Purple of Cassius- False Positive

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In the spoon, try diluting 1 drop with 3 or 4 drops of distilled water. Then add 1 drop of stannous chloride and see what you get. Sometimes you get better results by diluting highly concentrated samples. It takes very little gold to show up.

By the way, porcelain spot plates are cheap and better than spoons.
http://www.hometrainingtools.com/porcelain-spot-plate

Porcelain spot plates are also very handy for dissolving and testing very small quantities of metals (or ores, concentrates, etc). In the field, I used them to test for various PM brazes on stators on jet engines. I filed off some of the braze (file fairly deep) with a very small triangular file onto a clean sheet of paper. I transferred a few filings to a spot plate and added a drop of nitric and 4 drops of HCl. When dissolved, I tested (for gold/nickel braze) with a drop of stannous chloride. I used other solutions to pinpoint the Ag/Cu and Ag/Cu/Pd brazes. To speed the dissolving, you can put the spot plate on a warm hot plate or a sheet of steel that's been sitting in the summer sun. You can also heat a spot using a cigarette lighter or small torch underneath that spot. Ms. Hoke talks about the hotplate thing in her Testing book (free download). She also uses an abrasive to roughen the spots for rubbing PM objects, like on a touchstone. Reading this book will convince you of the value of spot plates.

They also work great for keeping the chunks of lead in proper order when doing fire assay cupellations - I numbered the spots 1 thru 12.

I assume these cheap spot plates (probably Chinese) will hold up to the heat and chemicals. I've always used the Coors brand but they are now $27 and up. There are dark blue ones, black ones and clear Pyrex ones that I haven't tried. I've always thought the black ones might be better for light colored things like silver chloride and DMG Pd. Coor's original black porcelain ones contained a uranium compound, I think.
 
Well, according to the document given by Grelko, both Selenium and Tellurium will come down with sulfur dioxide. So, most likely they will come down with stanus also, giving a messed up test.
Just a thought.
 
Platdigger said:
Well, according to the document given by Grelko, both Selenium and Tellurium will come down with sulfur dioxide. So, most likely they will come down with Stannous Chloride also, giving a messed up test.
Just a thought.
Your probably right, however Se and Te are soluble in HNO3, which will require another digest, possibly 24 hours of the Au precips to elute the Se & Te before you anneal the gold. Otherwise it may go up in smoke.
 
I haven't processed ore, but I have a knack for finding information. This might help you or other members find out what's causing your problem.

Documented Gold Bearing Telluride/Oxide Ores http://goldrefiningforum.com/phpBB3/viewtopic.php?f=44&t=8709&p=81710&hilit=gold+selenite#p81710

Gold-Selenide Separation http://goldrefiningforum.com/phpBB3/viewtopic.php?f=44&t=7308&p=206968&hilit=gold+selenide#p206968

http://www.ptable.com/ (Dynamic periodic table) click on Se or Te, theres alot of information about each of these.

Be careful, since Se and Te can be toxic, even the smoke/fumes.

Edit - I'd try what GoldSilverPro has suggested first. He would know alot more about recovery/refining, than I would.

Also (tin with selenium) http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=49&t=19477 might explain your stannous problem.

---------------------------
New Edit - Microscopic Determination of the Ore Minerals, Issue 914 https://books.google.com/books?id=bejQAAAAMAAJ&pg=PA206&lpg=PA206&dq=selenium+stannous+chloride+gold&source=bl&ots=Jkp_TLYsGX&sig=LdEBF95uNG_M3bm90xdNGrgHij4&hl=en&sa=X&ved=0ahUKEwiPx4XezqfKAhWDPj4KHe8hAnsQ6AEIMzAF#v=onepage&q=selenium%20stannous%20chloride%20gold&f=false

Bottom of page 206 - (stannous chloride precipitates tellurium as a black powder, which obscures to a large degree, the red selenium precipitate)

This is most likely the reason for your false reading for gold.
 
Tellurium and selenium are both thrown down (one as black, the other as a red powder) with sulfites or SO2 post aqua regia digest. Most often you can smell their presence (I can at least, selenium and tellurium both stink to me!).

This is why roasting, or ozone, is important to remove chalcogenides such as these.


Lou
 
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