Aqua regia gold stuck in solution electrolysis

[electrochemgold]

Hello I tried a new method on extracting and encountered a really weird situation. In short I have gold in my solution that I cant precipitate with sodium metabisulfate.
I originally extracted some gold ore with direct aqua regia, then added sulfuric acid and vacuum filtered twice. Test with stannous chloride confirmed there was gold. From the resulting solution I started a 5v electrolysis in which gold started to plate and precipitate from the cathode beautifully.
View attachment PXL_20231030_141058630.mp4
Eventually a gold layer on the bottom of the glass formed. I originally used graphite electrodes which the anode started falling apart. So I switched to steel anode. However some time later the current started to shoot up very quickly, over 25amps, originally was around 6a. Solution heated up to almost 80c and all the gold on the cathode and bottom of the glass disappeared. Previously only gas bubbles were bring formed from the anode now the cathode was vigorously bubbling. After the gold disappeared I switched to a titanium cathode as you see in the second video. Green wire is negative.

View attachment PXL_20231030_184928585.mp4

I tried adding hcl nothing happened, I tried adding nitric acid and solution turned black. Eventually I added a bunch of SMB and a bunch of iron crashed out. I vacuum filtered it however testing the solution with stannous chloride still showed gold. Solution is neutral in PH and further SMB has no reaction. Solution is also a dark blood red color. Im stuck other than trying to boil it off and starting over. Very puzzled what happened however and what could cause and create a gold solution that wont precipitate out?

 

[FrugalRefiner]

Very puzzled what happened however and what could cause and create a gold solution that wont precipitate out?

Really?! Let's review.

You "originally extracted some gold ore with direct aqua regia, then added sulfuric acid and vacuum filtered twice. Test with stannous chloride confirmed there was gold. From the resulting solution I started a 5v electrolysis in which gold started to plate and precipitate from the cathode beautifully."

It is rarely a good idea to try to "extract gold from ore". There are often other metals present that can ruin your day. Do you have an assay for your ore?

So, you started to try to electrowin the gold you hoped you had in solution. Your graphite anode started falling apart, so switched to a steel anode. Your amperage spiked, and your temperature followed. Your gold disappeared and you had vigorous bubbling from your cathode. So, you switched to a titanium cathode.

That wasn't working for you, so you threw in some HCL, and when that didn't work you threw in some nitric. Then you added "a bunch of SMB", and a bunch of iron crashed out.

But your solution still tests positive with stannous, your pH is neutral, and more SMB doesn't do anything.

You have created what we call a mess. You kept throwing different stuff at a potentially toxic solution created by throwing acid on unknown rocks, and now you're puzzled at what happened. I'm sorry. I don't mean to bust your chops, but you seem to have just tried a bunch of different things without any real idea of what you're doing.

I guess I should start by directing you to So, you think your rocks are valuable? READ THIS BEFORE YOU POST ABOUT ORE!.

Dave

 

[Golddigger76]

Did you see the methods that you tried on a YouTube video ?

There a YouTube channel that is called My Adventure, he does have a few good videos about gold prospecting but some of the videos where he chemically removes gold from his ore is not safe or a good way to do it without knowing what besides gold is in the ore.
What you have done reminds me of one of the videos he made...

And with all of the acid that you have added exactly what has made the ph be at neutral ? 😐

How much solution have you made, a gallon or less ?

 

[electrochemgold]

Really?! Let's review.

You "originally extracted some gold ore with direct aqua regia, then added sulfuric acid and vacuum filtered twice. Test with stannous chloride confirmed there was gold. From the resulting solution I started a 5v electrolysis in which gold started to plate and precipitate from the cathode beautifully."

It is rarely a good idea to try to "extract gold from ore". There are often other metals present that can ruin your day. Do you have an assay for your ore?

So, you started to try to electrowin the gold you hoped you had in solution. Your graphite anode started falling apart, so switched to a steel anode. Your amperage spiked, and your temperature followed. Your gold disappeared and you had vigorous bubbling from your cathode. So, you switched to a titanium cathode.

That wasn't working for you, so you threw in some HCL, and when that didn't work you threw in some nitric. Then you added "a bunch of SMB", and a bunch of iron crashed out.

But your solution still tests positive with stannous, your pH is neutral, and more SMB doesn't do anything.

You have created what we call a mess. You kept throwing different stuff at a potentially toxic solution created by throwing acid on unknown rocks, and now you're puzzled at what happened. I'm sorry. I don't mean to bust your chops, but you seem to have just tried a bunch of different things without any real idea of what you're doing.

I guess I should start by directing you to So, you think your rocks are valuable? READ THIS BEFORE YOU POST ABOUT ORE!.

Dave

Hello no need to be disrespectful. As I stated in the beginning I was simply conducting a experiment. If you dont like how I do my stuff thats fine but to insult that "I have no clue what im doing" is simply being rude.

 

[Shark]

I wonder what Harold is up to these days?

 

[electrochemgold]

Did you see the methods that you tried on a YouTube video ?

There a YouTube channel that is called My Adventure, he does have a few good videos about gold prospecting but some of the videos where he chemically removes gold from his ore is not safe or a good way to do it without knowing what besides gold is in the ore.
What you have done reminds me of one of the videos he made...

And with all of the acid that you have added exactly what has made the ph be at neutral ? 😐

How much solution have you made, a gallon or less ?

The video that primarily got me interested was the following.

the solution became PH neutral after adding the SMB
Currently I have a little over a liter of the solution.

 

[Yggdrasil]

Hello no need to be disrespectful. As I stated in the beginning I was simply conducting a experiment. If you dont like how I do my stuff thats fine but to insult that "I have no clue what im doing" is simply being rude.

Assuming your description of your project is correct, he is just describing the plain truth.
You obviously have no understanding of what you have been doing.

If you study the links below you can how ever gain the knowledge to understand why things ended up in a horrible mess.
Put your chemicals away and study these links and then come back with a plan which we may approve or improve.

We ask our new members to do 3 things.
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

https://goldrefiningforum.com/threads/gold-refining-forum-rules.31182/

 

[Yggdrasil]

The video that primarily got me interested was the following.

the solution became PH neutral after adding the SMB
Currently I have a little over a liter of the solution.

A solution do not get pH neutral by adding SMB, at least used in sensible amounts.
How do you know it is neutral anyway, did you test the pH?
Did you test your solution with Stannous to verify it held values, before and after?
Edit to add:
Do you have pictures of said Stannous tests?

 

[Yggdrasil]

The video that primarily got me interested was the following.

the solution became PH neutral after adding the SMB
Currently I have a little over a liter of the solution.

IShore has no high regards in this forum.
This video did not give much of an impression either and did not change that much.

 

[electrochemgold]

Assuming your description of your project is correct, he is just describing the plain truth.
You obviously have no understanding of what you have been doing.

If you study the links below you can how ever gain the knowledge to understand why things ended up in a horrible mess.
Put your chemicals away and study these links and then come back with a plan which we may approve or improve.

We ask our new members to do 3 things.
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

https://goldrefiningforum.com/threads/gold-refining-forum-rules.31182/

What is exactly wrong with attempting to electrolyze PM directly out of a aqua regia solution?
yes im aware that direct ore acid extraction is not preferable. Thats why im trying a new method to see if it can be done via electrolysis without having to first extract out other metals/other steps. And it worked. If I simply stopped the electrolysis before the amperage spiked up and it overheated I would have a amazing success. No where can I find that overrunning it will cause the gold to redissolve. and im pretty sure it occurred simply due to the iron electrode.

as for the "bunch of other chemicals" I added. Its simply HCL and Nitric, which is whats inside aqua regia aka the original solution. I didnt "add a bunch of random chemicals" simply readded what was originally in there in the first place. I was curious if one of the acids got used up in the electrolosis and got converted which I was correct in. So again, what is wrong with experimenting and trying new methods???

 

[electrochemgold]

A solution do not get pH neutral by adding SMB, at least used in sensible amounts.
How do you know it is neutral anyway, did you test the pH?
Did you test your solution with Stannous to verify it held values, before and after?
Edit to add:
Do you have pictures of said Stannous tests?

Yes I tested the PH. Yes I tested the solution with stannous chloride before and after.
on a separate successful test where I stopped the run once amps shot up, I tested that with stannous chloride before and after and it showed negative afterwards.
here is a video of the stannous chloride test before electrolysis
I dont have any video of afterwards but effect was the same.

View attachment PXL_20231030_125204867 (1).mp4

 

[Martijn]

In short I have gold in my solution that I cant precipitate with sodium metabisulfate.

I have no solution to electrowinning pm's from AR, but to get any values out:
https://goldrefiningforum.com/threads/when-in-doubt-cement-it-out.30236/

 

[Martijn]

Yes I tested the PH. Yes I tested the solution with stannous chloride before and after.
on a separate successful test where I stopped the run once amps shot up, I tested that with stannous chloride before and after and it showed negative afterwards.
here is a video of the stannous chloride test before electrolysis
I dont have any video of afterwards but effect was the same.

View attachment 60089

That is a very clear and positive stannous test for Copper. not gold.

 

[electrochemgold]

IShore has no high regards in this forum.
This video did not give much of an impression either and did not change that much.

not sure why this forum enjoys to attack people's character instead of information but ok. I agree that the video has a few mistakes but im not describing it as a holy grail nor ever did. Simply linked it as my source of inspiration to attempt it. Again, it worked amazing. Knowing my current mistakes I would simply stop the power once current shoots up. But im fascinated what could cause the gold to dissolve and stay dissolved so well

 

[Yggdrasil]

What is exactly wrong with attempting to electrolyze PM directly out of a aqua regia solution?
yes im aware that direct ore acid extraction is not preferable. Thats why im trying a new method to see if it can be done via electrolysis without having to first extract out other metals/other steps. And it worked. If I simply stopped the electrolysis before the amperage spiked up and it overheated I would have a amazing success. No where can I find that overrunning it will cause the gold to redissolve. and im pretty sure it occurred simply due to the iron electrode.

as for the "bunch of other chemicals" I added. Its simply HCL and Nitric, which is whats inside aqua regia aka the original solution. I didnt "add a bunch of random chemicals" simply readded what was originally in there in the first place. I was curious if one of the acids got used up in the electrolosis and got converted which I was correct in. So again, what is wrong with experimenting and trying new methods???

First, there is nothing wrong with trying new methods.
Just be aware that the chances of actually finding a new method that is either better or more economically sound then the ones the industry is already using is quite slim.
People have been extracting and refining Gold for millennia and it has gradually evolved to the methods the industry use today.

But here is the catch, if you are to do such a thing it has to be done in a methodical and planned way so you understand what is happening and why.
This is where you fail, you just keep adding stuff hoping to solve a problem you don't understand the nature of.

To solve your problem we need some information.
We can start with this.
1 How did you make your Aqua Regia?
2 Did you test the liquid with Stannous before your electrolysis, if so how and how did it look. Pictures please.
3 Did you decompose your Nitric in the AR before the electrolysis?
4 How much Sulfuric did you add?

 

[Yggdrasil]

Yes I tested the PH. Yes I tested the solution with stannous chloride before and after.
on a separate successful test where I stopped the run once amps shot up, I tested that with stannous chloride before and after and it showed negative afterwards.
here is a video of the stannous chloride test before electrolysis
I dont have any video of afterwards but effect was the same.

View attachment 60089

Sad to inform you that there is no Gold in that Stannous test.
Her is how it looks.
Courtesy of LazerSteve.
Edit, removed Satannous

 

[Yggdrasil]

not sure why this forum enjoys to attack people's character instead of information but ok. I agree that the video has a few mistakes but im not describing it as a holy grail nor ever did. Simply linked it as my source of inspiration to attempt it. Again, it worked amazing. Knowing my current mistakes I would simply stop the power once current shoots up. But im fascinated what could cause the gold to dissolve and stay dissolved so well

We do not attack people, but we do clearly notify people when they do something wrong.
And that has to be like that, since we deal with dangerous chemicals that can maim and kill you if you treat them wrong.
Bruised egos do not get any sympathy in here, better alive and bruised than dead.

 

[Martijn]

Satannous test

I thought anything religious was a no go?

 

[electrochemgold]

Sad to inform you that there is no Gold in that Satannous test.
Her is how it looks.
Courtesy of LazerSteve.
View attachment 60090

I definetly seen gold in the ore and the electrolysis plated it out.

 

[Yggdrasil]

I thought anything religious was a no go?

OOps I'll fix that promptly