1. refining of recovered gold, HCl-wash => coffee brown

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solar_plasma

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I don't know, if this topic is placed correct in Help Needed, since I don't need help, but rather would like to hear some advices.

I have dissolved all´my 7g recovered gold (from my first ceramic cpu experiments to my last more skilled experiments) in AR and used goldbutton method to get rid of excess nitric, though the gold button was not pure,but from my first ceramic cpu recovery. I let it sit for a week with the gold button.

I precipitated with potassium metabisulfite and got a light brown precitation at first, later more dark, almost black. So, obviously and like expected I had some impurities in it.

Then I decanted until the wash water stayed clear and decanted 2 times more.

Finally I let it sit for 2 weeks in 33% HCl, which got a coffee brown colour. This makes me wonder, since the first solution in AR was strongly yellow, as I would expect from a properly done gold solution.

Today I made a first and quick test on q-tips (later I will make better tests on spotplate when I am in the lab) with DMG 1% in alc. and SnCl2-solution, which was old, but still showed positive on my standard gold solution. DMG turned brown, SnCl2 at first yellow, after 30 min almost discoloured but in good light very slightly pink.

Before I go on, I will make fresh and better test solution: DMG/NaOH instead of alc. and fresh SnCl2.

At this point I like to believe the coffee brown colour might indicate Pd/Pt, which ofcourse has to be tested. But my question at this point is, why has it been yellow in AR before? Or maybe I haven't worked properly enough at any point?

This fairly poor description leaves room for speculations, but maybe some of you like to give their two cents...
 
The coffee brown color to which you make reference was something I experienced when processing waste materials from certain manufacturing jewelers. What I discovered was that it is far more soluble in water than in HCl. When it was present (not always), the precipitated gold came down quite dark brown instead of the familiar light tan color we all hope to see. No amount of washing appeared to be successful in removing all of the unknown substance, so it was my routine to melt this material, then use it as the added gold for evaporation. Once so processed, the brown material was gone.

When this material is melted, even after considerable washing, there was always a reaction that was troubling to me. Small bits of gold would fly from the melting dish, as if they were meteors. In my simple mind, it appeared that the material would ignite, with considerable energy being released. I don't know that I'm right.

I was never able to make a determination what the substance was, not being a chemist. Don't even know if you and I are talking about the same material. Just thought I'd comment on my experience in the hopes it might be helpful.

Harold

edit:
I noticed your suggestion that it may be related to the platinum metals. I never found a connection, at least not by testing with stannous chloride or DMG.
 
Do you think this post from Etack about DMG in solution with alcohol mixed with AG in solution causes Booms, might apply to either of Solars or Harolds posts.
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=51&t=19307&view=unread#unread

I know neither of you mentioned silver in your solutions but maybe it snuck (sneaked) in somehow.
 
Thanks, Tom. There might be traces of silver from the impure gold button and I think I read traces of silver might be soluble in AR, but until now, none of my q-tipp tests did blow. I never used the DMG alc. for recovery, only tests. But good to know.
 
Not sure if i was on to anything or not. I just read the mentioned thread before reading this one and with Harold mentioning some of his melts seaming to "ignite" got me thinking.
I'd rather ask a (possibly foolish) question about a possible negative reaction, than read about a friend that was injured by something I "didn't" ask.

Did Sir Newton theorize about gravity after "watching" an apple fall, or did the apple fall, hitting him and causing him to ponder the theory :?: :lol:
 
Now,I finally have replaced that unholy alcoholic DMG 1% and used the advised DMG/NaOH and please look what I got!

The silver solution gave immediately a thick cloud of brown precipitate.

The HCl solution which I told about, I had used it in order to wash my goldpowder and it turned coffee brown. With DMG that one immediately produced a pale yellow voluminous precipitate.

Both settled.

Please make my day and tell me, I have platinum in my silver and palladium in my gold washing solution????? 8) :p

If so, is it possible to guess how much it may be? The gold washing is from 7g unrefined gold (source: all kind of e-scrap, gathered by AP, AC, AR, sulfuric cell and iodine processes) and has a volume of about 80ml. The silver solution (source: old plated flatware) had about 80g silver in 500ml solution.
 

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Bad mistake.... in future I will have the books beside me, when testing and Testing with stannous chloride is critical to success. (Harold) ....so, I still have to find my tin and make fresh stannous (my oldone tests still positive with standardAu, but not as fine as fresh one)...will be back!
 
HCl wash solution: stannous showed positive for at least gold, I can only guess I hadn't wash well enough, next I leave not nothing to chance

Added small portions of SMB at it dropped black-brown, solution ist almost colourless now with a yellowish tint. I will perform all tests tomorrow and start anew with the powder and treat it properly like an unknown precious metal alloy in order to exclude any mistakes and prejudices.
 
solar_plasma said:
...
I precipitated with potassium metabisulfite and got a light brown precitation at first, later more dark, almost black. So, obviously and like expected I had some impurities in it.

Then I decanted until the wash water stayed clear and decanted 2 times more.
MISSING STEP
Finally I let it sit for 2 weeks in 33% HCl, which got a coffee brown colour. This makes me wonder, since the first solution in AR was strongly yellow, as I would expect from a properly done gold solution.

...

MISSING STEP=

What I normally do:

1. Decant (from initial settled drop)
2. Add hot water from tap
3. Settle for about 15 min till water is clear and ambient temperature
4. Decant
5. Add hot water from tap
6. Boil for 5-15min (after this boling gold is heavy)
7. Settle to ambient temperature
8. Decant
9. Add cold water
10. Settle for 5-10min
11. Decant
12. Add cold water
13. Settle for 5-10min
14. Decant
15. Add HCl and boil for 5 min (you left it for 3 weeks...boiling in HCl dissolves traces of Cu, not sure if keeping it for long time at ambient temperature will do the same)
16... repeat steps from 1 to 14 with Distilled Water

You can reduce settling times - use filter and do not forget to process your filters once you have a bucket full. Last time I have recovered about 3gr of gold from used filters collected within 12 months.
 

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