Mysterious brownred and white deposits

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Goldenrod757

Active member
Joined
Jun 30, 2012
Messages
26
Hi let me say a big hello to all the refiners out there. This is my first post.
I have been visiting the forum occasionally and picked up a few very useful tips. i was led here while doing other searches for info. This forum is obviously a huge resource that will take much time to utilise.
Im a new refiner working with jeweler's scrap so far. Polishings and sometimes floor sweepings. Im just completing only my third one. I found that floor sweepings appear too create some complications but iv recovered a fair amount of stuff each time.
Ive been using nitric bath to remove silver and copper, followed by water wash, second nitric bath and then AR. My second refining contained a sizable amt of gravel/dirt and it treated it with NaOH first followed by the aforementioned process. My 3 attempt i omitted the NaOH step.
From experimentation with my first batch i split the majority of the dissolved metals in two and neutralized half with urea and the other i boiled to almosts dryness which caused some of the gold to appear. Both were precipitated with SMB sol. The urea step was very indistinct and produced slightly less gold and came out somewhat dirty with a chocolate coating on one side of the stuff. Later i got the missing 4 grams that i expected with came out on the container i left the soloution in . The dried down portion produced a light brown powder with gold showing also. Iv concluded i prefer the boiling step. I the urea probably created some contamination as it was fertilizer grade.
The last two refinements both contained a reddish brown residue that spat and accumulated on the side of the beaker as the liquid got thick. I tried to separate it from the yellow stuff where possible. I have not tested it but think it may be palladium or rhodium chloride. It is soluble in HCL.I will attempt to post a pic of it. Can anyone say what that is? Where iv found white insoluble crystals (11grams collected and stored) i suspect silver chloride. But i see a white soluble powder in the third refining . If the dark brown/black stuff is not gold chloride decomposing, how should i separate this impurity.
Btw my first recovery was 5 grams of wonderful soft hi purity gold.
 

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Hello Goldenrod and welcome to the forum.

The third picture is a bit disconcerning, it makes me feel that you really have boiled your gold solution. You should never boil a gold solution. You should evaporate just below boiling so that you don't lose gold. When boiling you get a lot of bubbles bursting and a fine mist of gold solution that goes off into the air. If you get it too hot you could lose gold as gold chloride that sublimes into the air.

I don't know why your gold have different colours but I could make a guess. Depending on the purity of the solution, the concentration and what other impurities there are gold can drop with different sizes if the particles. The smaller the particles are the darker the powder looks and it will also take longer time to settle, as you noticed.

/Göran
 
Altho i boiled it down and it looked very dirty and the pics show, I added water and it turned a brownish milky and left it to settle. Poured off the water and boiled it in HCl. An orangeish to brown liquid which i will decant and continue to dissolve all other materials except the gold. Since is look as tho it could contain gold chloride i will retain it for further testing. There is stuff in the gold mud, whitish flakes. This is the first time this has happened but of course im still learningi. The other half of this batch was apparently dirtier and contained less polish. That was boiled down but not as much and didnt show any colour when boiled in HCL. The residue of gold looked like coffee grounds had surprising weight and was smelted with some difficulty - probably my torch isnt that strong and probably there are some impurities but it looks like hi karat gold. Is it possible to have some palladium or rhodium in there with a smelting with just and air/propane flame? I know their melting temps are higher but small amts may possibly alloy with gold at somewhat lower temps. Just speculating. Thanks for the thought that gold chloride may sublimate...didnt think of that...will check back the material data on it. And the fact that smaller gold particles look darker. Thanks
 
I might be wrong, but after the ar and boiling you might have had a lead sulfate come down. (The white flakes) I agree with what was stated above. It looks like you really boiled that sucker down.
 
Red jewelers rouge is iron oxide. Perhaps you carried over some iron salts?

No mater what it was your dark powder wasn't ready to melt. Refining a second time from the powder form as Harold recommends works for me.
 

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