Aqua regia gold stuck in solution electrolysis

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You may already be aware of this testing method but if not give it a try.
I have problems reading the spoon or dish test myself.

If you will use a cotton swab to stannous test it will show your results a lot clearer.
Put a drop of stannous where the cotton meets the stick, then dip the tip of the cotton swab in your solution.
Where the solution and stannous meet up on the swab makes a very clear and distinct line that will show you if you have gold, platinum or platinum.
To avoid getting stannous in your solution, I would swap those two. Dip the tip in the solution and then dip it in a drop of stannous.
 
You may already be aware of this testing method but if not give it a try.
I have problems reading the spoon or dish test myself.

If you will use a cotton swab to stannous test it will show your results a lot clearer.
Put a drop of stannous where the cotton meets the stick, then dip the tip of the cotton swab in your solution.
Where the solution and stannous meet up on the swab makes a very clear and distinct line that will show you if you have gold, platinum or platinum.
I used 1 kilo of crushed ore, 200ml of nitric, 800ml of HCL
yes it was high grade ore that I visually confirmed had gold. from a existing mine that already extracts gold.
its too late now to use the stannous method as the solution has been basified but thanks alot for that suggestion. Ill do that next time instead of my cup method which is very wasteful.
my current plan is to completely basify with baking soda, boil off dry. and do a fire assay.
 
Forgot to attach pictures of ore. this is a piece I found while hammering that had gold. Picture quality doesnt show it well enough
PXL_20231023_200730562.jpg
 
I used 1 kilo of crushed ore, 200ml of nitric, 800ml of HCL
yes it was high grade ore that I visually confirmed had gold. from a existing mine that already extracts gold.
its too late now to use the stannous method as the solution has been basified but thanks alot for that suggestion. Ill do that next time instead of my cup method which is very wasteful.
my current plan is to completely basify with baking soda, boil off dry. and do a fire assay.
So basically you do not need to assay, you have a known ore containing gold, but want to try another extraction process?
AR is often recommended NOT to do on ore. Because of possible cyanide, arsenic, mercury, etc. becoming dangerous when treating with AR.
 
So basically you do not need to assay, you have a known ore containing gold, but want to try another extraction process?
AR is often recommended NOT to do on ore. Because of possible cyanide, arsenic, mercury, etc. becoming dangerous when treating with AR.
correct ill be doing another extraction process. Sodium chlorate leaching. I mistakenly rushed things by going through AR. My intentions coming to this forum wasnt to be gaslit that my ph strips are expired and that im just experiencing gold fever. The amount of personal attacks here especially by the admins is ridiculous. I simply wanted to share a interesting experience and maybe if someone else had a theory why the gold would redissolve in electrolysis once the amperage spiked up, and why SMB neutralized the solution. share my failures so others can learn (as I find limited information on ore electrolosis) and some suggestion on how I can recover the mess I made. currently my plan is to boil it down dry and do a fire assay.

I also still plan on repeating this exercise on a smaller scale and properly documenting it so I can determine what caused the issue. If it was cause of the iron electrode, solution heating up, or something else. Experimenting and trying new things staying positive instead of attacking someone's "glassware" even though im sure I have more proper labatory glassware than most people here. I simply enjoy using glass jars* for mixing as they are cheap and plentiful.
 
When you ran the cell the cathode accumulated what you suspect to be gold. Could you simply scrape a small amount of the deposit into a beaker and add a small amount of aqua regia. Then test with stannous?

Let’s confirm you actually deposited Gold before we go chasing ghosts.
 
Having just re-read the entire thread on a laptop instead of a phone, I noticed one thing you did not mention. And it would be obvious. If the precipitate that sloughed off your anode in the first video was gold, when you added additional Nitric Acid you should have seen a red fume. It is quite obvious and if you are not working in a hood even more obvious. If the original precipitate was gold you would have generated NOx as it re-dissolved. Did you see the red cloud?
 
correct ill be doing another extraction process. Sodium chlorate leaching. I mistakenly rushed things by going through AR. My intentions coming to this forum wasnt to be gaslit that my ph strips are expired and that im just experiencing gold fever. The amount of personal attacks here especially by the admins is ridiculous. I simply wanted to share a interesting experience and maybe if someone else had a theory why the gold would redissolve in electrolysis once the amperage spiked up, and why SMB neutralized the solution. share my failures so others can learn (as I find limited information on ore electrolosis) and some suggestion on how I can recover the mess I made. currently my plan is to boil it down dry and do a fire assay.

I also still plan on repeating this exercise on a smaller scale and properly documenting it so I can determine what caused the issue. If it was cause of the iron electrode, solution heating up, or something else. Experimenting and trying new things staying positive instead of attacking someone's "glassware" even though im sure I have more proper labatory glassware than most people here. I simply enjoy using glass jars* for mixing as they are cheap and plentiful.
The only viable leaches for ore is either Cyanide based or Hypochlorite based.
And only after a proper assay so one knows what else is in the mix, Arsenic, Cadmium, Mercury or other nasties.
Going from one bad process to another will not change much, if AR did not get it, Chlorate will not either.
 
Having just re-read the entire thread on a laptop instead of a phone, I noticed one thing you did not mention. And it would be obvious. If the precipitate that sloughed off your anode in the first video was gold, when you added additional Nitric Acid you should have seen a red fume. It is quite obvious and if you are not working in a hood even more obvious. If the original precipitate was gold you would have generated NOx as it re-dissolved. Did you see the red cloud?
I did not see any red cloud I can confidently confirm that. Im working on getting a stannous chloride test on some leftover gold on the anode electrode that you suggested earlier.
 
The lack of the red cloud eliminates any appreciable metallic iron, copper, or Gold as all result in the red-brown nitrogen dioxide cloud.

My refining career has always involved concentrates of all of the precious metals, so my first inkling, when you mentioned 1 kg of material was a substantial precipitate or deposition in this case. But this was ore, which focuses my attention to Kurts question
So - how much gold were you expecting to recover from your kilo of ore ?
From a kilo of any typical ore, a single gram per kilo would be the find of a lifetime. Your photo’s show deposits greatly in excess of what should be contained in a kilo of ore.
 
correct ill be doing another extraction process. Sodium chlorate leaching. I mistakenly rushed things by going through AR. My intentions coming to this forum wasnt to be gaslit that my ph strips are expired and that im just experiencing gold fever. The amount of personal attacks here especially by the admins is ridiculous. I simply wanted to share a interesting experience and maybe if someone else had a theory why the gold would redissolve in electrolysis once the amperage spiked up, and why SMB neutralized the solution. share my failures so others can learn (as I find limited information on ore electrolosis) and some suggestion on how I can recover the mess I made. currently my plan is to boil it down dry and do a fire assay.

I also still plan on repeating this exercise on a smaller scale and properly documenting it so I can determine what caused the issue. If it was cause of the iron electrode, solution heating up, or something else. Experimenting and trying new things staying positive instead of attacking someone's "glassware" even though im sure I have more proper labatory glassware than most people here. I simply enjoy using glass jars* for mixing as they are cheap and plentiful.
If you treat kilo of ore with AR, and assuming that you leached the gold out, there comes the question - how much of the gold could actually be there ?
Regular ores yield below 1ozt/ton, that means one kilo of ore will contain at best 30 mg of gold. IF you leached all of it, say with 1L of AR, now you have solution of 0,03gAu per liter. And here comes the problem - in this low concentration, stannous will usually show nothing.

Cementation should give you some precipitate to work with. Only if you dissolve this precipitate in AR once again and test this solution with stannous, you will obtain relatively reliable result.

BTW, what is approximate purity of the gold in the ore ? I am asking because if you have high silver content in it (say 60-70% Au, rest silver), dissolution in dilute AR would be very slow and leaching efficiency minimal.
Acids on rocks isn´t a good technique. If there is freemill gold in the ore, there is no point in acid treatment. It is dangerous and wasteful, inefficient, simultaneously creating much more hazardous waste than mechanical separations.
 
The lack of the red cloud eliminates any appreciable metallic iron, copper, or Gold as all result in the red-brown nitrogen dioxide cloud.

My refining career has always involved concentrates of all of the precious metals, so my first inkling, when you mentioned 1 kg of material was a substantial precipitate or deposition in this case. But this was ore, which focuses my attention to Kurts question

From a kilo of any typical ore, a single gram per kilo would be the find of a lifetime. Your photo’s show deposits greatly in excess of what should be contained in a kilo of ore.
its concentrated picked out ore. Not just excavated rocks
 
its concentrated picked out ore. Not just excavated rocks
So it is the equivalent of hard rock mining where the vein is chiseled out to get the good stuff. That is plausible. But if you took the time to mill it to a powder, why didn't you pan off the overburden and keep the heavy pieces for your digestion. I think that at least part of the problem here is salts of the minerals you put into solution.
 
If you treat kilo of ore with AR, and assuming that you leached the gold out, there comes the question - how much of the gold could actually be there ?
Regular ores yield below 1ozt/ton, that means one kilo of ore will contain at best 30 mg of gold. IF you leached all of it, say with 1L of AR, now you have solution of 0,03gAu per liter. And here comes the problem - in this low concentration, stannous will usually show nothing.

Cementation should give you some precipitate to work with. Only if you dissolve this precipitate in AR once again and test this solution with stannous, you will obtain relatively reliable result.

BTW, what is approximate purity of the gold in the ore ? I am asking because if you have high silver content in it (say 60-70% Au, rest silver), dissolution in dilute AR would be very slow and leaching efficiency minimal.
Acids on rocks isn´t a good technique. If there is freemill gold in the ore, there is no point in acid treatment. It is dangerous and wasteful, inefficient, simultaneously creating much more hazardous waste than mechanical separations.
freemilling ore is wasteful. heres a fun stastistic. over 75% of all gold mined is done via leaching
another fun statistic. mercury amalgamation only is 10-20% efficient. aka up to 90% of the gold is not extracted.
most miners are losing most of there ore. However im not here to argue how concentrated my ore is or what method is best. Your favorite method is your opinion. im simply here to discuss about electrolysis and a interesting phenomenon I discovered. I dont see any benefit in hearing people gaslight me into what I already know and seen.
 
So it is the equivalent of hard rock mining where the vein is chiseled out to get the good stuff. That is plausible. But if you took the time to mill it to a powder, why didn't you pan off the overburden and keep the heavy pieces for your digestion. I think that at least part of the problem here is salts of the minerals you put into solution.
Please read above comment. I have my theory and reason to believe thats a ineffective way of doing things. Again im not here to debate why I did things a certain way. I agree there were certain mistakes I did, the way i properly wanted to do it is completely different. But im trying to get information related to electrolysis and chemistry involved in it. Why gold dissolved and amps shot up and why SMB neutralized the solution. Two very weird phenomena that ive never seen before
 
I feel like ive had to answer far more questions about my personal stuff and the reasoning on what im working with rather than the actual topic at hand... I understand theres amatures and people who make very dumb mistakes. and I agree I am a amature to you all. However arguing to prove something I know is factually true is just a waste of everyone's time
 
Well you said you selected the pieces that looked promising visually. We can go back and forth all day here and prove nothing. What we want to determine is if there is gold in your sample and if there is how much. Typically that is done by fire assay but you have ruled that out. A lot of refiners who have been around the block have commented here but it is you who said this;
I dont see any benefit in hearing people gaslight me into what I already know and seen.
All we are asking you is to say how you already know it without a fire assay. A lot of preliminary signs, like no NOx emitted and as yet no positive stannous test, dispute what you already know. Please show us how you know it without thinking we are gaslighting you. You may have stumbled on a revolutionary new process so let's see if it's real or if you are gaslighting us.
 
Well you said you selected the pieces that looked promising visually. We can go back and forth all day here and prove nothing. What we want to determine is if there is gold in your sample and if there is how much. Typically that is done by fire assay but you have ruled that out. A lot of refiners who have been around the block have commented here but it is you who said this;

All we are asking you is to say how you already know it without a fire assay. A lot of preliminary signs, like no NOx emitted and as yet no positive stannous test, dispute what you already know. Please show us how you know it without thinking we are gaslighting you. You may have stumbled on a revolutionary new process so let's see if it's real or if you are gaslighting us.
I am going to do a fire assay! im working on that currently. I mentioned that I wanted to boil down the solution dry and do that.
no nox emmition only occured after electrolosis and gold redissolved. I saw nox emissions when I initially was dissolving the material. The reasons I believe there is gold because I saw it in the ore. I saw it precipitate out. and I saw it in the stannous chloride test which in my opinion looks very similar to many other tests other people conduct on aqua regia on impure gold solution.
I think there was some miscommunication between us. I dont view you as gaslighting, you have been more than helpful and so have a few other users. But many others especially those who orginally commented have not. Being told my ph test strips are expired I know is simply factually wrong for example
 
freemilling ore is wasteful. heres a fun stastistic. over 75% of all gold mined is done via leaching
another fun statistic. mercury amalgamation only is 10-20% efficient. aka up to 90% of the gold is not extracted.
most miners are losing most of there ore. However im not here to argue how concentrated my ore is or what method is best. Your favorite method is your opinion. im simply here to discuss about electrolysis and a interesting phenomenon I discovered. I dont see any benefit in hearing people gaslight me into what I already know and seen.
That is a fact for sure, but not with acids. And there are plethora of reasons why companies do not use acids to treat ores. Maybe some rich cons in some instances, but not raw milled ores.

Back to electrolysis. When performing it, did you separated the anode and cathode by some membrane ? Electrolysis will plate metals from solution on one electrode, but electrolysis is kinda "forced redox" reaction, and on the another electrode, equal equivalent of oxidant is created. In AR solution, this oxidant is chlorine gas. It is well possible that you redissolved some of the gold back into the solution.

Anyway. Conceptually, this can and should work, but with good ammount of theory put into it. If the metal deposited on the cathode is still connected to it (it makes good electric contact), it most probably won´t redissolve. Also, anode must be made from material, that does not oxidize with chlorine /or oxidize, but don´t wreck the whole process/ - on the budget, probably carbon electrode.

If you want to elaborate more on this concept, I would suggest to simulate the "best scenario" conditions = make some solution by digesting some ore in acid and lace it with known ammount of gold. This would give you solution where gold is certainly present. Then perform the electrolysis, and analyze as we suggested above. Then you can compare the result with actual gold put in, to calculate efficacy of the process and evaluate it/tweak it.
 

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