# 29.9 gram. How did I do?



## qst42know (May 26, 2011)

From karat scrap, I just don't find much e-scrap. Twice refined and powder washed by Harold's wash routine (Thanks Harold!).

Makes the 14k ring look very pale.


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## Claudie (May 26, 2011)

That is a very nice looking piece of gold. :mrgreen:


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## jimdoc (May 26, 2011)

Very nice indeed.

Jim


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## dtectr (May 26, 2011)

the crystallization & fern-like pattern says PDP (pretty Darn Pure) to me!


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## adam_mizer (May 26, 2011)

Wow a real beauty both sides, appears very pure.
I'd say you did greeeeaaaatttt!


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## floppy (May 26, 2011)

Absolutely gorgeous! Congrats


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## Harold_V (May 27, 2011)

Looks very nice! Great job of processing. 

I'm impressed with the form. Did you pour to a round mold? Bottom side is exceptional (very nice corner radius).

Harold


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## Oz (May 27, 2011)

Nice job QST.


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## qst42know (May 27, 2011)

Harold_V said:


> I'm impressed with the form. Did you pour to a round mold? Bottom side is exceptional (very nice corner radius).
> Harold



I allowed it to set up in the melting dish but there was just a little bit more borax than was absolutely necessary, the surplus pooled slightly around the edge. It made it difficult to pull from the dish much like a strong suction cup.


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## Anonymous (May 27, 2011)

Very nice indeed! All of my gold has been incredible purity,since I have been refining twice.And its not that hard is it? 
Your nugget has awesome character!


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## Fournines (May 27, 2011)

Looks like gold! Good work.


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## Harold_V (May 27, 2011)

qst42know said:


> I allowed it to set up in the melting dish but there was just a little bit more borax than was absolutely necessary, the surplus pooled slightly around the edge. It made it difficult to pull from the dish much like a strong suction cup.


Amazing. I melted countless buttons in that fashion---don't recall, ever, getting one to come out as nicely as that one did. Very well done!

Harold


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## qst42know (May 27, 2011)

I'm certain this wouldn't look anything like this without the knowledge shared by all the smart helpful folks on the forum.

Thanks All. :mrgreen:


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## HAuCl4 (May 31, 2011)

8) :shock: 8)


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## qst42know (Jun 26, 2011)

I haven't seen this before, pipe on the bottom?

Anyway in the same dish with to much borax I added a pinch of soda ash, thinking it would thin the borax and aid in pulling the button from the dish. It worked, the button lifted easily but with some side effects. It produced a mirror finish on the bottom as well as the pipe. I really like the fern like patterns on the bottom. 8) 

The blue gray streaks in the photo are the clouds in the sky at the time.


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## Anonymous (Jun 26, 2011)

qst42know said:


> I haven't seen this before, pipe on the bottom?


I've had some that had "craters" in the bottom.However I believe this was created from the gold boiling,then air pckets being trapped under it.It's only happened a couple of times.Now I keep my heat much lower,and I don't tend to see it as much.Of course I could be wrong.


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## qst42know (Jun 26, 2011)

I don't believe it was boiling, and I'm certain it wasn't stuck. It was melted in a dish setting on a fire brick. By moving the brick slightly without lifting I had the metal spinning in the dish like a marble in a bowl.


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## Anonymous (Jun 26, 2011)

No I meant my gold was boiling,not yours.The pipe you have there on the bottom is tiny compared to the ones I had.I am positive my gold was boiling,I am just not positive that is what created such a large cavern on the bottom of a few of my buttons,although it would make sense.


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## Harold_V (Jun 26, 2011)

I question the wisdom of using soda ash when melting your gold. 

My comment may be controversial, but the reaction one experiences when cleaning a melting dish leads me to believe that soda ash results in trapping contaminants in the gold instead of allowing the flux (borax) to remove them from the molten gold. The oxides that are normally removed are, instead, reduced, so the resulting metal alloys with the gold. That explains the lustrous surface, which would normally be slightly hazed by oxides. 

Harold


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## qst42know (Jun 26, 2011)

I had wondered if the soda ash would cause issues. 

The first time I melted this batch it looked like this.

The accumulation of my earliest experiments before I had acquired any DMG to test for palladium. Digested again it tested positive for palladium.

Being the root of many experiments I attempted to recover the palladium with DMG. You weren't kidding Harold akin to working with grease, or perhaps anti-seize or ink. Then refined a third time I was reasonably certain there wasn't anything left to cause issues with soda ash, perhaps a trace of palladium but I couldn't detect any with DMG.

Many lessons learned from this bit of gold. :mrgreen:


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## Anonymous (Jun 26, 2011)

Yes,this discoloration is usually a result of,either soda being introduced,or the button being completely covered in liquid borax (flux),when it cools back to a solid.When the button is covered over in flux,the base metals are not able to oxidise,from the lack of exposure to the oxygen in the air,therefore,will stay agglomerated with the gold(for the most part).


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## Oz (Jun 26, 2011)

I agree that soda ash does not belong in your melting dish unless you are cleaning it. 

If you have precipitated your gold once and suspect Pd contamination, redigest it. Then something easier than removing the Pd with DMG is to leave the Pd in solution when precipitating your gold. SO2 gas/SMB precipitates Pd very effectively with your gold or without it from chloride solutions. Using oxalic acid as your gold precipitant the second time around works very well for leaving the Pd in solution.


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## qst42know (Jun 26, 2011)

The original discoloration was from a considerable amount of palladium as a contaminant, melted with no soda ash. 

I won't be trying DMG again I just wanted to attempt it once. Ammonium oxalate is by far superior like an insanely beautiful snow globe. I do love the crystalline sponge it precipitates.


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## Harold_V (Jun 27, 2011)

qst42know said:


> Many lessons learned from this bit of gold. :mrgreen:


It's obvious from the surface color and texture that the button is contaminated. May not be by much--but when you're shooting for 4n's, it's way too much!

The test with DMG is extremely sensitive--minute traces are well defined, especially if you test in a spot plate and allow a little time for the resulting material to agglomerate. 

If a test (with DMG) shows no further palladium, you may look elsewhere for contamination. A re-refining, using clean nitric and HCl will often result in a good display of the contaminating metal, but in solution after precipitation. 

I screwed around with my gold for a long time, trying all of the "tricks" that are reputed to help bring up the quality when it's borderline. My conclusion was that they were, for the most part, a waste of time. By the same token, is one chooses to use potassium nitrate and a full flux covering, results will indicate some improvement, but don't lose sight of the fact that a full flux cover will disguise (absorb) oxidation, leaving one with a false indicator that there are no base metals present. That most likely won't be the case. 

The best results I managed to achieve, based on the resulting pipe, color and clarity of the surface, was by refining a second time. It has an amazing ability to lower trace contaminants. Needless to say, that should always be followed by extensive washing. 

It doesn't take long to come to terms with the notion that DMG isn't a good idea for use as a precipitant. The sheer volume created makes it a bad idea, to say nothing of the difficulties in handling the resulting palladium. I can't think of a better way to express the material than the one you chose ---greasy. It sure as hell is!

Harold


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## etack (Jun 27, 2011)

i was trying to find out what Ammonium oxalate was and I think this is the shortest Wikipedia description ever. http://en.wikipedia.org/wiki/Ammonium_oxalate


Eric


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## qst42know (Jun 27, 2011)

etack said:


> i was trying to find out what Ammonium oxalate was and I think this is the shortest Wikipedia description ever. http://en.wikipedia.org/wiki/Ammonium_oxalate
> 
> 
> Eric



It's in Hoke under "Alternate methods" (oxalic acid solution to which an amount of ammonia has been added), and part of Lou's ultra high purity post.

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=39&t=3079&hilit=ultra


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