• Refining Palladium concentrates.

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9kuuby9,

I just now found this/your thread, and as one who is preparing to have a go at Pd very soon but has
never done it before, I can say that this photo tutorial is immensely valuable, providing a right-brain
guide to what things should look like if everything is being done correctly.

Very well done!

Cheers,

Mike
 
9kuuby9 said:
Some pictures on Refining Palladium concentrates.

I used the outlined process provided by our fellow member of the forum "4metals"
(additional steps that are marked with "***" and start with "▪" are not from the original steps but are additional steps that may improve this process)

http://goldrefiningforum.com/~goldrefi/phpBB3/viewtopic.php?f=51&t=6638&start=20#p72403

let's start with the first three steps;

▪ Calculate and add, stoichiometrically half of the needed amount to dissolve Palladium and add the remaining half in increments, cease addition when no more reaction occurs. It's not easy to Dennoxx a nitrate solution without HCl.***

• Digest the impure palladium metal in 50% nitric / distilled water.

▪ Evaporate solution down to 10ml-15ml of solution per gram of Palladium.***

• Raise the pH to anywhere between 1 and 2 with NH4OH

▪ Evaporate solution down to 10ml-15ml of solution per gram of Palladium.***

• Filter the solution to remove any turbidity or sediment, which may be AgCl.

View attachment 22992

View attachment 22993
Click to expand...
 
Per-Ove,
Sounds swedish to me !
Yes, I have a lot to say about this but dont really know where to begin...
Im trying to get PD out of PLCCs and can certainly need some guidance.
Ive been looking at some videos on Youtube and Im quite sure they do it right to begin with...but the end product is not correct...
- I have to study this text more thoroughly and then ask some questions which someone hopefully can assist me with :)
 
Not quite Swedish no, close but no Cigar ;).
I was referring to you quoting a post without adding anything to it.

And I guess you mean MLCC, but then you need high grade or old.
Most newer contain nothing but Nickel.

Wet chemistry wise, they disintegrate by HCl with time.
Nitric will take Ag and Pd.
And smelting with copper silver or lead as collector well do the bit.
So first you need to find out what you have.
Nickel is magnetic, silver and Pd not.
 
Yggdrasil said:
Not quite Swedish no, close but no Cigar ;).
I was referring to you quoting a post without adding anything to it.

And I guess you mean MLCC, but then you need high grade or old.
Most newer contain nothing but Nickel.

Wet chemistry wise, they disintegrate by HCl with time.
Nitric will take Ag and Pd.
And smelting with copper silver or lead as collector well do the bit.
So first you need to find out what you have.
Nickel is magnetic, silver and Pd not.
Click to expand...
 
You did it again...
What do you accomplish with a quote, with no comment, question or anything else??
That is just saying with nothing to say.
Please get your things straight.
Goeran are you on this?

Sorry English keyboard
 
Yes, MLCC's sorry.
Yes, I got quite a lot...all 2005 or older...
Started out in 2L pet bottles with about 15% HCL to get rid of the tin (and perhaps outside nickel). Believe I was pretty succesful as I ended up (after about a week) with a purple transparent liquor with grey mass in the bottom (tin ?).
Out with the MLCC's and let them just dry up for a while. Bought two mixers with extra blades and grinded the MLCC's to dust (almost). Then into new pet bottles and added concentrated nitric acid. Red smoke and red fluid. The mass changed color into greenish/grey.
Let it stand for about a week (shaking every day). Out of the bottles and filtered. I have saved the grey green mass in the filters. Dont want to throw away.
The components (whats left of them) into a plastic tray for keeping.
The filtered fluid a bit black/green.
Added concentrated HCL and the fluid changed color to dark red and in the bottom a separated beige/red mass appeared (silver ?).
I believe this is correct so far...
I have taken some other measures from here but it doesnt seem right.
For ex. adding sodium to the dark red fluid...
Im a bit stuck...
 
Lou said:
Bit of a grotesque simplification on Rh, Ir, Ru, and Os.
Click to expand...
I merely fixed the link for him. Now I feel like I should have read it again before I did :) . I think I will read it agsin now considering how old it is.

Steve
 
4metals said:
That post was 13 years ago! Oh how the prices have changed. The first 4 metals in the post were by far the most sought after in refining. The last 4 not as popular.
That’s why I picked 4metals as a forum handle and not 8metals!
Click to expand...
Fantastic to see that you are still around here at the forum.
I'm particular interested in palladium refinement, since I got a nice source for it (Pd/C, PdCl2, Pd(OAc)2, etc). My intent is to reduce all to Pd metal.
 
The carbon, burn. It gives PdO plus silicates from the ash. Reduce that with formic acid, then digest in aqua regia.
Filter out the residues, rinsing til colorless and add them to the PdCl2, Pd acetate, etc. and reduce with ammonium formate at pH of 3.5. You will have pure Pd metal
 
9kuuby9 said:
• A redução está completa quando o Pd cai para o fundo, a solução se torna incolor e o pH estará entre 7 – 8. algum Pd recuperável permanece nos líquidos, então guarde os líquidos como antes para a cimentação.

View attachment 23090

-Observe o borbulhamento; provavelmente uma reação catalítica.

View attachment 23091

View attachment 23092

View attachment 23093
Click to expand...
hllow 9kuuby9, hope i`ts great, this process can be used to recover capactors pownder, where there are impurities such as cooper, silver, etc dissolved in nitric ? and congratiulation for ecxellent work.
 

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