Some new troubles

[adam_mizer]

Wow I'm seeming to have many troubles lately.

Lets start with that I have been cleaning out cemented (with copper) PM values I thought from old stock pots.
The stock pots (gallon plastic bottles) before started were cleaned out of any solids.
From about 10 jugs I pulled (filtered) the bottom cement values (solids).
Then washed (rinsed) in water several times to remove color.
Processed in Nitric for silver, nitric had no silver or PM's but has pulled out any copper in its solution.
Then washed (rinsed) in water to remove color. Disgarded solution into jug.
Processed remaining solids in AR. Stannous showed positive, purple type color, started dissappearing after a while. I though maybe palladium and gold.
Evaporated to remove free nitric.
Tested with stannous still shows PM (light purple color).
Add SMB and got a drop.
Let settle over night.
Rinse with heated and cold water several times.
Appeared a couple layers of powder with slight different colors, blue/gray mostly and maybe what appeared like traces of gold maybe.
Put in HCl, took all into solution no problem after a little stirring.

Solution now a yellow tinge color with light green, very clear. No solids.
Diluted with water a few times over to raise PH as I wanted to drop any gold with oxalic acid.
Slightly heated and oxalic acid was added, quite a bit of oxalic was added and there was absolutely no precipitant.

Added SMB and all dropped out of solution and residual solution was very clear like water.
Removed solution tested with stannous and had no values.
Solids were a Blue/Gray color.
Still not happy with this, as it appears as mixed PM's still unknown to me.

This has gone on for a while, last final try.
Process in Nitric should get any palladium right, or am I wrong?
Took the solids and added some powders (only a gram of palladium/gold drops from previous smb drops(why not)).
Solution looks good and is very dark red.

Here's a picture of the remaining solids.
Maybe the picture does not show properly but its more of a off white color.
Now these solids (salts) don't remind me of gold but makes me wonder if after all this processing if I ended up with some other chloride of Gold like I/III?
After all this, should I melt this chloride or will it go up in smoke?
Okay thats enough of the off/white solids.

Here's a second picture of the precipitant from ammonium chloride.
Funny just from ammonium chloride I got this precipitation and check the stannous swab, its a light purple and dry from a day later.
EDIT ADD: the swab appears like palladium when freshly tested, from light purple to black some green, also right when stannous hits the swab its red then goes dark.
This is not good. (Metal salts mix). What to do?

So now I'm really messed up and not happy at all from all the work I did do.
Think I'm going crazy!
Hope you can easily understand the processes I did.

John

 

[adam_mizer]

Forgot to add removal of some early solids while processing.
Here's a pic of those.
Also don't know what to do other than try to torch them?

Edit: add a picture of the palladium pregnant dropped salt (used sodium chlorate), this was from 2 batches. The one in question above and other materials.
Thought you might like to see.
Still at question is that some other PMG or what dropped out with the ammonium chloride.?

 

[Palladium]

Wow I'm seeming to have many troubles lately.

Lets start with that I have been cleaning out cemented (with copper) PM values I thought from old stock pots.
The stock pots (gallon plastic bottles) before started were cleaned out of any solids.

1. From about 10 jugs I pulled (filtered) the bottom cement values (solids).
2. Then washed (rinsed) in water several times to remove color.
3. Incineration
4. Processed in Nitric for silver, nitric had no silver or PM's but has pulled out any copper in its solution.

John

 

[adam_mizer]

Thats the step I missed!!!
How could I have completely forgot?