Aqua regia gold stuck in solution electrolysis

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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
SMB can not and I emphasize this, Can Not neutralize any acidic solution, since it is by itself acidic.
You simply can not neutralize an acid with another acid.
That is another fun fact and this one you will find all the math and calculations, if you bother reading the books of chemistry.
Admittedly one may make it a tad less acidic by using a weaker acid.
 
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
A fire assay is done on finely milled ore and the selection is mixed and randomized
so one get a good representative of the ore body.
On e do not do fire assays on the residues from leaching, it would be less wasteful to just smelt it and check from Gold.
Information wise this will only tell if there is Gold or not in the ore, not how much.

And if your solution is in fact neutral, then you have done things you have not told us about,
or used the wrong chemicals somewhere, which in fact is quite scary if that is true.
 
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.
I did not use a membrane. Not sure of a membrane that could withstand such harsh chemicals. I havent looked too far into that however. It definetly did work. I saw the precipitate and it was amazing. Worst case I simply can connect a arduino to a shunt and measure once amperage shoots up to turn off current. I also am going to use sodium chlorate as a acid next time so hopefully simply boiling it will neutralize it. im not sure of any anode other than graphite that is resistant. The graphite I used however was very loose and exfoliated rapidly. I plan on trying copper next. Sacraficing some of it is fine, but im worried the iron resulted in some weird effect
I definetly want to replicate this and simulate what happened. Replicating it on a much smaller sample and carefully tweaking the variables till I find what makes it different. different electrodes etc. could simply be due to the spike in amperage and temperature redissolving. will be a while till I can replicate, hopefully soon. in the meantime will do a fire assay on the junk I created
 
SMB can not and I emphasize this, Can Not neutralize any acidic solution, since it is by itself acidic.
You simply can not neutralize an acid with another acid.
That is another fun fact and this one you will find all the math and calculations, if you bother reading the books of chemistry.
Admittedly one may make it a tad less acidic by using a weaker acid.
im not sure how to reply. Its like someone telling me black flamingos dont exist when I clearly seen it with my two eyes
 
im not sure how to reply. Its like someone telling me black flamingos dont exist when I clearly seen it with my two eyes
To test your strips, take one with known acid, next with water and one with some Sodium bicarbonate in water and check.
 
To test your strips, take one with known acid, next with water and one with some Sodium bicarbonate in water and check.
I have in fact dont exactly this many, many times and the ph strip works perfectly. Im done addressing and proving whether my PH strips are expired or not. If you dont believe me then theres no further conversation to be had in distrust.
 
Why are you so argumentative? pH test strips do deteriorate with age. Yggdrasil has given you a simple way to test them. Even if you have tested them in the past, they could be expired now.

You're new here. We don't know your level of experience, or the materials you're using.

People are trying to help you, and you just seem to want to argue.

If you know everything we all know, then why did you come here asking questions?

I would recommend toning down your attitude, taking a small dose of humility, and trying to help those who are trying to help you. If not, people are going to get tired of trying to help and they'll just ignore your posts until you get frustrated and leave. That won't help any of us.

Dave
 
Why are you so argumentative? pH test strips do deteriorate with age. Yggdrasil has given you a simple way to test them. Even if you have tested them in the past, they could be expired now.

You're new here. We don't know your level of experience, or the materials you're using.

People are trying to help you, and you just seem to want to argue.

If you know everything we all know, then why did you come here asking questions?

I would recommend toning down your attitude, taking a small dose of humility, and trying to help those who are trying to help you. If not, people are going to get tired of trying to help and they'll just ignore your posts until you get frustrated and leave. That won't help any of us.

Dave
I tested them today
 
Thanks for letting us know that. It's much more helpful than saying "I have in fact dont exactly this many, many times and the ph strip works perfectly."

"Many times" could be months ago, but doing telling us you did it today is much better.

Honestly, people are trying to help you. Work with them, just as you just responded to me.

Dave
 
I used 1 kilo of crushed ore, 200ml of nitric, 800ml of HCL

Per the bold print - 200 ml of nitric (plus 800 ml HCL) is enough nitric to dissolve 200 grams of gold

So - IF (the VERY BIG IF) your kilo of ore had even a gram of gold in it - 200 ml nitric would be 200 time more nitric then needed to dissolve that 1 gram gold

What that means is that with that much "free nitric" - the nitric will ether -----

1) not allow the gold to precipitate at all (because the "free nitric" keeps the gold dissolved) or ---

2) if the gold precipitates - the "free nitric" will just keep "re-dissolving" the gold nearly as fast as it precipitates

Kurt
 
So - you are trying to run an electro "winning" cell

A "winning" cell works by depositing metals that are dissolved in a solution onto the cathode

The problem with a winning cell is that it is not "selective" to winning only gold but in fact will win (deposit) MANY metals from a solution (such as copper, nickel, chrome, tin, etc. etc. etc.)

These are all metals commonly found in ores including in ores that may (or not) contain gold

rarely (if ever) do ores have just one metal in them but "in fact" will have "several" metals in them

So when you used AR on your ore - you most likely dissolved "several" different metals (which may - or not - have included gold)

Then when you run the AR in your winning cell it deposited whatever metals the AR dissolved to the cathode (which may or not include gold)
I definetly seen gold in the ore and the electrolysis plated it out.

Therefore what you show in this picture is not "poof" of gold - it is only proof the AR dissolved metals & that metals were then won to the cathode - & there is a whole host of metals (besides gold) that would do that

Kurt
 
Sodium Meta Bisulfite and the other Sulfites can drop Gold, but only from highly acidic liquors.
And you claim yours is neutral, in which it won't work.
ive repeated multiple times this statement. The SMB neutralized the solution. The solution WAS PREVIOUSLY ACIDIC. You have done nothing but doubt everything I say and make me repeat the same exact statement I said in the original post for 4 whole pages on this thread. Being accused by a liar by you over and over is harassments at this point. please leave me alone.
 
ive repeated multiple times this statement. The SMB neutralized the solution. The solution WAS PREVIOUSLY ACIDIC. You have done nothing but doubt everything I say and make me repeat the same exact statement I said in the original post for 4 whole pages on this thread. Being accused by a liar by you over and over is harassments at this point. please leave me alone.
Sorry mac, we do not leave unsolved impossibilities alone in this forum.
They can at a later situation lead to losses or injuries by others.

I/we have kept the door open for it to be a freak mistake somewhere down the line, either with your process or your chemicals.

The ONLY possibility for your "SMB" to neutralize a solution, is that it in fact is not SMB at all.
Dissolve a teaspoon of your "SMB" in water and test the pH of it. It should be around +/- 4

So by being so argumentative and unwilling to discuss what happened openly,
you have actually muddled the possibilities to find a solution to this in the shortest possible time.
 
I did not use a membrane. Not sure of a membrane that could withstand such harsh chemicals. I havent looked too far into that however. It definetly did work. I saw the precipitate and it was amazing. Worst case I simply can connect a arduino to a shunt and measure once amperage shoots up to turn off current. I also am going to use sodium chlorate as a acid next time so hopefully simply boiling it will neutralize it. im not sure of any anode other than graphite that is resistant. The graphite I used however was very loose and exfoliated rapidly. I plan on trying copper next. Sacraficing some of it is fine, but im worried the iron resulted in some weird effect
I definetly want to replicate this and simulate what happened. Replicating it on a much smaller sample and carefully tweaking the variables till I find what makes it different. different electrodes etc. could simply be due to the spike in amperage and temperature redissolving. will be a while till I can replicate, hopefully soon. in the meantime will do a fire assay on the junk I created
As person who have more than 10 years of experience in professional chemistry, I can only recommend these steps:

1. Perform assay to PROVE that you have gold (and how much of it, this is also very important) in your ore, otherwise this can go nowhere and in the end for nothing at all.

2. If you want to prove your concept is actually working, SIMULATE best-case scenario conditions. Take some similar type of rock with NO GOLD in it, crush it as you crushed your ore. Leach it as you leached your ore and in the end, spike it with KNOWN ammount of gold in solution (weigh the gold, dissolve it in AR, pour it in, some 50-70 mg will be more than OK). Then perform electrolysis, redissolve the cement/metal deposit, and reclaim your gold in usual ways (de-NOx-ing and SMB precipitation). By weighing the resulting pure gold powder obtained, you will clearly see how much of the gold you can recover with your technique. Only then move to real samples. There are too many variables and possibilities/tweaks/mishaps that can ruin it completely. You need to know it beforehand, otherwise you can be celebrating recovery of 10mg of gold from ore sample, while not knowing you thrown away 50mg with "barren" rock, waste and sludges.

3. After validation of your methodology and technique, you can process the actual ore by this technique and expect realistically some accuracy and reproducibility of the procedure.
This is how it is done in real world, by real scientists, in industry. Anytime, when we need to actually know if something is working or if it is a viable way/approach to do something. There are reasons for us doing it this way. Long list of reasons.
-----------------------------------------
Last note:

If your anode will be made of material that can react with liberated chlorine, or if it can oxidize under potential (voltage) applied, you will practically only dissolve the electrode, which will dissolve into solution and plate on the cathode (copper will do exactly this). Even platinum won´t work in this case. Only common electrodes that can work in this scenario are graphite and RuO2 electrodes. Graphite will deteriorate, but not alter the composition of the electrolyte significantly.
This is how metals are actually electrorefined. Anode is made of impure metal (eg. iron/copper/nickel/silver/gold), and indiferent cathode/or made from pure metal which will be purified (stainless steel/metal of interest/graphite/platinum etc...). Under applied voltage, metal of the anode will oxidize (electrons removed) and dissolve into solution, simultaneously being plated on the cathode, where these electrons added back, closing the circuit.

Go with graphite for anode. Trust me.
 
... maybe if someone else had a theory why the gold would redissolve in electrolysis once the amperage spiked up ...

The solution turned red and the gold dissolved after you switched to a steel anode. Could the culprit oxidizer here be ferric chloride? A steel anode in a hot HCl solution rapidly dissolves to vivid red ferric ions. This paper indicates ferric chloride can dissolve gold in a hot acidic solution:
https://acris.aalto.fi/ws/portalfil...netics_and_mechanisms_of_gold_dissolution.pdf

Generally I run electrowinning with a lab power supply in constant current mode so I get to decide the amperage--to get clean metal separation in a lab scale experiment, I've had better results from small currents well under one amp. At high amperage, the gas bubbles can rapidly change the pH (due to directly removing hydrogen as a gas!), as well as creating corrosive hazardous mists.
 
The solution turned red and the gold dissolved after you switched to a steel anode. Could the culprit oxidizer here be ferric chloride? A steel anode in a hot HCl solution rapidly dissolves to vivid red ferric ions. This paper indicates ferric chloride can dissolve gold in a hot acidic solution:
https://acris.aalto.fi/ws/portalfil...netics_and_mechanisms_of_gold_dissolution.pdf

Generally I run electrowinning with a lab power supply in constant current mode so I get to decide the amperage--to get clean metal separation in a lab scale experiment, I've had better results from small currents well under one amp. At high amperage, the gas bubbles can rapidly change the pH (due to directly removing hydrogen as a gas!), as well as creating corrosive hazardous mists.
Thank you soo soo much! finally a very helpfull answer. I definetly agree this is a very reasonable theory. Also thanks so much for that and especially with the later knowledge. I suppose higher amperage simply is waste so controlling it is important. What current density (amps per square cm/inch) are you running for your setup?
 

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