Screw up.

[dansdismantling]

Good afternoon members!! After more than two months off due to shingles on the face and in the eye I decided to try to work with the acids again and I had two different batches going both close to being done,so here’s what I screwed up I had one batch that I dropped the gold,mind you these were both dirty due to some oils I didn’t clean off of materials. So one dropped and the other was ready for AR I accidentally did the AR in the beaker I had just precipitated so now I have a combination of SMB with AR in it. Actually it was H202 34% and Hcl with now Smb. So the gold ore was re-dissolved. I was so irritated with myself I put everything away and went home. Just got back to the shop and the solution in the mishap beaker is full of slush???? I have water bottles that didn’t freeze and it’s like 40F here?? Did the smb mixed with H202 quagulate?? I’m stumped and disappointed I made this mistake. Now how to fix this,since it has Hcl smb and H202 34% steam it off and start over??? Any help would be greatly appreciated!!!!

 

[dansdismantling]

Good afternoon members!! After more than two months off due to shingles on the face and in the eye I decided to try to work with the acids again and I had two different batches going both close to being done,so here’s what I screwed up I had one batch that I dropped the gold,mind you these were both dirty due to some oils I didn’t clean off of materials. So one dropped and the other was ready for AR I accidentally did the AR in the beaker I had just precipitated so now I have a combination of SMB with AR in it. Actually it was H202 34% and Hcl with now Smb. So the gold ore was re-dissolved. I was so irritated with myself I put everything away and went home. Just got back to the shop and the solution in the mishap beaker is full of slush???? I have water bottles that didn’t freeze and it’s like 40F here?? Did the smb mixed with H202 quagulate?? I’m stumped and disappointed I made this mistake. Now how to fix this,since it has Hcl smb and H202 34% steam it off and start over??? Any help would be greatly appreciated!!!!

 

[dansdismantling]

I forgot to mention it is also saturated with silver chloride…..

 

[Yggdrasil]

I forgot to mention it is also saturated with silver chloride…..

Can you clarify.
AR or HCl/Peroxide?
Anyway anything with Chlorides will not dissolve Silver.
What was your material?

 

[dansdismantling]

Can you clarify.
AR or HCl/Peroxide?
Anyway anything with Chlorides will not dissolve Silver.
What was your material?

Hcl and high strength peroxide 34% dissolves gold no problem. The material is old pins in their sockets. Once the foils came off I removed the sockets. I dissolved the gold then precipitated the gold then accidentally dumped smb in it again. I got the two beakers mixed up.

 

[Yggdrasil]

Hcl and high strength peroxide 34% dissolves gold no problem. The material is old pins in their sockets. Once the foils came off I removed the sockets. I dissolved the gold then precipitated the gold then accidentally dumped smb in it again. I got the two beakers mixed up.

That is not AR and it do not need denoxing.
Just keep it close to boiling and stir it for a while.
Then add SMB, or other precipitant of your choice.
If that do not work, use a piece of solid Copper to cement it out.
If you have added too much SMB add water and heat it while stirring until the extra SMB dissolves, then siphon off the liquid.

Any thing with Chloride will NOT dissolve Silver.

 

[Martijn]

in your first post you say you did AR again in the precipitated beaker (decanted or added acids to the solution with SMB?)
and in your second post you said you added SMB to the precipitated gold.. which is it?

I forgot to mention it is also saturated with silver chloride…..

What is full of AgCl? The foils or the precipitated solution?
Any silver should have been filtered out before precipitating the gold.
so you got me confused.

 

[dansdismantling]

Can you clarify.
AR or HCl/Peroxide?
Anyway anything with Chlorides will not dissolve Silver.
What was your material?

They were late 60’s pins in sockets. Dissolved the base metals in hcl peroxide 3% then removed them from the sockets then dissolved using hcl and 34% peroxide. So the initial solution was 3% peroxide then the AR was composed of 34% peroxide and hcl. The decanting never happened because of the screw up.

 

[Yggdrasil]

They were late 60’s pins in sockets. Dissolved the base metals in hcl peroxide 3% then removed them from the sockets then dissolved using hcl and 34% peroxide. So the initial solution was 3% peroxide then the AR was composed of 34% peroxide and hcl. The decanting never happened because of the screw up.

AR is HCl/Nitric, nothing else.
So when you say AR and you do something else it gets confusing.

 

[dansdismantling]

AR is HCl/Nitric, nothing else.
So when you say AR and you do something else it gets confusing.

Sorry you’re correct. Is there a name for the high strength peroxide method? A gallon is $22 for 34% a mile away and works great at dissolution.
I simmered it all day yesterday and now I have about 1/4 the solution I had. The wire wrapped pins are Ag coated cu wires hence the silver chloride.

 

[Yggdrasil]

Sorry you’re correct. Is there a name for the high strength peroxide method? A gallon is $22 for 34% a mile away and works great at dissolution.
I simmered it all day yesterday and now I have about 1/4 the solution I had. The wire wrapped pins are Ag coated cu wires hence the silver chloride.

We call it HCl/Peroxide.
The AP is actually Cupric Chloride.
No need to boil long.
As long as it test negative just let the excess SMB and other water soluble salts dissolve and the siphon it off.

 

[dansdismantling]

in your first post you say you did AR again in the precipitated beaker (decanted or added acids to the solution with SMB?)
and in your second post you said you added SMB to the precipitated gold.. which is it?

What is full of AgCl? The foils or the precipitated solution?
Any silver should have been filtered out before precipitating the gold.
so you got me confused.

Sorry I’m doing this on my phone and it doesn’t update quotes so if out of order it’s my fault. I have AgCI because the wire wrapped pins are Ag coated Cu wires. Yes I tested them they’re silver coated copper wires. So I had two batches going one getting ready for dissolution of foils and the other I dropped with Smb. I then got called away to help my father came back and added high strength 34% peroxide and Hcl to the beaker that just had the smb put in it. So one beaker is untouched and one now has hcl smb 34% peroxide and h20.

 

[Martijn]

They were late 60’s pins in sockets. Dissolved the base metals in hcl peroxide 3% then removed them from the sockets then dissolved using hcl and 34% peroxide. So the initial solution was 3% peroxide then the AR was composed of 34% peroxide and hcl. The decanting never happened because of the screw up.

So if i understand it correctly, you dissolved the base metals in AP, fished the sockets out, added 34% H2O2 to dissolve the gold, added SMB, and then added 34% H2O2 by mistake, all without filtering or decanting?
So all of this happened in the same solution?

 

[dansdismantling]

in your first post you say you did AR again in the precipitated beaker (decanted or added acids to the solution with SMB?)
and in your second post you said you added SMB to the precipitated gold.. which is it?

What is full of AgCl? The foils or the precipitated solution?
Any silver should have been filtered out before precipitating the gold.
so you got me confused.

So if i understand it correctly, you dissolved the base metals in AP, fished the sockets out, added 34% H2O2 to dissolve the gold, added SMB, and then added 34% H2O2 by mistake, all without filtering or decanting?
So all of this happened in the same solution?

Correct. I did filter it but the silver was still in solution so it didn’t catch nearly as much that still remains. I will definitely remove the wire wraps next time so there’s zero AgCI
Now I just got back and the beaker appears to have frozen solution this is really aggravating because I have water bottles that are t frozen.

 

[Yggdrasil]

Correct. I did filter it but the silver was still in solution so it didn’t catch nearly as much that still remains. I will definitely remove the wire wraps next time so there’s zero AgCI
Now I just got back and the beaker appears to have frozen solution this is really aggravating because I have water bottles that are t frozen.

If you have used any Chloride at all there will not be any Silver in solution.
And since you used HCl there is plenty.
Ergo, no Silver in solution.

 

[Martijn]

Correct. I did filter it but the silver was still in solution so it didn’t catch nearly as much that still remains. I will definitely remove the wire wraps next time so there’s zero AgCI
Now I just got back and the beaker appears to have frozen solution this is really aggravating because I have water bottles that are t frozen.

That looks more like hydroxides... what is the pH?

 

[snoman701]

Back to basics.

When you add Hydrogen Peroxide to HCl, the hydrogen peroxide releases chlorine gas from the HCl. This is what will oxidize gold, as well as all of the base metals. At this point, you should have been able to fish the plastic remains out of the beaker, leaving only a green liquid, possibly with some cloudiness if there was silver or lead present. Silver chloride is insoluble in water. Lead chloride is insoluble in cold water, but soluble at higher temps. If you tested your liquid with stannous, and there was gold present in the pins you dissolved, then it should test positive at this point.

The pregnant (with gold) liquor should at this point have sulfuric acid added in a small amount. This causes any lead present to precipitate. The liquor should then be allowed to cool, and be filtered. The filtrate should be clear.

Now, since you used hydrogen peroxide, there is no need to denox. If there was an abundance of oxidizer, just leave it on a hot plate for a while. All of the oxidizer (being chlorine gas) will gas off.

You should be able to add SMB and precipitate gold.

My guess, is that you added so much hydrogen peroxide that you turned a good amount of the HCl into water, the pH came up, and the base metals precipitated as hydroxides.

You can test that by taking a small amount of the sludge and adding fresh HCl to it, without hydrogen peroxide. It should all go into solution except the gold present. Once you have all of the copper / zinc in solution, it's then and only then that you add additional oxidizer (Hydrogen Peroxide) to get the gold to go into solution.

 

[dansdismantling]

Unfortunately yes. Was back there again today and the solution appeared frozen like a slushy. Heated it back up and went to liquid state. Upon filtering it froze up once it hit the air. I’ve put it to the side until I get a good grasp on what went wrong other than the obvious. For one thing I should’ve ran everything in my electric parts cleaner and another was leaving the silver coated copper wires on the pins…. I had shingles on my face and my eye and the fumes were making it unbearable so I tossed it all in ap and let sit for 40 some days.

 

[dansdismantling]

I haven’t tested the ph.

That looks more like hydroxides... what is the pH?

I’m still dealing with shingles on my eye and only do a little bit at a time even though I have goggles and a respirator and am outside the fumes still irritate my eye. This is day 66 with these damn shingles. I will test soon.

 

[dansdismantling]

Back to basics.

When you add Hydrogen Peroxide to HCl, the hydrogen peroxide releases chlorine gas from the HCl. This is what will oxidize gold, as well as all of the base metals. At this point, you should have been able to fish the plastic remains out of the beaker, leaving only a green liquid, possibly with some cloudiness if there was silver or lead present. Silver chloride is insoluble in water. Lead chloride is insoluble in cold water, but soluble at higher temps. If you tested your liquid with stannous, and there was gold present in the pins you dissolved, then it should test positive at this point.

The pregnant (with gold) liquor should at this point have sulfuric acid added in a small amount. This causes any lead present to precipitate. The liquor should then be allowed to cool, and be filtered. The filtrate should be clear.

Now, since you used hydrogen peroxide, there is no need to denox. If there was an abundance of oxidizer, just leave it on a hot plate for a while. All of the oxidizer (being chlorine gas) will gas off.

You should be able to add SMB and precipitate gold.

My guess, is that you added so much hydrogen peroxide that you turned a good amount of the HCl into water, the pH came up, and the base metals precipitated as hydroxides.

You can test that by taking a small amount of the sludge and adding fresh HCl to it, without hydrogen peroxide. It should all go into solution except the gold present. Once you have all of the copper / zinc in solution, it's then and only then that you add additional oxidizer (Hydrogen Peroxide) to get the gold to go into solution.

I barely added the peroxide. However the difference between the 3% peroxide and the 34% could be the culprit because today it didn’t smell of acids at all. It has since been boiled off to about 1/4 the solution. I’m going to add some fresh hcl and go from there. I’m using 2000 ml beaker and after my first drop had cooled off there was about 1 inch of silver chloride on the bottom. Put it back on the heat that’s when I was called away to help my father. Came back and both beakers were on heat and this is where I screwed up by going to dissolve the wrong beaker with h202 @ 34% and hcl. These shingles has really put me through hell.