yellow palladium from ammonia, what is next.

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tracar

Member
Joined
Feb 17, 2022
Messages
11
Location
Alberta
20.2g palladium purified in ammonia precipitated out with Hcl. how do i reduce it to metal from here using formic acid / hydroxide method ?.
i see many videos of converting red brick to metal. not much on yellow.
 
20.2g palladium purified in ammonia precipitated out with Hcl. how do i reduce it to metal from here using formic acid / hydroxide method ?.
i see many videos of converting red brick to metal. not much on yellow.
I think, both Formate reduction and calcining will work for both the red and yellow salts.
 
i tried another way, i added enough water / conc nitric to liquefy it, a bit of heat, a bit of stirring 10 min, and let it cool, then added NaOH until all dissolved. this was now a dark redish brown semi clear liquid, brought to a near boil then slowly added the formic, took 15min till reduction, if added too fast it likes to run away and boil over 5 times its volume. learned that from Streetips ;) left with a nice black clumping powder in the clear solution :)
 
i tried another way, i added enough water / conc nitric to liquefy it, a bit of heat, a bit of stirring 10 min, and let it cool, then added NaOH until all dissolved. this was now a dark redish brown semi clear liquid, brought to a near boil then slowly added the formic, took 15min till reduction, if added too fast it likes to run away and boil over 5 times its volume. learned that from Streetips ;) left with a nice black clumping powder in the clear solution :)
What about reading Hokes book or the forum and doing it properly.
I have not seen Sreetips video on this but it is not according to standard methods I believe.
I’m afraid you might have losses.
 
In the conversion, I do not recognize your procedure.
Even if it somewhat similar to the methods in Hokes book and here on the forum.

Have you read the recommended links, especially the one on safety?
PGM salts are extremely toxic, not immediately but accumulative.
 
In the conversion, I do not recognize your procedure.
Even if it somewhat similar to the methods in Hokes book and here on the forum.

Have you read the recommended links, especially the one on safety?
PGM salts are extremely toxic, not immediately but accumulative.
what loss in the conversion do you mean?

and by metal ions in solution should not be rolled rubbed licked or splashed in the eyes or poured on your lab partner , yes i learned this years ago. fortunately my lab has a nice fume hood to do all the unrecognized procedures in.
 
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what loss in the conversion do you mean?

and by metal ions in solution should not be rolled rubbed licked or splashed in the eyes or poured on your lab partner , yes i learned this years ago. fortunately my lab has a nice fume hood to do all the unrecognized procedures in.
Sorry, I have been on the road most of the day.
We have members dying from exposure to PGM salts, so it is no joke.
What you describe is our everyday salts, not PGM salts.
Regarding PGM salts always gloves when handling even cleaned vessels used.
No other refining in that part of the Hood and everything that has been close to the actual site, is "burned" as can not be used elsewhere.
Ask Orvi or Lou or the others refining PGMs.

So this is no joke, and then talking about licking stuff.
Do not do that again!!!

You have never replied to reading the safety section or even Hokes book?
 
Sorry, I have been on the road most of the day.
We have members dying from exposure to PGM salts, so it is no joke.
What you describe is our everyday salts, not PGM salts.
Regarding PGM salts always gloves when handling even cleaned vessels used.
No other refining in that part of the Hood and everything that has been close to the actual site, is "burned" as can not be used elsewhere.
Ask Orvi or Lou or the others refining PGMs.

So this is no joke, and then talking about licking stuff.
Do not do that again!!!

You have never replied to reading the safety section or even Hokes book?
You must be tired from driving too much,
If Talking about what not to do gets you angry then there are bigger issues. So please do not do that again.

I will add that this was 23g of palladium disolved in AR and PD seperated from its fractions. so how you came up with this being Everyday salts eludes me.

And to answer your question. Yes i have an offline version of her documents.

Take care and get some rest !
 
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There's a huge difference between anger and concern.
Platinum group metals are extremely dangerous and will kill you.
I have refined my share of platinum and palladium but not without a plan.
I educated myself before I got started because of the known dangers and I would not recommend trying without the knowledge or a plan in place even though I have learned better ways than when I first started I had a very good understanding of how to safely recover my PGM's while minimizing
my exposure to the metal salts.
Please don't get offended by anyone's concern for your health because this forum and its members are here to help you learn techniques and safely.
 
and by metal ions in solution should not be rolled rubbed licked or splashed in the eyes , yes i learned this years ago. fortunately my lab has a nice fume hood to do all the unrecognized procedures in.
There's a huge difference between anger and concern.
Platinum group metals are extremely dangerous and will kill you.
I have refined my share of platinum and palladium but not without a plan.
I educated myself before I got started because of the known dangers and I would not recommend trying without the knowledge or a plan in place even though I have learned better ways than when I first started I had a very good understanding of how to safely recover my PGM's while minimizing
my exposure to the metal salts.
Please don't get offended by anyone's concern for your health because this forum and its members are here to help you learn techniques and safely.
I get it. I confused your love for a more condescending note. Im sorry
 
You must be tired from driving too much,
If Talking about what not to do gets you angry then there are bigger issues. So please do not do that again.

I will add that this was 23g of palladium disolved in AR and PD seperated from its fractions. so how you came up with this being Everyday salts eludes me.

And to answer your question. Yes i have an offline version of her documents.

Take care and get some rest !
You need to wind down a few notches.
We are trying to help our members and that includes keeping them alive.
Dead people do not learn much.

PGMs are an order of magnitude worse than any other salts we handle and needs to be handled with care and respect.
So I suggest reading this nice book you have and then rereading it, before you implement modern safety protocols to what she writes.
Search and read everything from Freechemist (RIP), Orvi , Lou, Lazersteve and more.
 
diamminopalladium (II) chloride, the salt you're talking about (made by acidifying the tetrammino palladium II cation that was produced by long digestion in c. ammonia) is easily reduced with formic acid at pH 4.5. Ammonium formate is preferred because it doesn't leave cationic impurities in the sponge produced. The sponge must be dried, washed with DI water, and compressed prior to melting under inert gas.
 
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diamminopalladium (II) chloride, the salt you're talking about (made by acidifying the tetrammino palladium II cation that was produced by long digestion in c. ammonia) is easily reduced with formic acid at pH 4.5. Ammonium formate is preferred because it doesn't leave cationic impurities in the sponge produced. The sponge must be dried, washed with DI water, and compressed prior to melting under inert gas.

Yes, i wanted to dissolve it completely before i added the formic to ensure there were no entombed particles that did not convert . It will remain as Black for catalytics later. Thankyou for the reply.
 
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