Inquartation mess

[autumnwillow]

So I tried to use recycled copper nitrate from silver nitrate that was precipitated with hcl, scavenged the hcl with silver nitrate. Apparently I didn't add enough silver nitrate so there goes my mess.

I used 40% of this copper nitrate and 60% 70% nitric ratio and a lot of silver chloride came out.

I added sulfamic to stop the reaction. For some odd reason it somehow dissolved the silver chlorides but the digestion stopped too.

So I just decided to filter,wash, then dissolve the silver chloride in ammonia, filter, wash then incinerate.

Did I do the right thing?
Can this incinerated flakes be Re digested in nitric?

 

[FrugalRefiner]

I'm afraid I don't understand your post.

So I tried to use recycled copper nitrate from silver nitrate that was precipitated with hcl, scavenged the hcl with silver nitrate. Apparently I didn't add enough silver nitrate so there goes my mess.

How did you get copper nitrate from silver nitrate that was precipitated with HCl? Was this a mix of copper nitrate and silver nitrate from dissolving something like sterling silver with nitric acid? If you precipitated the silver as silver chloride by adding HCl, then you would have a weak solution of copper nitrate.

Then you say you scavenged the HCl with silver nitrate. If you added too much HCl in the first part, then adding silver nitrate would cause more silver chloride to precipitate until there was no more free chloride in the solution. Is that what you did?

But you say you didn't add enough, so you have a mess. :?

I used 40% of this copper nitrate and 60% 70% nitric ratio and a lot of silver chloride came out.

I don't understand how adding nitric acid to this solution would cause silver chloride to come out. If you had both silver and copper in the solution, nitric would not cause either to precipitate. If there was still chloride in the solution, then there couldn't be any silver in it. I'm missing something here.

I added sulfamic to stop the reaction. For some odd reason it somehow dissolved the silver chlorides but the digestion stopped too.

What were you digesting? You didn't mention that anywhere above.

So I just decided to filter,wash, then dissolve the silver chloride in ammonia, filter, wash then incinerate.

You didn't mention reacidifying this solution. If you dissolved silver chloride with ammonia, you have the possibility of creating explosive compounds. The standard practice is to add HCl to the solution to reprecipitate the silver to avoid creating these explosive compounds. Never allow a solution with silver and ammonia to dry!

Did I do the right thing?

I have no idea, since I really don't understand what you've really done.

Can this incinerated flakes be Re digested in nitric?

What flakes? Ifyou dissolved the silver chloride with ammonia, where did you get flakes?

I'm not trying to be mean. I just don't understand what you've done.

Dave

 

[autumnwillow]

The copper nitrate solution I used were not freely out of hcl.

So when I dissolved my inquarted gold. Silver chloride precipitated because of hcl content.

 

[Topher_osAUrus]

Ah, i think i understand.

You had some silver and copper nitrate, that had silver removed/ precipitated with hcl to remove silver. (leaving free hcl in the solution)
You inquarted some gold.
You digested inquart gold with copper nitrate that had been used in the agcl process.
You now have silver chloride, copper nitrate, and a bit of silver nitrate...?right?

Edit to fix MY clarity

 

[autumnwillow]

Correct topher

 

[FrugalRefiner]

I added sulfamic to stop the reaction. For some odd reason it somehow dissolved the silver chlorides but the digestion stopped too.

So I just decided to filter,wash, then dissolve the silver chloride in ammonia, filter, wash then incinerate.

Did I do the right thing?
Can this incinerated flakes be Re digested in nitric?

OK, I think I understand.

"Can this incinerated flakes be Re digested in nitric?" Yes.

"Did I do the right thing?" Well, not what I would have done, but you should be fine. I wouldn't have added the sulfamic to stop the reaction unless you added a huge amount of excess HCl. If you still had a reaction going I would have let it continue. If it stopped, you could try to break the AgCl shell, or pull out the pieces, dissolve the AgCl with ammonia, and then return them to the nitric leach. Nitric is expensive, so as a frugal refiner, I hate to waste it. :wink:

I do hope you promptly acidified your ammonia wash.

Dave

 

[autumnwillow]

Well, I tried the incinerated stuff, it did not digest it.
So I ended up with melting, then inquarting again. It wen't well this time. I have already precipitated using 200g of SMB, yield is supposed to be 198g. Tomorrow i'll proceed with the washing and melting. I hope there won't be much losses, this is my first refine after 2 months of break.

What do you guys do with your ammonia wash? Acidifying it will precipitate chlorides again, can't I just throw this in the stock pot?

 

[Topher_osAUrus]

Keep the acidified ammonia separate from your stockpot.

 

[autumnwillow]

Topher may I ask why? If the stock pot is acidic anyway the ammonia solution cannot increase the ph of the stock pot not unless a large amount of ammonia was used.

I got 180.1g, lots of silver chlorides in the ar part (my bad here). I converted the silver chlorides to silver thru lou's sulfuric iron process, melted and got 44g of somewhere in 33% gold.

 

[Topher_osAUrus]

I believe I read that it should be kept separate to avoid any issues, but I cannot find the thread that gave that issued warning at the moment.

But, one reason I can think of, is. The stock pot is a combo of acids that have either dissolved gold or other pm's and been precipitated or whatever else. And they still may contain precious metals.

The only precious metal ammonia contained was silver, and if it was already dropped out with HCl, then it is a barren solution and deserves no stockpot, just proper waste treatment.

This is just a guess, a poorly crafted one, as it is early and I have yet to have my coffee, so I feel as dumb as a bag of rocks.

Besides that logic, another reason (if you want to call it that?), is even if I have reacidified my ammonia rinses to ph 1, I still get these *huge* soapy bubbles that seem to not go away.

 

[butcher]

Ammonia or ammonium salts can cause problems or even dangers with solutions, metals, or in a process, you may choose to use later with material from your stock pot.