After some nitric acid baths i have a dense brown precipitate, what is this? (Images attached)

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Ellias

Well-known member
Joined
Jul 6, 2024
Messages
54
Location
VA
Hello everyone!

I am processing around 500 grams of PROMs for fun. The process i took was the following:

1. Incinerated until white

2. Grind with mortar and pestle

3. Strain the powder

4. Grind strained substances

5. Incinerated again

6. HCl bath for 2 days

7. Cleaned and washed around 15 times with boiling water and hot water

8. 2nd round of HCl bath under heat for 4 hours (light boil)

9. Washed 15-20 times and made REALLY SURE to clear any residual ash and HCl (HOT water/Boiling water and some very deep spatula stirring)

10. Put in a nitric acid bath and now i am here. And my head is a bit puzzled.

[THIS IS WHERE I STOPPED]

I started the nitric with 50/50 nitric water but had to add a bit more water as the reaction almost got too reactive, too fast

Left reaction on heat for 4 hours. However right now my powder at the bottom slowly turned into a dark brown color (near the beginning prior to Nitric, I saw my line of gold and some black powder on top at first)

My question is - what the heck is this?

And should i give it a shot of nitric acid to clear it up and return it to a more blue color?

I am wondering if this is due to remaining iron in my solution and adding more water turned it to rust or if it was something else. Please let me know what this dark brown substance is (if not rust).

I am going to wait a whole night before decanting and trying to recover silver but please let me in on some insights/solutions or what ive done wrong.
 

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