1st attempt at nitric and AR

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Wizzlebiz

Active member
Joined
Jan 10, 2019
Messages
38
Good morning refiners. I am Wizzle. I finished hokes book. Read through some of the forums. And began my journey to refining my refining. 

I had to wait until yesterday do use nitric due to waiting for a chem mask and face shield. Nitric bath was good. I didnt get a boil over and wasted all the nitric. I did not filter hot. Which left me with picture 1.
20190119_095816.jpg
I also tested with some AR some material i had messed up during processing which was intersting. These were processed in AP. Pinnless cpu with mcll still attached. When using urea i got zero reaction. However it was cold. I warmed it and still got no reaction. Dropped with smb and got white powder at very little bottom with brown powder on top. I assume its lead and maybe a small amount of silver and the gold has settled on top of it.
20190119_095834.jpg

So I am going to heat all of this separately of course and refilter. 

Am I on the proper path here or is my understanding of mistakes off?
 
Wizzlebiz,
I want to make sure you know there is no chemical mask that will protect you from Nox fumes. I see in another post you mention covering a reaction with an inverted beaker in a pan of water to protect yourself from the fumes. Some of those fumes will be absorbed but that is not a good way to keep yourself safe. When you remove the beaker you are likely to see a big red cloud appear again.
It seems like you are experimenting with several processes at once. That is not really a good idea. You will end up with a lot of extra waste and effort. Depending on what kind of material/equipment you have to work with you should work with one at a time until you can get it to completion. What is your plan for the filter in picture 1? What was it when you started?
 
bigpagoda said:
Wizzlebiz,
I want to make sure you know there is no chemical mask that will protect you from Nox fumes. I see in another post you mention covering a reaction with an inverted beaker in a pan of water to protect yourself from the fumes. Some of those fumes will be absorbed but that is not a good way to keep yourself safe. When you remove the beaker you are likely to see a big red cloud appear again.
It seems like you are experimenting with several processes at once. That is not really a good idea. You will end up with a lot of extra waste and effort. Depending on what kind of material/equipment you have to work with you should work with one at a time until you can get it to completion. What is your plan for the filter in picture 1? What was it when you started?
I did each process separately. Giving each its own personal attention. I am also aware that the mask will not fully protect me. I used the inverted beaker to lower the fumes. I wouldnt assume I can get rid of the completely.

Filter 1 will be rinsed excessively with boiling water i think. I am assuming it is lead i am encountering.

I began reading about 6 months ago. Between Hokes book, the forum here, and refiners notes from a friend in NY.

I also worked out the AR in picture 2. Wasnt a problem at all.
 
I would decant solution and then dissolve residue in AR again.
After dissolving you must wait minimum 24 hours and then decant/filter solution. Add one or two drops of sulfuric acid can percipitates lead in form of lead sulfate
 
saadat68 said:
I would decant solution and then dissolve residue in AR again.
After dissolving you must wait minimum 24 hours and then decant/filter solution. Add one or two drops of sulfuric acid can percipitates lead in form of lead sulfate

Thank you. I felt like I was forgetting something. The sulfuric.... thank you.

I decanted the AR solution with boiling water 3xs, then boiling HCL then boiling water 2 more times. That cleaned it out.

Keep in mind this was a small sample test. I only used 50 grams of the non pinned cpu with mcll on them to see how hard it would be to seperate.

Next batch will be same but with mcll removed with a air hammer to not have the contamination. Will post next progress.
 
Im not sure I understand your decanting step. The boiling water 3X ? Did you mean rinses?
The white precipitate could be silver chloride ( my guess). And with that small of a batch of pinless CPUs, I don’t believe there would be enough gold to drop and notice.
There are a lot of good videos, articles and essays available to learn from. Tried and true methods and advice from very experienced and skilled experts right here on this board. No need to reinvent the wheel and needlessly make toxic waste.
 
Refining Rick said:
Im not sure I understand your decanting step. The boiling water 3X ? Did you mean rinses?
The white precipitate could be silver chloride ( my guess). And with that small of a batch of pinless CPUs, I don’t believe there would be enough gold to drop and notice.
There are a lot of good videos, articles and essays available to learn from. Tried and true methods and advice from very experienced and skilled experts right here on this board. No need to reinvent the wheel and needlessly make toxic waste.
Yes I meant I used boiling water to rinse then decant. My apologies for the confusion.

I wondered if it could be silver chloride due to the MCLL I left on.

Keep in mind this was a small test. I was aware I wasnt getting much out of it on the gold. It wasnt trying to reinvent the wheel. I was trying to get a grasp on on hand factors.

Thanks for your reply.
 
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