seperation issues :hno3

[bgp_scrap]

Hi, everybody
First off, the problem. I have a,larger beaker (maybe 200-400ml mason jar) of seperated,solution
Black oil like on top, what,looks like gold dropping out of solution and in the bottom, light brown flakes/chunks and powder.
Now, what ive done :
I soaked some "gold plated" snake chains in hno3 to remove base,metals from the gold. Well these chains turned out to be toned, not plated.
But the solution was pregnant aqua regia colour.
I did not test with stannous chloride.
Instead, as they were toned I figured the balues were so small id just filter(no.2 cone coffee filters in a silicone funnel) after diluting with 1/2 water.
It caught a few flakes, so I took solution and added nacl (as suggested by hokes, to drop silver chloride)
Let it sit 2 hours, no colour. (would have let it sit over night if values started forming)
so. In confusion I forgot about stannous, and added copper as a way of consuming nitrates and cementing ant possible values. It started droping black/brown(no silver) values. I let this sit until no further reaction occured, and let it rest. The values floated to the top of the jar but a brown powder formed on the bottom( usual gold powder look) and between is,the usual regia/smb colour. So I added smb(for? The reason im unsure of myself in retrospect) yo ensire all values dropped. Thst created more black cloud that settled atop the solution, after sinking to the bottom( smb instantly turned red/brown very little reaction, no noticable fumes.)

Amybody ever have this happen? Will post a,picture shortly.

 

[bgp_scrap]

Okay hold on here... When I added nacl. I introduced cl to solution allowing aucl2 to form... Cemented by the copper and smb would infact drop now,in solutiob values,thanks to smb..... Solved that..
Now.. Why has it settled on top *insert confused,face*
Guess I answered 2/3 of it myself, but did I just find a poor mans hcl/ar? By introduction of cl to hno3?....

 

[bgp_scrap]

Heres the picture

 

[Claudie]

It is hard for me to understand your question, or even what you have done. How did you get AuCl2 when there is no Gold present? Solutions can have many colors because of the metals in them, but you cannot identify which metals by the color of the solution alone.
Nitric acid alone will not dissolve Gold, but even if it could, how would the solution contain Gold that was never there to begin with?
The base metal of the chain could have been anything from Aluminum to who knows what, then you added Copper, so we know that's in there.

My experience using Nitric acid is limited, so my advice to you is to stop adding anything to the solution and wait for a more experienced member to help you out.
I wouldn't be working with Nitric inside of a building without using a fume hood.

 

[g_axelsson]

I would say you got nothing except maybe a few cents worth of gold flakes in the filter.

What you should do is to read a lot more and do the acquaintance experiments in Hoke.
How do I know you haven't done it yet? Well, your description of getting the silver tells me that. Silver nitrate + sodium chloride... you can't mistake that reaction. If you don't get it then you don't have silver in solution.

Treat your toxic mess as waste or deposit it safely at a collection center.

Göran

 

[bgp_scrap]

Thanks, however.
I have done many of the acquaintance tests. And ive used nacl many times to to obtain values, and as hokes suggests using sulferic in a ratio to water of 1:10-20. Ive also done quiet a few copper cementations.
Allow me reiterate my question in laymens terms
Will nacl+hno3 react to produce a "poor mans" regia dissolving what gold there was into solution as aucl2.
Second of all. Why did it seperate.
I seek not an arguement merely answers to my direct questions. Do not confuse this with ignorance or arrogance, as ive done several successfull batches of material and a successfull melt for each batch,( now upwards of 1toz gold, along with a 1/4toz platinum group and 2-3 toz silver) . I've just never seen it seperate like this.

 

[bgp_scrap]

Claudie: thanks.
But of course I always work outside, I moved the jar,into my shed over night as my town isnt exactly full of role model citizens.
Unsure if there was gold or not, but the copper cemented something out.
As far as the object in question goes I wad told it was gold filled, turned out to be toned, which is like.. If im correct 1-3 microns? Enough to colour it.
I have a fair bit of experience with hno3, bit I know to make regia you add small amounts of hno3 to hcl, I just wasnt sure if adding salt(nacl) would cause,the,reaction and dissolve what little gold was there into solution.
Thanks for the advice you could offer with your experience.
Im hoping somebody can tell me why this solution has seperated. As thats my main concern. If theres nothing in the solution it will be treated as waste, was prepared to waste it but wanted to make sure I wasnt missing something first.

 

[Claudie]

For someone with your experience, I am surprised you didn't use Stannous Chloride for testing. It is my understanding that Gold toned is a color, not real Gold at all.

 

[bgp_scrap]

Yup, my tin salts are another 2 days in the mail along with the rest of my stock. Just using up whats left of the nitric to get a few foils stocked up lol I did forget. But it came along side being out of it.
Ive been told goldtone is like 1 micron or so. Literally just enough to make it look like gold. You still produce flakes/foils. But such a miniscule amount, so ive experienced anyways. That its not worth your acid cost.

 

[FrugalRefiner]

Ive been told goldtone is like 1 micron or so.

It's more likely a microinch or two, not a micron. One micron = 39.37 microinches.

Dave

 

[Harold_V]

Im hoping somebody can tell me why this solution has seperated. As thats my main concern. If theres nothing in the solution it will be treated as waste, was prepared to waste it but wanted to make sure I wasnt missing something first.

I'm surprised that if you have the experience you claim, that you have not tested with stannous. Doesn't matter what anyone says on this board in regards to what you may or may not have in solution, for even if you started with something of value, there's no guarantee that it remains in solution, considering what you've been doing.

Test with stannous that is known to be good and functions properly. To ensure that, you should have a small amount of gold standard solution. If the stannous responds to the test positively, using the standard solution, you then can use the stannous with confidence on your unknown solution. Assuming it has little to no free nitric, the resulting test should indicate if there's any values present, or not.

I will NEVER understand why anyone dissolves gold and does not test the results. Without a stannous test, you really have no clue. Sorry, but that's how it is! I refined for more than 20 years, thousands of ounces of gold and silver, a generous amount of platinum and palladium. To my last day in the lab, my stannous chloride as well as my DMG was used regularly. I assumed nothing.

Perhaps that's a lesson you need to learn.

Harold