first melt newbie problems

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baby_beans
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first melt newbie problems

Postby baby_beans » June 19th, 2018, 10:05 pm

I think this a good sign in the melting cup after rather a lot of borax was melted with unknown PGM recovery dust. But I'm completely new to this, is this possibly just copper or tin? Thanks.
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Re: first melt newbie problems

Postby kernels » June 19th, 2018, 10:34 pm

Where did the PGM dust come from ? It isn't really possible to tell you what it could be without knowing where it came from.

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Re: first melt newbie problems

Postby denim » June 19th, 2018, 11:07 pm

Looks like a satellite picture to me.

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Re: first melt newbie problems

Postby baby_beans » June 20th, 2018, 12:32 am

A method I'm exploring where electronic waste is converted to mixed hydroxides then rinsed with ammonia leaving hopefully only second row transition metals, then melted, poorly

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Re: first melt newbie problems

Postby baby_beans » June 20th, 2018, 2:15 pm

Sorry, all but first row, I have no plan of attack to remove Hg so far and I'd not like to remove Au


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Re: first melt newbie problems

Postby baby_beans » June 20th, 2018, 8:17 pm

Finished lump
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Re: first melt newbie problems

Postby Geo » June 20th, 2018, 11:01 pm

Definitely a lot of copper.
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Re: first melt newbie problems

Postby Smack » June 21st, 2018, 7:19 pm

Looks like you need more heat.
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Re: first melt newbie problems

Postby baby_beans » June 22nd, 2018, 2:42 am

Thanks for all the replies, I tried more heat, pretty happy with the color
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Re: first melt newbie problems

Postby Rachello » June 23rd, 2018, 2:39 am

Baby,

So many times I thought I would get a better melt than I did. It looks copper, but so does rose-gold.

One thing you can do is re-melt & smelt.

I “scrub” all gold I refine b/c sometimes that is all it needs to cross the point of “worthwhile”.

One technique I use is something bought in your local Home Depot...Spectracide stump remover. It is a potassium nitrate. Some will argue it can contaminate your melt with copper. I have found the opposite. If your melt consists primarily of gold it will “cleanse” it.

It will flame a brilliant white & burn off many lesser metals on the periodic table.

I use it religiously, just in case or to bring a nugget over the bar.

Hope this helps :D

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Re: first melt newbie problems

Postby baby_beans » June 25th, 2018, 5:40 pm

Thanks Rachel, nice signature also. I read that borax does basically the same thing but I read it on Wikipedia, so who knows if its true. I did burn off a bunch of green and blue flames but I doubt one can hit 100% of the copper

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Re: first melt newbie problems

Postby Geo » June 25th, 2018, 11:45 pm

You can't refine by fluxing. It can be argued that any concentrating of your target metal is refining but it is a general consensus that a certain percentage should be expected to call it refining. Did you put the button in acid to remove impurities from the surface or clean the button in any way? I don't see how just heating would have made that big of a difference in the color.
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Re: first melt newbie problems

Postby boarteats » June 26th, 2018, 1:06 am

baby_beans wrote:I think this a good sign in the melting cup after rather a lot of borax was melted with unknown PGM recovery dust. But I'm completely new to this, is this possibly just copper or tin? Thanks.

Great pic! Can't tell you what's in the melt from it, but A+ as abstract art.

Seems to me, the very first thing you need to do is to determine what precious metals (if any) are in your PGM recovery dust. This info will help you to decide on a course of action. For example, you can melt gold with a propane torch. Platinum, not so much. Platinum's melting point is greater than 3200 F.

My suggestion is that you read up on the topic of testing with stannous chloride. Creating/buying stannous chloride is pretty straightforward. This forum has a lot of info on the topic. The more challenging bit is that this test requires that you dissolve the precious metals into solution. There are a few different approaches to this, some safer than others. Again, you'll find these approaches described in the forum.

Good luck!

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Re: first melt newbie problems

Postby Rachello » June 26th, 2018, 7:59 pm

Geo wrote:You can't refine by fluxing. It can be argued that any concentrating of your target metal is refining but it is a general consensus that a certain percentage should be expected to call it refining.


While I agree with your above statement, you can increase purity of a melt slightly by using a flux. While this is no where nearly as drastic as refining it will raise the bar on your button a small amount of several % points. Multiple smelts will increase purity in much smaller increments than the first.

I melted a button the other day that I had tested by XRF & it came back 94.4%. The contaminating metal was copper. I didn’t feel like dissolving it so I melted it with the below flux & let it “cook” for a little bit. I did this 3x. I had the same button re-tested today via XRF. It came back @ 98.7% Au & less than .2% CU.

The remainder was Pd! That will really teach me to mix up my gold crucible with my palladium one! Must have been a couple Pd beads left over :x

Didn’t improve it to 99.9 but definitely helped out some :D it ended up weighing 11.4 DWT

In my flux I use a combination of:
Sodium Bicarbonate
Anhydrous borax
Silica glass

I let it cook for a while & then at the end I use the Potassium Nitrate
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Re: first melt newbie problems

Postby anachronism » June 27th, 2018, 10:46 am

Rachello to be honest I don't recall the last time my gold had that much copper in it at melt.

I prefer to clean the powder thoroughly before melting it. Even from a dirty drop from something like ceramic processors 30 minutes cleaning gives over 99% before even thinking about re-refining it.

That's got to be the quickest easiest option.
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Re: first melt newbie problems

Postby Rachello » June 27th, 2018, 11:41 am

Yup that was why I added to this thread in gold melts I screwed up. It was a heavy black cake that filled a coffee filter up to about 2 inches. I rinsed & let it dry in the filter. Added alcohol & put heat to it.

After melting I realized there must have been something copper ((maybe a small earring) in the middle of the cake & it contaminated my melt.

I always refine as much as I possibly can while the Au is still a powder. The main reason why I tried to improve it with a flux...I was annoyed I melted it & didn’t feel like starting over again!!

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Re: first melt newbie problems

Postby Geo » June 27th, 2018, 12:07 pm

I reclaim the gold in the first dirty drop and then refine the dropped powder. If I'm not satisfied with the color or texture, I may refine the powder again. It is much easier to dissolve powder than larger solids. HCl and sodium hypochlorite (bleach) will easily dissolve powders and the excess oxidizer (bleach), if there is any, is easily removed by heating and stirring. So very easy to work with powders as opposed to heavier solids that it seems ridiculous not to refine dropped powder a second time. Of coarse this is based on the need for purity.
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Re: first melt newbie problems

Postby nickton » July 12th, 2018, 1:53 am

I wonder what the silica glass in flux does.

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Re: first melt newbie problems

Postby Geo » July 12th, 2018, 3:07 am

The silica is absorbed by the flux. When smelting or in certain melting processes, silica is added to the flux to help absorb other impurities.
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Re: first melt newbie problems

Postby nickton » July 12th, 2018, 4:24 pm

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. I think one mistake I made was not putting it into AR solution twice, to re-refine it. I did however add some sulphuric acid so I don't think it has lead. Interesting. :?

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Re: first melt newbie problems

Postby FrugalRefiner » July 12th, 2018, 5:21 pm

nickton wrote: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.

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Re: first melt newbie problems

Postby nickton » July 13th, 2018, 2:45 am

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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Re: first melt newbie problems

Postby nickvc » July 13th, 2018, 2:54 am

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.

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Re: first melt newbie problems

Postby baby_beans » July 13th, 2018, 5:55 pm

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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Re: first melt newbie problems

Postby FrugalRefiner » July 13th, 2018, 8:16 pm

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.

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Re: first melt newbie problems

Postby baby_beans » July 13th, 2018, 8:20 pm

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.

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Re: first melt newbie problems

Postby baby_beans » July 13th, 2018, 8:31 pm

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)

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Re: first melt newbie problems

Postby nickvc » July 14th, 2018, 4:17 am

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.

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Re: first melt newbie problems

Postby Geo » July 14th, 2018, 12:22 pm

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.
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Re: first melt newbie problems

Postby baby_beans » July 14th, 2018, 1:29 pm

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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