first melt newbie problems

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nickton said:
Well I finally got a small button, but it's not quite gold colored. Looks more like white gold. Now I don't know how to get rid of the silver color.
Refine it.

A frugal approach would be to use it when you have excess nitric acid in some AR in the future. You can add your button to use up the excess nitric, and kill two birds with one stone.

Dave
 
Ahh yes. Good idea. Well I had another go at it today on my original batch from ram fingers and after re-refining it what do you know: Success! My first pure gold. I almost can't believe it:
...now if I can figure out how to make it look a little neater... I guess that will come in time. Some of it appears to be still caught in the crucible as well. Perhaps I used too much flux? I tried Rachel's recipe of sodium bicarbinate, glass, and borax. Seemed to work good except I couldn't get it to flow into a perfect pool. :D :!: :G
 

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I’d say not enough heat looking at your photos so insulate your crucible and it should melt much easier and produce a bead rather than a blob.
 
Thanks for all the replies and suggestions. Well spotted Geo, I lied, I actually melted a piece of copper that was sitting in unknown pgm chl, I think. I haven't been able to reproduce gold of that quality so far, it barely got flakey after several minutes of Puritest 10k test acid, but I think my problem is Palladium based on stannous, which isn't the worst problem. As for Au dust, I think I'm making nanoparticles because they go right through a coffee filter and very slowly coalesce to brown yellowish dirt, but even that seems to have Pd. I can't seem to find a complete reactivity series for noble metals or a table of what does and does not form complexes with ammonia and the same for glycine, if anyone has access to those gems of scientific knowledge I would be grateful to know. Today I dropped some hydroxides from chl, any ideas on what these two colors might represent?
In my ignorance I'm thinking Iron and Pd as the chl was made by soaking pgm plated copper in hcl and simultaneously, for no good reason, replacement rxn plating a pair of tweezers. So my theory is practically only the Pd dissolved in the hcl which then replaced iron while I slept leaving a heck load of iron and some Pd in solution.
 

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baby_beans, I think you should find a different hobby. This is not the type of pursuit to do things "for no good reason". It's a good way to hurt or kill yourself or those around you.

Dave
 
I do everything outside and usually while holding my breath, but yes there are toxic aspects, thank you for your concern. I also drink a lot of glycine in water which may help detox heavy metals, might be good for everyone here to research.
 
I filtered some of the yellow hydroxide, precipitated from the mother liquor in a different vessel, added about 30 drops of hcl (hardware store muriatic) and tested the resulting dull yellow chloride with stannous and only got a weak teal/Pd, I can't do Rhodium stannous because I lack a borosilicate test tube at the moment so I tried cementing it onto a dime and test with Pt test acid. The dime is still shiny silver colored after a little buffing but an untreated dime dissolved down to the copper in less time. Rhodium? Just Pd? Should I just get a new hobby? (Jk, I won't)
 
I sometimes think I’m repeating myself endlessly on the forum but here I go again.
PGM salts are highly toxic and can and will kill and are absorbed through the skin and by inhalation so while this might seem like fun research platinosis before you continue, it’s a cumulative disease so you never know when it will strike until too late. To be working with PGMs you need a proper hood and a scrubber and decent gloves at the very least and a very good knowledge of the chemistry of them, please be very careful when messing with them.
 
I agree with nickvc. PGM's is the basis for the most common chemotherapy drugs used in cancer treatment. It is very toxic to all living things in an ionized state. With that being said, there is an obvious flaw to your approach. Trying to dissolve a noble metal with acid in the presence of a higher reactive metal, like copper, will simply put copper in solution while leaving the noble metal intact. Look up the electromotive series of metals. In an acidic environment, the most reactive metal will dissolve first. That's why you can't strip gold from gold plate with acid.
 
Yes, highly toxic, I know. I have a few years of organic chemistry under my belt dealing with even more deadly compounds. Doesn't scare me, life is but a dream anyway. That being said, for the environment's sake I don't use nitric (except a drop here and there for testing), any sulfur compounds, or cyanide. Pd chl is 90% excreted in a normal human in 3 days, add glycine to the diet and that number should increase. I will certainly invest in a fume hood and scrubber if I'm able to make a profit and I continue to involve myself in PGM extraction.
This endless discussion about not attempting to make money because it might be dangerous sort of comes down to the economy. America has less social mobility than Medieval Europe. People are doing life threatening things everyday to try to save their families from a lifetime of struggling financially because we have a corrupt joke of a "judicial" system. Some people would rather die knowing they tried rather than just going along to get along like a worm.
The copper was electroplated pretty thick with nobles, I imagine after some amount of deposition acids can't attack the base metal, may be wrong there, and the iron bit wasn't added until after the solution turned golden (not my understanding of Cu reaction with hcl)
Attached is a picture of a drop of stannous on the alleged PGM chl salt. Maybe someone could help me by giving an opinion on what its showing? None of these pictures come from the inside of a house or even a building within 100yards of a residence so rest assured precautions are being taken. Stannous chl is loudwolf brand purchased online.
 

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So when you test, one drop to one drop. Using one drop on a soaked paper is really hard to interpret.

What is chl? Are you saying chloride? Just us Cl, or spell out chloride. It's important.

baby_beans said:
This endless discussion about not attempting to make money because it might be dangerous sort of comes down to the economy. America has less social mobility than Medieval Europe. People are doing life threatening things everyday to try to save their families from a lifetime of struggling financially because we have a corrupt joke of a "judicial" system. Some people would rather die knowing they tried rather than just going along to get along like a worm.

Look, I'm not going to disagree with you. In fact, I will completely agree on the financial situation in this country. My dad was a custodian, my mom was an office manager, I dropped out of college as a senior. BUT...I'm busting my butt to do things as close to correct, and as properly, as possible. Because in order to climb that ladder of social mobility, you have to move past doing this in buckets and tupperware on your picnic table, holding your breath...and learn how to do it properly. You don't make real money doing it in a small fashion, and you always have everything at risk. You need reasonably good ventilation in a controlled atmosphere, or you are best off not doing it all. You make the investment, call it a hobby...and if it seems like it can pay off, you just keep investing.

Geo said:
Definitely a lot of copper.

Not necessarily, even though I think he's now said it was? I'm personally having trouble following this thread.

But...a small amount of contamination can cause what appears to be copper. I just sold a button yesterday that assayed at 98.75 Au and the outside was red. In fact, I was quite annoyed because I gave them three buttons that were all beautiful, and what came out of the crucible had all of the junk on it. In fact, I was quite annoyed as I also dumped a bunch of silver, and was left to stare at an ugly lump of gold while I waited for the silver to melt. Well, it turned out that it was all surface contamination.
 
Thanks for that reply, the stannous in that picture is on dried salt not solution. Chl is an abbreviation for chloride, yes. It might be an ochem ppl thing. I have fantastic ventilation, I promise, and I agree with everything else.
 
Did a drop of pgm chloride and a drop of stannous, and a picture of what's happening to what was a piece of steel wool. Melting point seems high I can get the sponge to fuse a little but then it just sits there glowing. Dropped in AP some shiny yellow metal remains so far, I'll try just AP on the sponge when it stops growing.
 

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I use white plastic spoons to test. They are cheap and disposable. The white background shows any color change. The spoons are collected in a container and incinerated periodically. Pd testing with stannous chloride will give a slightly reddish reaction at first and then slowly turn green after a few minutes. Not an even color green but increasing green toward the center of the drop. Some people describe it as rainbow colors because several different shades can appear. You should get some known metal and practice testing solution to get familiar with the results.

Copper melts different than gold. The color, the texture of the metal, the graininess of the surface can all give clues as to what's in a melt. If you do it enough, you will see the difference. Nothing beats a conclusive test but casual observation can give you something to go by.
 
I'd also recommend that you do a bit better job of both photographing your results, and describing what you are doing...starting with the material you are refining or recovering from, then listing steps you are taking including what chemicals you are using.

I for one can't make heads or tails of what you are doing.


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That background is white snoman, not sure how it could be whiter. My LG camera absolutely sucks though and only has auto white balance. After about two hours the brown part disappeared leaving just a teal stain. Starting material is unassayable ore, that's all I'll say about that. I'm going to go with Pd/Au based on AP leaving a bit of brown/black dirt(hard to tell through green solution) I sent a few grams to a refinery based on a positive stannous test so I will see what happens there. Afaik the only false positive Stannous gives is after the addition of sulfur compounds and its dark brown not teal. To obtain the hydroxides I slowly added NaOH to aqueous Cl solution of suspected PGMs. I read somewhere that can be used to assay but my phone apparently got hacked because it self deleted several textbooks and pdfs. Very annoying.
 
Typical palladium reaction with stannous.
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Stannous dropped on the tip, yellow is the unreacted solution.

Göran
 
g_axelsson said:
Typical palladium reaction with stannous.

Stannous dropped on the tip, yellow is the unreacted solution.

Göran
And it doesn't dissipate.


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