Unidentified material in aqua regia

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Reddic

New member
Joined
Dec 3, 2019
Messages
3
Location
Houston, TX
Any help will be appreciated...recently I left some gold in solution while on vacation. When I came back I found white fiberglass type crystals at the bottom of the solution. I filtered them out, set it aside, recovered the gold, no issues. Later I found more of the stuff in the bottom of one of my stock pots. Anyone know what this stuff is? Thanks in advance.

1. I was recovering gold from gold filled jewelry.

2. The stockpot did have a dissolved filter paper in it.
 

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Thanks for the reply...no it didn't. Btw, it is very heavy and when I rinse it, it immediately settles to the bottom of the glass. I did not try boiling it though.
 
I think Lino hit the mark pretty well. Silver Chloride will darken in sunlight. Lead Chloride is soluble in hot (boiling or near boiling) water.

If either fails to establish what the crystals are, you will need to answer many more questions regarding feedstock and process.

Time for more coffee.
 
My guess, lead chloride. It forms long thin needle-like white crystals. Dissolves in hot water.

Forms a white precipitate of lead sulfate if you add a bit of sulfuric acid to a solution.

Could there have been lead solder with the source material? Did you add sulfuric acid before filtering the aqua regia?
If you answer yes and no, then I think it's quite certain it's lead chloride.

Göran
 
Thanks everyone for your help. Based on your comments and further research, it must be lead chloride. I originally used hot tap water. I'm not sure how it got into my gold solution though. Back to Hokes. Thanks again guys.
 
Hey guys (and gals),
One question, if anyone can comment and help -
Watching several refining videos, I've seen the importance of removing all the "base" metals from gold-coated material (non-jewelry) first then using AQ-R to further refine the Au foils once all the base metals are dissolved.
But I recently viewed one video where they took gold-coated pins, etc., and treated initially with AQ-R AND (after dropping with SMBS), they ended up with 23.6 Karat Au. How is this possible? Wouldn't most of the base metals get dissolved in the AQ-R and then also get dropped with the Au?? Unless they left out some details, I'm a little confused how this is possible. I mean, why bother properly removing the base metals if AQ-R will selectively remove the gold coating, right?
Any guidance would be appreciated.
Thx,
Buckly
 
The reason you try to eliminate as much base metals as possible is because it's always easier to get a clean product from a smaller sample. It's also a way to keep the amount of waste down, making it easier to treat the waste properly.

Of course, there is a golden middle way to go, you have to know when it's time to switch method. It will differ between different persons and their situation. What works well for me is a waste of time for Jon. It's something you learn over time.

There are two main reasons the gold can come out more or less contaminated after a refining cycle, bad filtering and mechanical drag down. If you still have solid particles as silver chloride that pass through the filter it can end up in your gold. Then there is the mechanical drag down. When the gold precipitate it will lock some of the original solution between the particles and some can be stuck on the surface of the grains.

So a dirty solution with a lot of base metals will produce dirtier gold. Some of it can be mitigated by proper washing techniques but the easiest way is to have a pure and concentrated gold chloride solution before you precipitate the gold.

You also have other sources for contamination as dirty lab ware, dirty melting dish, even the torch can contaminate pure gold.

The skill of the refiner shows off in the purity of the product. I've seen Nick taking pure crap and turn it into a shining bar in one step. It was a joy to see him work. :D

I thought I had a handle on it, but my twice refined, first shot for a big button turned out to have palladium contamination. It took me a third refining cycle to get the purity up to where I was happy about it.

Göran
 
OK, thx for the replies - very helpful
So, let's say you have "dropped" a dirty solution.
Is there a way to take that "brown mud" (hydrated Au) and re-refine it then or is it too late?
 
Simple. Redissolve the "brown mud" in a minimum amount of AR (aqua regia - I've never seen it referred to as AQ-R before). Then drop again. For a cleaner drop, use a different precipitant the second time. Many use ferrous sulfate for a first drop from dirty solutions, then SMB for the second drop. Since you already used SMB, it's fine to use it a second time. Just use the minimum amount of AR to dissolve, and a minimum amount of precipitant.

Please avoid the use of text lingo like "thx". It can cause problems for our members who have to use translators to read the forum.

Dave
 

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