Ceramic Processor Refining trouble, Any Advice?

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CONCEPTUALGENIUS

New member
Joined
Jun 10, 2014
Messages
3
Hello everyone,

I am new to the forum and I have read all the rules and Guidelines of the forum. I have read Hokes book twice and many others on the subject of refining PM waste. I have successfully processed over 100 pounds of ceramic processors in the last 5 years and managed to get results after every batch. The last batch I processed was a bit confusing to say the least and I could use any help or advice anyone would like to offer.
I ran into a few complications along the way but always found solutions in past forum posts and around the net.
I Recently refined 7.75 pounds of mixed Ceramic Processor scraps.
The problem is that I had almost 2 pounds of undigested grey powder on the bottom of the beaker after heating the aqua regia for a few hours. I usually don't mix my processors but I did this time due to time and material issues. Most were very old late 70's early 80's Nec,IBM, Motorola Some had no identifying numbers or names. Some had lids which were removed and some glass cover lids also removed. The processors were broken into small pieces not chunks and dissolved in 3000 ml of HCL and sodium nitrate added in increments. after the reaction stopped and most gold was dissolved there was a thick layer of grey powder at the bottom of my beaker. I filtered the solution and removed the powder then chilled the solution with ice as I have numerous times added a little sulfuric to precipitate the lead and waited 24 hrs before decanting the solution. Silver & lead dropped out and my solution was a very transparent and clean. Filtered again and finally precipitated the gold with SMB in small increments waiting and testing with stannous to insure all gold precipitated. I cleaned the powder as always 3 boiling tap water washes then a hot HCL wash Then 2 distilled water washes then aqua ammonia wash then 1 more distilled water wash. Gold was nice golden brown.
Managed to drop 14 grams of 99.95% gold, Not what I was expecting from 7.75 pounds of ceramics that old. I figured at least an oz from what I have yielded in the past with other batches.

Now I have almost 2 pounds of grey powder that I heated almost red hot on a propane burner for 2 hours and I can not tell what the powder is. I put 3 grams of this powder in HCL and boiled it, Test light positive for gold with stannous, light purple color. I then added a little sodium nitrate and heated the solution. Powder did not dissolve much. This time tested with stannous and it was a strong positive for Gold Dark Black purple. Dropped .4 grams of gold from this solution. Dried the grey powder and now I have to ask could I have trapped my gold in this grey powder somehow? I tried boiling it in hot water nothing dissolved so not lead, strong 67% and dilute nitric No reaction, Tried dilute sulfuric acid no reaction, Then I tried aqua regia again and it released a little more gold. Could my gold be trapped by another metal? What did I wind up with ? Any advice would be great, I searched the forum for grey powder that will not dissolve and came up a little short for answers.
Attached is a few pictures of the grey powder in the beaker and after dried.
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I fear you have tin there. Take some of the powder and dry it then heat it to red heat and allow to cool and then add hydrochloric acid to dissolve the tin. The other possibility is silver chloride again that's easy to determine if the powder starts to darken when exposed to light then it's a strong possibility if not then tin is your best bet.
 
Thank you for your response Nick,

I have already heated this powder to as hot as I could get it in a pan over a propane burner and after I boiled it hcl and it tested positive for gold again. Not much of the powder dissolved in hot hcl and after it was dried it was set out in direct Florida sunlight and it did not darken. I will post pictures of the powder after it was dried and boiled again in hcl and the stannous swab test from the hcl that it was boiled in.

It's got meet wondering for sure.

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The powder needs to be heated until it is glowing red and stirred to allow oxidisation and then if it is tin it will dissolve in hot hydrochloric acid. Incineration also removes all the acid so no values can go into solution.
 

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