I have a very dirty AR solution

[MISHUNCONTROL5]

I used AR method to refine military gold pins 1.1 lbs
Covered pins in HCL, let it set for 20 minutes
Repeated this twice to get rid of base metals.
Washed the pins in filtered water 3 times

Covered pins in HCL, Added Nitric slowly and watched the reaction closely.
As soon as the reaction subsided I carefully added more
Nitric ...VERY SPARINGLY.
I let it settle and cool for several hrs.

Solution was a very dark color at this point. Almost black...never had this happen before.
I suspected a lot of copper was in the solution.
I used a piece of Stainless steel metal to cement the copper out of the solution.
There was an immediate reaction stainless steel bar was full of copper instantly.
The solution was still very dark green almost black still.....
I did this until no more copper was collecting on the stainless steel bar.
Solution lightened up a bit but not much still very dark green .
Did Stanous test, gold was heavily present.... very dark brown , gold test looked great.
I NEVER HAD A COPPER PROBLEM EVER BEFORE.

So I filtered it again. At this point I saw black thick dust covered in the filter. Silver and Copper chlorides formed and were caught in the filtering process. Some crystals formed again but not a lot . I suspect this was some of the base metals from the stainless steal bar. I kept this mud aside ... Solution was pretty much clean of Chlorides and black mud , Strained the solution to clean it up a bit 3 times, But still very dark green, almost black.... puzzled my mind.

Added a touch of Sulfuric to drop any lead.no lead ...
Filtered the black mud again 3 times.

I doubled the volume with water

Added stump out.

No gold dropped.
Solution turned brown then a red burnt brown color.... NO GOLD DROP.....

SIDE NOTE: Smelted the black mud, it was extremely hard to melt. Turned out to be a silvery grey metal brittle as hell. I Suspect Nickel and PT, IR.

Back to the BOTCHED AR:

Tried heating the botched AR to drive off S02
Added more HCL , 2 times volume.
Added a touch of distilled water...
Tried the stump out drop again.... same reaction as before.
Did stanous test gold is heavily present.
STILL NO DROP!

WHAT IN THE HECK IS GOING ON ?

I've done this 100 times and always drop the gold.

I searched the site and found no answers.

CAN SOMEONE HELP!?

 

[FrugalRefiner]

I see multiple mistakes in your process.

I used AR method to refine military gold pins 1.1 lbs
Covered pins in HCL, let it set for 20 minutes
Repeated this twice to get rid of base metals.
Washed the pins in filtered water 3 times

20 minutes in HCl isn't going to get rid of much of the base metals, even if you do it three times.

Covered pins in HCL, Added Nitric slowly and watched the reaction closely.
As soon as the reaction subsided I carefully added more
Nitric ...VERY SPARINGLY.
I let it settle and cool for several hrs.

Solution was a very dark color at this point. Almost black...never had this happen before.
I suspected a lot of copper was in the solution.

That's because you didn't eliminate much in your HCl baths.

I used a piece of Stainless steel metal to cement the copper out of the solution.
There was an immediate reaction stainless steel bar was full of copper instantly.
The solution was still very dark green almost black still.....
I did this until no more copper was collecting on the stainless steel bar.

If you were trying to recover the gold from a dirty solution, you should have used copper.

Solution lightened up a bit but not much still very dark green .
Did Stanous test, gold was heavily present.... very dark brown , gold test looked great.
I NEVER HAD A COPPER PROBLEM EVER BEFORE.

That sounds more like a false positive.

So I filtered it again. At this point I saw black thick dust covered in the filter. Silver and Copper chlorides formed and were caught in the filtering process. Some crystals formed again but not a lot . I suspect this was some of the base metals from the stainless steal bar. I kept this mud aside ... Solution was pretty much clean of Chlorides and black mud , Strained the solution to clean it up a bit 3 times, But still very dark green, almost black.... puzzled my mind.

Your gold is probably in that black dust.

Added a touch of Sulfuric to drop any lead.no lead ...
Filtered the black mud again 3 times.

I doubled the volume with water

Added stump out.

No gold dropped.
Solution turned brown then a red burnt brown color.... NO GOLD DROP.....

I'm guessing you didn't have any gold in solution.

SIDE NOTE: Smelted the black mud, it was extremely hard to melt. Turned out to be a silvery grey metal brittle as hell. I Suspect Nickel and PT, IR.

Why do you think you had platinum and iridium?

Back to the BOTCHED AR:

Tried heating the botched AR to drive off S02
Added more HCL , 2 times volume.
Added a touch of distilled water...
Tried the stump out drop again.... same reaction as before.
Did stanous test gold is heavily present.
STILL NO DROP!

WHAT IN THE HECK IS GOING ON ?

I've done this 100 times and always drop the gold.

I searched the site and found no answers.

CAN SOMEONE HELP!?

Gold in solution should give you a purple to dark purple to nearly black result with stannous. Perhaps if you show us a picture of your stannous tests we can help.

Dave