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

[Ellias]

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.

 

[Ellias]

@Shark @Yggdrasil hoping to pike you guys about this one.

 

[BGDOCK]

Do you mind if I ask
Did you use a magnet to seperate any ferrous material ?
Could be some iron hydroxide
Draw a couple of samples off , of that brown compound and add some distilled water ,apply gentle heat see what happens first then add some nitric see what happens to that brown compound ,
Might have to drain the green solution off to attack the brown material
You got this, have patience

 

[Shark]

Stannous test the solution. Always stannous test.

There is a lot of copper in the solution for all the HCl soaking. Did you magnetically remove any material before hand, especially before using nitric? Iron in nitric will often produce iron oxide (I think the oxide is right) basically plain old rust in a very fine state. Filtering can be a nightmare. If this is the case, I would ...
Stannous test. If positive, either drop it or decant and drop separately. Then follow the procedure outlined next...

If negative.

Decant the solution off, and go to AR. Filter, as often as needed to get the solution clear of debris. Drop it, and then move to cleaning the gold.

My first time doing IC's went really well. The second time was nearly a disaster. I spent days trying to find all the missing gold and about week later I finally got most of it back. It sure made me glad I had a stockpot in use.

Looking forward to others opions on how they would proceed.

 

[Yggdrasil]

@Shark @Yggdrasil hoping to pike you guys about this one.

As Bgdock asks, did you separate out the magnetic parts?
If not, the brown will most certainly be Iron in various states.

 

[Ellias]

Stannous test the solution. Always stannous test.

There is a lot of copper in the solution for all the HCl soaking. Did you magnetically remove any material before hand, especially before using nitric? Iron in nitric will often produce iron oxide (I think the oxide is right) basically plain old rust in a very fine state. Filtering can be a nightmare. If this is the case, I would ...
Stannous test. If positive, either drop it or decant and drop separately. Then follow the procedure outlined next...

If negative.

Decant the solution off, and go to AR. Filter, as often as needed to get the solution clear of debris. Drop it, and then move to cleaning the gold.

My first time doing IC's went really well. The second time was nearly a disaster. I spent days trying to find all the missing gold and about week later I finally got most of it back. It sure made me glad I had a stockpot in use.

Looking forward to others opions on how they would proceed.

This worked out! I did not separate the metallic parts. Thank you so much

 

[Ellias]

This worked out! I did not separate the metallic parts. Thank you so much

@Shark @Yggdrasil @BGDOCK
I recovered Gold! At first it wasnt dropping so i added a bit of HCl and doubled the water and a tiny bit of SMB to drop.

Thank you so much guys. Waiting the rest of the night to see if anything else settles.

I started with like a little less than 1 Pound of non ceramic EPROMs. Is this really the type of yield for those?

Thank you so much for the continued support and knowledge.

 

[BGDOCK]

What does the filtrate look like ?

 

[Ellias]

Hmm it looks dark grayish.... this was crystal clear prior to SMB. Drat...another failed SMB drop.

Stanneous test shows negative now. PH was at 1.

I just dont understand this gold drop. I had 1 PERFECT gold drop in my qhole time doing this. I processed 493 grams of non ceramic e PROMs (expecting low yield but this is nuts.)

 

[Ellias]

Hmm it looks dark grayish.... this was crystal clear prior to SMB. Drat...another failed SMB drop.

Stanneous test shows negative now. PH was at 1.

I just dont understand this gold drop. I had 1 PERFECT gold drop in my qhole time doing this. I processed 493 grams of non ceramic e PROMs (expecting low yield but this is nuts.)

This was like 5 in a row failed drops. I added only 1 gram of SMB muxed with water.

 

[BGDOCK]

Sounds like the values are redissolving .
try to Cement out using a copper pipe use a bubbler or a spray bottle to remove PMG off the copper into a beaker
Reprocess/ Dissolve
Edited for clarity

 

[Ellias]

Sounds like the values are redissolving .
try to Cement out using a copper pipe use a bubbler or a spray bottle to remove PMG off the copper into a beaker
Reprocess/ Dissolve
Edited for clarity

Ill wait 1 night with the copper bar as it has only been 3 hours but, What is this grey powder? Silver? But how is that possible after the many nitric baths? I dont believe it to be lead due to my sulfamic acid treatment. Is it possible that my poor mans aqua regia was made incorrectly?

Below is picture of filterant.

Additionally i made poor mans Aqua regia by

1. Mix 80 ml of distilled water with Sodium Nitrate (28g)

2. Warm

3. Add in hcl (125 ml 30%)

4. Boil for 20 minutes (added picture of end result)

I feel like it has to be working because there was a very obvious line of gold in my beaker. But after AR it is gone.

 

[Shark]

Got a picture of the grey material?

 

[Ellias]

Got a picture of the grey material?

Attached seems like the light grey is forming on the copper bar too... (very light dusting) but i tried recovering during nitric bath step and no white came out after adding HCl. @Shark

 

[Shark]

Maybe tin?

 

[Ellias]

Maybe tin?

Is that possible with 2 days in HCl bath and another treatment of HCl boiling 4 hours?

 

[BGDOCK]

Ellias I need to catch up here let’s slow down a bit please

Ill wait 1 night with the copper bar as it has only been 3 hours but, What is this grey powder? Silver? But how is that possible after the many nitric baths?

+++Please cement out for 2-3 days even longer would be better .anything under copper on the periodical table will cement out .


I dont believe it to be lead due to my sulfamic acid treatment. Is it possible that my poor mans aqua regia was made incorrectly?

+++ Did you filter the poor man’s nitric
NaNO3 + HCl ---> NaCl + HNO3.
Makes Nitric and Salt

Below is picture of filterant.

++++ I was asking about the filtrate in The picture with the brown material and black flecks. the reason was you had asked about your gold yield I wanted to see how those Ic chips looked . They appear black so you may have to reincernate , crush and reprocess .

Additionally i made poor mans Aqua regia by

1. Mix 80 ml of distilled water with Sodium Nitrate (28g)

2. Warm

3. Add in hcl (125 ml 30%)

4. Boil for 20 minutes (added picture of end result)

I feel like it has to be working because there was a very obvious line of gold in my beaker. But after AR it is gone.

+++What did the stannous test show ?
++++And what’s the pH ?

Attached seems like the light grey is forming on the copper bar too... (very light dusting) but i tried recovering during nitric bath step and no white came out after adding HCl.

+++ Are you cementing out your values then using a nitric bath then adding HCl ?

Attachments​

• 
  Is this you poormans AR

Edited for clarity

 

[Ellias]

Ellias I need to catch up here let’s slow down a bit please

Ill wait 1 night with the copper bar as it has only been 3 hours but, What is this grey powder? Silver? But how is that possible after the many nitric baths?

+++Please cement out for 2-3 days even longer would be better .anything under copper on the periodical table will cement out .


I dont believe it to be lead due to my sulfamic acid treatment. Is it possible that my poor mans aqua regia was made incorrectly?

+++ Did you filter the poor man’s nitric
NaNO3 + HCl ---> NaCl + HNO3.
Makes Nitric and Salt

Below is picture of filterant.

++++ I was asking about the filtrate in The picture with the brown material and black flecks. the reason was you had asked about your gold yield I wanted to see how those Ic chips looked . They appear black so you may have to reincernate , crush and reprocess .

Additionally i made poor mans Aqua regia by

1. Mix 80 ml of distilled water with Sodium Nitrate (28g)

2. Warm

3. Add in hcl (125 ml 30%)

4. Boil for 20 minutes (added picture of end result)

I feel like it has to be working because there was a very obvious line of gold in my beaker. But after AR it is gone.

+++What did the stannous test show ?
++++And what’s the pH ?

Attached seems like the light grey is forming on the copper bar too... (very light dusting) but i tried recovering during nitric bath step and no white came out after adding HCl.

+++ Are you cementing out your values then using a nitric bath then adding HCl ?

Attachments​

• 
  Is this you poormans AR

Edited for clarity

Apologies

- The orange/yellow color flask attachment is my poor mans aqua regia (on top of hot plate with sun shining on it)

- stannous showed a positive reaction prior to SMB drop. Also a line of hold could be seen.

- the filterant is shown in attachment (should look like pitch black coal ish)

- PH value prior to SMB drop was showing value of 1.

-I am cementing the failed drop and reprocessing

Final - I just realized i had too much free HCl and SO2. So i literally heated it on hot plate and now i have my brown yield!

Whew no worries everyone looks like i do know what im doing haha! After heating - the grey precipitant disappeared and turned brown.

@BGDOCK

 

[BGDOCK]

If that picture is you ic chips I would incinerate them again grind and reprocess

 

[Shark]

If that picture is you ic chips I would incinerate them again grind and reprocess

Agreed. It looks like a lot of leftover plastics.