# My first Gold, not too pretty but beautiful to me!



## TomVader (Apr 16, 2013)

Refined an assortment of 10k and 14k jewelry. Calculated the weight so that I would end up with 1TOz, I was a little off. I realized that when I did my inquartation, some bits of alloy were stuck to the inside of the crucible. I assume that would account for the missing gold. Those scraps will go into my next batch. The black specks on the surface I think are bits of graphite from the crucible, at least I hope so because if they're not, I don't know what they are! I know everyone says this, but I want to express my gratitude to the members of GRF for the excellent information posted here. The Safety section of this forum quite likely saved my life (or at least my lungs). I was ready to start making nitric and refining before I stumbled upon this forum and started reading the Safety section. It gave me a clearer understanding of how dangerous some of these chemicals can be and what precautions MUST be taken. I would especially like to thank Butcher, Lazersteve and Kadriver.
Besides sending my gold out for assay, is there any way to get an idea of it's purity? Thanks in advance.


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## its-all-a-lie (Apr 16, 2013)

Boil it in nitric for 20-30 minutes, that will clean the surface and make it look better.


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## nickvc (Apr 16, 2013)

Your button looks a little off colour but it could be the flux stuck to it. Did you just inquart and then melt or did you inquart and then put the gold through AR? Either process if done correctly should give you 95%+ purity but with AR you can get 999+ gold if you follow the process correctly and do the rinses advised by Harold V. The most common contaminant from gold karat scrap refining is usually silver which can be in solution but will drop out if you chill the solution and then filter it out and the rinses should then remove any remaining silver and copper that have been dragged down while you precipitate your gold. If you want really pure gold then a second refining should produce a good finished product but it's easier to do from the powders than a melted button but if you intend to refine more then just use this button at the end of the dissolution stage to consume excess nitric, it's another of Harold's tips.


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## Anonymous (Apr 16, 2013)

What material and what amount of material did you use to get that?

From looking at the button, it seems that you haven't filtered your solution good enough or you skipped over the sulfuric acid drops to get rid of the lead.

It looks nice as a refined button, but it doesn't look as nearly as pure as many buttons or gold bars I've seen so far here from the members here.

Tell us more about what you've done to get that button.

* Did you use a clean or a used gold melting dish?

* A crucible is not used for inquartation. A crucible is used to pour the molten metal in or (unless it's a graphite crucible used to do the melting.. electric or possibly gas furnace). I believe you mean melting dish. If I'm wrong, someone will correct me.

If it was me, I'd redo the button.

Kevin


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## artart47 (Apr 16, 2013)

Hi Tom!
Good job on the button. You lucked out on the safety section! Commend you on your mentioning it in your post. I try to put it in with anything I post dealing with chemicals.
I'd hate to think that some beginer getting injured because of reading something I wrote and trying it
If you process the button back to powder, look up Harold's washing instructions. I have gold powder that I've refined twice, did the Harold wash and it still has a dark film on it. From searching and reading posts I believe it's silver contamination so, my next step will bw washing it in nitric acid to see if dissolves.
Good luck artart47


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## TomVader (Apr 17, 2013)

Testerman you are amazing! I did skip the sulfuric to precipitate lead and I'll tell you why... after I inquarted (I used an electric furnace with a graphite crucible) and gave the alloy a series of hot nitric baths (until the liquid was nearly clear) I rinsed twice in D-water, then went on to AR. My nitric is homemade (from Lazersteve's formula) and distilled, so I don't know it's concentration. I wanted to avoid the problem of excess nitric so I proceeded as if my nitric was 68%. I added HCl and then added nitric in small increments on gentle heat. The first addition was only 20ml but produced a vigorous reaction. When everything had settled down I could see that there was still a considerable amount of gold still undissolved. I added nitric again, same result. Added again... for some reason all of the gold would not go into solution. I added even MORE nitric. By the fifth addition I realized I had gone too far. I let this sit overnight. The next day, my solution was a beautiful deep yellow but still had quite a bit of black powder in the bottom. I started out with gold sponge, and now it was powder, had it dissolved and then somehow spontaneously precipitated? I added MORE nitric, no change. I reasoned that if I used sulfuric to preciptated the lead, that it would just fall on top of my gold, so I skipped it altogether and just added the sodium metabisulfite (32g in enough D-water to dissolve it). It produced a violent reaction but no precipitation. (too much nitric). So I nuetralised with urea and added more SMB. The next morning my solution was crystal clear and tested negative with SnCl. All the gold was in the bottom of the container. I decanted and washed three times with hot D-water, dried and melted. It was when I went to melt it I noticed some tiny BBs of 6k alloy stuck to the bottom and sides of my crucible. I scraped them out and went ahead and melted my gold. I can see my mistakes in hindsight. I should have decanted my AuCl, precipitated the lead, then poured it back onto the undissolved gold powder. I should have used a clean crucible for the gold (I have a new one on the way!) I think I will use this button as a way to use up excess nitric as suggested. Thanks for all your interest and thanks for looking!


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## Anonymous (Apr 17, 2013)

TomVader said:


> Testerman you are amazing! I did skip the sulfuric to precipitate lead and I'll tell you why... after I inquarted (I used an electric furnace with a graphite crucible) and gave the alloy a series of hot nitric baths (until the liquid was nearly clear) I rinsed twice in D-water, then went on to AR. My nitric is homemade (from Lazersteve's formula) and distilled, so I don't know it's concentration. I wanted to avoid the problem of excess nitric so I proceeded as if my nitric was 68%. I added HCl and then added nitric in small increments on gentle heat. The first addition was only 20ml but produced a vigorous reaction. When everything had settled down I could see that there was still a considerable amount of gold still undissolved. I added nitric again, same result. Added again... for some reason all of the gold would not go into solution. I added even MORE nitric. By the fifth addition I realized I had gone too far. I let this sit overnight. The next day, my solution was a beautiful deep yellow but still had quite a bit of black powder in the bottom. I started out with gold sponge, and now it was powder, had it dissolved and then somehow spontaneously precipitated? I added MORE nitric, no change. I reasoned that if I used sulfuric to preciptated the lead, that it would just fall on top of my gold, so I skipped it altogether and just added the sodium metabisulfite (32g in enough D-water to dissolve it). It produced a violent reaction but no precipitation. (too much nitric). So I nuetralised with urea and added more SMB. The next morning my solution was crystal clear and tested negative with SnCl. All the gold was in the bottom of the container. I decanted and washed three times with hot D-water, dried and melted. It was when I went to melt it I noticed some tiny BBs of 6k alloy stuck to the bottom and sides of my crucible. I scraped them out and went ahead and melted my gold. I can see my mistakes in hindsight. I should have decanted my AuCl, precipitated the lead, then poured it back onto the undissolved gold powder. I should have used a clean crucible for the gold (I have a new one on the way!) I think I will use this button as a way to use up excess nitric as suggested. Thanks for all your interest and thanks for looking!


Another thing you skipped on was the HCL bath after the gold dropped. In order to get your gold as pure as possible, you can't just wash it with distilled water. You have to use HCL first, then the distilled wash.

Also, you don't use gold to get rid of excess nitric. You will be better off using silver, which you can recover later on.

If it were me, I'd put the button in a AR bath, and then go from there. This time make sure to use the sulfuric acid, and then after the gold drops, use the HCL to wash away some other metals that may have gotten this far. Your 2nd wash of HCL must be heated for about 5 minutes. After that, wash well with distilled water. After that, dry it out, and on to the melt.

Kevin


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## Anonymous (Apr 17, 2013)

I received a pm from a member and I was advised that gold is the recommended method for using up the excess nitric acid (told it's Harold_V method and others agree). If that is so, then I need to edit my last reply.

On the same note, I know that nitric acid doesn't dissolve gold by itself. It'll do it if you make AR (HCL+Nitric). I am still learning, but I don't understand gold being used to get rid of excess nitric when a less valuable metal can be used (silver, or even copper).

Anyway, I'll definitely check into this and if I'm incorrect, I'm sorry for giving wrong information. 

Kevin


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## TomVader (Apr 17, 2013)

I'm pretty sure they mean excess nitric IN aqua regia, after gold sponge is dissolved, before precipitation.


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## TomVader (Apr 17, 2013)

...in that case you wouldn't want any more base metals in solution.


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## g_axelsson (Apr 17, 2013)

testerman said:


> I received a pm from a member and I was advised that gold is the recommended method for using up the excess nitric acid (told it's Harold_V method and others agree). If that is so, then I need to edit my last reply.
> 
> On the same note, I know that nitric acid doesn't dissolve gold by itself. It'll do it if you make AR (HCL+Nitric). I am still learning, but I don't understand gold being used to get rid of excess nitric when a less valuable metal can be used (silver, or even copper).
> 
> ...


Kevin, let's do a thought experiment.

If we start with a solution of relatively pure gold (inquarted or foils from fingers for example) dissolved in aqua regia with an excess of nitric, lets check what would happen if we added different metals...

Add copper to that solution... we would get copper to dissolve, adding extra copper chloride to the solution. We would also cement some of our gold until all the copper is consumed. In the end we have gold powder mixed with other solid materials that didn't dissolve (like silver chloride, lead chloride, tin oxide ...) In the solution we have all our copper chloride that will contaminate our gold via drag down, producing a less pure end product when we drop the gold in solution. Not good!

Add silver to that solution... well, silver in aqua regia would not dissolve, it would be covered with a thin surface of silver chloride and then the process would stop. It just wouldn't work.

Add an even less noble metal than copper... basically the same thing as copper but faster. We would also cement copper with the gold powder. In the end, just as bad as copper.

And finally, add a solid gold button to our aqua regia solution... the gold will be dissolved, adding gold chloride to our solution. It will stop dissolving when the nitric is consumed. If we need to know how much extra gold we have added, just weigh the button before and after adding it to our solution. We can easily recover the gold that didn't dissolve and we don't add a lot of contaminates to our gold chloride solution that would contaminate the gold we drop in the end.

Kevin, I hope you now understand why we don't use anything else than gold to use up the excess nitric in aqua regia.

Göran


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## Anonymous (Apr 18, 2013)

I guess that does make sense. I'm so used to refining silver and I've refined gold just 2 times so far and made AR just 2 times so far. Since I don't have much gold refined yet to use for neutralizing the nitric, I know it's best to not use too much nitric in the first place. Just use a bit at a time.

Kevin


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