in on the conversation. Yggdrasil, you answerd to the positive about copper powder in this scenerio. Could CuCl2 also be used to isolate values and expidite the solubility? (Forgive me if I violated any forum rules with my question here.)

 

[Yggdrasil]

Excuse me for jumping in on the conversation. Yggdrasil, you answerd to the positive about copper powder in this scenerio. Could CuCl2 also be used to isolate values and expidite the solubility? (Forgive me if I violated any forum rules with my question here.)

No I do not believe that, the CuCl₂ is already an ionic compound so it can not cement out anything.
You need a Metal for that (Valence 0), and Copper is best suited for this purpose.

Edit for spelling

 

[Dreamer]

No I do not believe that, the CuCl2 ia already an ionic compound so it can not cement out anything.
You need a Metal for that (Valence 0), and Copper is best suited for this purpose.

Thank you. Acedemic error on my part. I need a refresher course on electromagnetic ligand selectivity. It's been a few decades since I studied elemental chemistry🙄. I failed to consider the (embarrassingly obvious) affect of the two missing valence e- on its reduction potential.

 

[Shark]

Sth …..?

 

[slsmp40]

So here is the issue, I washed the dust like powder I was given by a friend, sth like 60g(the gold is of ore source, probably river, he got it as a payment from somebody and I think the dude has even worked on it with cyanide). first with water, then nitric acid, then added the AR(I went slowly, first HCl then nitric, not much nitric was needed cause as soon as I poured in the HCL it started turning yellow then red was observed and when heat was applied and strong steering(65 C) for 16 hours dark red, I believe it to be super pure since without nitric it was going but I added in total maybe sth less than 30ml(65%) but a lot of HCl was used, sth like 250ml(30%) and 1.5ml of concentrated sulfuric acid(98%) was also added to deal with lead, the entire thing was 320ml on my beaker at the end I applied 120C heat and strong steering with magnetic steerfish for and hour then I let it cool before vacuum filtering it a couple of times over the same filter and washing the filter with distilled water) the damn thing was filtered(I got only silver in my filter paper) and the dark red solution was boiled down to almost half of its original amount, it was blackish red, then I diluted it with distilled water to twice its size(400 ml), which turned it to gold yellow and cooled it to about room temp. then SMB was directly added, first some red foam was observed so I assume my denox wasn't that good, anyway, I kept adding SMB till no brown fume was observed, some dust formed and disappeared before it settles, then the solution turned green, a pale greenish really cloudy solution and no gold, not even a microgram.
I doubled the amount of water, applied heat and kept steering to dissolved the undissolved SMB at the bottom and not much is happening and I'm clue less as to what to do next.
P.S. I added a milliliter of H2O2 and I can see the gold is still there + Stanious test is super positive
P.P.S: despite addition of More water to almost full my 1Lit beaker, there is a lot of SMB at the bottom and some sort of Crystals are forming on top of the solution(very tine and shallow for now).
I was thinking of adding more Hcl to kill the excess SMB maybe and turn it back to yellow then work my way from there again maybe take the NaOH route but I really am scared since in theory I didn't go side track from what I was supposed to get but if I go side track what could I get!!!!
anyway help is urgently required if anyone is kind enough to assist me, I really am clue less, I was thinking of adding some a dilute NaOH solution then H2O2 to let the gold oxide precipitate out and heat it till its pure but I Think I would ruin the whole thing and I know the reaction to be extremely delicate as it can foam like crazy and blow all over the fume hood.

I really would love to know where did I go wrong!!!!! I went by the book for this

update: the solution was neutral, I poured in some HCl and dissolved the remaining SMB in the vessel, the cloud is gone, but the green is still present and no gold still.

I hate to say this because you have something from a friend and it seems that you are certain that it was gold. Your material is acting like it had a very high iron content.
The one thing that it is not acting like is gold. Hcl will not attack gold without an oxidizer of some sort. You added hcl and the reaction went yellow and then red. It is telling that it went yellow red first. If you have a mix of metals the most reactive will likely react first. Since you didn’t get a secondary coloration with the addition of nitric that means that you started with a copper free product. The green after smb is indicative of iron sulfide. I am trying to figure out how gold could be hiding in your solution, but I don’t see it. Let us know how you make out!

 

[nickton]

Maybe you didn't entirely rinse out the initial nitric acid.

 

[galenrog]

Maybe you didn't entirely rinse out the initial nitric acid.

That is the first thing I would consider.

Time for more coffee.