Black Sand + HCl + Hypochlorite = White Snot

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Gratilla

Well-known member
Joined
May 25, 2009
Messages
187
Location
Indonesia
Some weeks ago I came across some black sand on my land. Under x100 magnification I could see a lot of black grains coated with, what appeared to be, gold. I magnetically separated this to about 70% magnetite and 30% tailings; the latter contained a lot of white grains (milky quartz?). I subjected 4 portions of the magnetite fraction to conc nitric acid, conc sulphuric acid and roasting with and w/o NaCl, with no apparent change - so not pyrites.

I then leached 1kg of the magnetite with HCl and Hypoclorite, adding the latter in small increments over 5 hours with stirring. I syphoned off and filtered 6 x 500ml beakers of golden orange liquid (chloroauric acid?). On diluting some I got a yellow liquid and putting some aside to evaporate I got yellow crystals (gold chloride?). I then split one beaker of liquid into 3 - 1 as control, to 1 I added 0.5M SMB and to 1 I added T-60, a proprietary precipitant (http://www.goldmineworld.com) and then raised the pH slowly with NaOH. At about pH 2.5 I got a large amount of brown precipitate from all 3. I filtered to get a reddish brown "mud" (gold hydroxide?). I boiled off a fraction of the original lixiviant to get a red-brown amorphous solid (gold oxide?). So far, (apparently) so good. Now is where everything starts to go "off the rails".

Gold oxide is supposed to be unstable to heating above 245C, so I heated to well above this temperature with no apparent change. Could I have platinum oxide?? To two 100ml portions of the original liquid I added saturated SMB and T-60, expecting to get a brown precipitate ie gold powder. What I got was some white cloudy precipite. I left overnight to settle and came back this morning to see a slight yellowish supernatent and cloudy white precipitate with the former and clear supernatent and a gelatinous precipitate (about 1/4 of the total) with the latter.

At this rate I'm going to be knee-deep in white snot without a single tiny flake of gold to show for my efforts. :cry:

What am I doing wrong?
 
Try testing the acid with stannous chloride. If you don't have an assay you don't even know if it contains gold. Stannous will tell you if there is gold in the acid. The brown you are getting at a pH of 2.5 is most likely iron.
 
4metals said:
Try testing the acid with stannous chloride. Stannous will tell you if there is gold in the acid.
I (kinda) tried. I'm in rather a remote location as far as chemicals are concerned - a day trip from "civilization". The best I could find locally was 60/40 tin/lead solder. I put a few cms into conc HCl and let it stand for a few days. When the solder started disintegrating, I also got some small white crystals. Anyway, I tried a spot of this liquid on a spot of my yellow solution and... nothing! No apparent change. Not conclusive as I don't know what I got from the solder alloy.


4metals said:
If you don't have an assay you don't even know if it contains gold.
Unfortunately, I don't have access to an assay. Any other way, apart from assay and SnCl2 that would confirm (or otherwise) that I've got gold?


4metals said:
The brown you are getting at a pH of 2.5 is most likely iron.
A logical observation, seeing as I'm aggressively leaching Fe3O4. But...
1) Iron what? We're talking a LOT of precipitate here - almost half my original solution drops as a precipitate. And,
2) Where is the iron in my yellow crystals? If it's a significant contaminant, it'd interfere with the crystallization, right? And if the yellow crystals are iron something, iron what?
 
Poor Mans SC

If your really stuck you can get an old Pewter cup from charity stores which usually contain 97% Tin (Like an old birthday mug someone has given to charity) break off a chunk and file it to a reasonably fine grain and add this to some HCL, heat the solution with a hair dryer if the HCL is diluted to speed up the process.
 

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