Refining MLCC´s for Palladium and Silver !

[Lars100]

All,
I managed to get together quite a pile of MLCC's which are of 2005 or older... Im far from a chemist but have been working with electronics for many years. Got on the track with Palladium when I learned about all the cathalyst´s being stolen from cars and realized that I had these MLCC´s.
So my goal is to extract as much Palladium and Silver as I can.
Started watching videos on YouTube how to do this refining and brought together necessary acids (so far...). Placed the MLCC´s in 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. Put the purple liquid aside.
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...yet).
The components (whats left of them) into a plastic tray for keeping.
The filtered fluid is black/green and fairly transparent.
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 and formic acid to the dark red fluid...and heat to about 80C. If I filter that potion and heat again it will only become a black mass.
If I pore Nitric Acid in that black mass then it melts into a orange/brown tranparent fluid (which in a way must be right but only takes me backwards...) !
Im a bit stuck...

 

[orvi]

Red-orange-brown colour is relatively what you are looking for. If you are in doubt, cement it out redissolve everything and cement on copper. Anything of value will come out of solution, but you need air bubbler or magnetic stirrer/mechanical stirrer. Liquid must be agitated while precipitating PGMs on copper.

 

[Yggdrasil]

I believe you have your chemistry wrong. Silver will transform into SilverChloride when it finds any chlorine ion. It do not dissolve in acids. It is a white fluffy substance that take time to settle. The substance you have is probably a mix of ceramics and metastannic acid. It is a nightmare to filter so most of us hate it. Dissolved Pd salts with chlorine will usually be brownish red, not bright red.
Did you do a stannous test?

 

[Yggdrasil]

Red-orange-brown colour is relatively what you are looking for. If you are in doubt, cement it out redissolve everything and cement on copper. Anything of value will come out of solution, but you need air bubbler or magnetic stirrer/mechanical stirrer. Liquid must be agitated while precipitating PGMs on copper.

You beat me to it again
I will need to move faster

 

[Lars100]

Im not sure I know what You talk about... Cement it out ? How do I do that ? Cement on copper ? Do I just put a copper plate in the red-brown liquid and wait for the palladium to stick ?
- I will take some pictures and show You what I got so far.
Please have patience with me. I basically have no clue and no earlier experience...

 

[Yggdrasil]

Im not sure I know what You talk about... Cement it out ? How do I do that ? Cement on copper ? Do I just put a copper plate in the red-brown liquid and wait for the palladium to stick ?
- I will take some pictures and show You what I got so far.
Please have patience with me. I basically have no clue and no earlier experience...

Another reason to take it easy.
The salts from PGMs are very toxic and can lead to severe health problems and death.
Cementing means putting in a more reactive metals so they swap place. But with PGMs it is crucial that the liquid moves quite fast to dislodge the cemented metal so it do not pasify the copper. An air bubbler will fix that.

 

[Lars100]

Thanks ! Ime trying to protect with ventilation, fans, rubber gloves and protective glasses. I don touch anything with bare hands.
Ok, please see the attached pics.
I look forward to hear Your comments /questions !

 

[Yggdrasil]

Silver chloride is bright white and fluffy. So the last picture may or may not be silver chloride, do not let it dry.
But you have to wash it clean first, until there is no color in the liquid. The liquid may contain some of your values.

Which lead to:
Did you ever test it with stannous?
Without a test it may be all trash, and you are wasting your acid.

 

[Lars100]

Thanks for input !
Ehh...Stannous-test...how do I perform such a test ?
Air-bubbler ? Any brand, type You can recommend ?

 

[Lars100]

And furthermore...clean the liquid ? How do I do that (and with what) without wasting all the goodies ?

 

[manorman]

Bare hands a handling toxic substances not a good idea. You need to slow down and read before you kill yourself or someone else.

 

[orvi]

MAN, PGM solutions and NO GLOVES ??? Seriously ?

 

[Lars100]

No no...See above...RUBBER GLOVES !!!

 

[galenrog]

What we have here is a dead man. His body just does not know it yet. Despite protestations otherwise, all images provided showing hands demonstrate no safety considerations of any kind.

An enclosed room with ventilation is NOT a safe environment to perform what you are doing. Handling contaminated glassware without proper protection can easily allow toxic metal salts to enter the body, causing vital organs such as kidneys, liver, and lungs to fail in a few months to a few years. Yes, just one exposure can do this.

Get you mind right. Put your toys away. Read the entire section on Safety. EVERY THREAD. At least three times. Come back when you have an understanding of the potential hazards of what you are working with.

Time for more coffee.

 

[Lars100]

Im glad I gave You something to talk about !
I am certainly aware of the danger with these products and keep myself protected (as much as I can).
The pictures from today (with bare hands) were just something I took with speed as I wanted to have something to show here.
We can of course continue to discuss safety or we can move forward and let me know what I need to do in order to purify the metals I got !
- P.S. Im not saying that I will live forever but I started out with this project in Nov-21 and it´s now April-22.
Im still feeling well despite the fact that I´ve had Covid twice.

 

[Yggdrasil]

Lars,
We recommend or more command, one thing from people coming here.
That is self study, read on the forum,
there is a handy search function, the information can be a bit overwhelming in the beginning.

And it is a must to read C.M. Hokes book. She takes you through most of what you need to know.
It is old so safety was not as today so I believe some chapters has been modified for that.

Some of the members has the link to the book in their posts.

It goes to the concept, give a man a fish and he eats today or learn him to fish and he is fed the rest of his life.

So please read, search and study. When you need help, ask questions about the issue at hand and you will be helped.

 

[Yggdrasil]

Im glad I gave You something to talk about !
I am certainly aware of the danger with these products and keep myself protected (as much as I can).
The pictures from today (with bare hands) were just something I took with speed as I wanted to have something to show here.
We can of course continue to discuss safety or we can move forward and let me know what I need to do in order to purify the metals I got !
- P.S. Im not saying that I will live forever but I started out with this project in Nov-21 and it´s now April-22.
Im still feeling well despite the fact that I´ve had Covid twice.

That is why we ask you to do a stannous test, it will show if you have values in there.
And the way you ask what it is, clearly tell that you have not studied enough.

Stannous refers to StannousChloride which is Tin dissolved in HCl.

When that meets Gold, Pt or Pd in solution, it forms colloids with distinct colors.
Purple for Au, Orange for Pt and greenish blueish color mix for Pd.

Search and you will find pictures of it.
Take your solution and drop one drop on some paper and then one drop of stannous on the same spot after.

If there are values you will see it immediately.

If not, the solution can be poured into the stock pot.

 

[Yggdrasil]

Thanks for input !
Ehh...Stannous-test...how do I perform such a test ?
Air-bubbler ? Any brand, type You can recommend ?

Aquarium bubbler of any kind

 

[Lars100]

Many thanks Yggdrasil !
I appreciate that You point me in the right direction !
Have a nice Easter (and I guess I´ll be back here next week) !

 

[Yggdrasil]

And furthermore...clean the liquid ? How do I do that (and with what) without wasting all the goodies ?

Since you do not say what you are referring to with clean the liquid, I presume it was referring to the SilverChloride. It is whiter than snow and what you show that may look like AgCl is dirty and has liquid with potential value in it. Fill it with distilled or DI water shake or stir it well, get it properly hot and then siphon off the liquid after it has settled.
Then do it again.
As long as the liquid test positive to stannous you keep it for further processing.
When it no longer test positive set it aside for stock pot and waste treatment.
What is left in the beaker should now be as white as fresh snow.
It can be set aside for later conversion, but do not let it dry or be subjected to light.