yellow fluffy pddmg

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arthur kierski

Well-known member
Joined
Feb 10, 2008
Messages
1,119
Location
são paulo---brazil
could i burn this yellow stuff(incinerate) to black(grey ) powder?---- and the pd obtained dissolve again in ar or nitric----or dissolve the yellow stuf in nh4oh,filter and add hcl to form pdcl2(yellow) powder? i am asking because i am finding dificulty in dissolving yellow pddmg in nh4oh---
thanks for any advise
Arthur
 
You can dissolve it in 8 M HNO3 with heating.then denoxxing to make chloride and classic sequence for(NH4)2PdCl6 precipitation
 
Hello Arthur,

You can incinerate the yellow precipitate in an open crucible first, with access to air at about 600-650 deg C, tempering at the same temperature for 1-2 hours, then cover the crucible with a ceramic lid, heat further up to at least 800 deg C, where PdO is decomposed to the metal, holding this temperature for another 1-2 hours and then let cool the covered crucible in the oven, under minimum access of air.

The thus obtained Pd-sponge is readily dissolved with 32% HCl, diluted with half it's volume water, by moderate heating (70-80 deg C) and slowly adding 35% H2O2, diluted with an equal volume of water with constant stirring. Alternatively oxydation can be achieved by the slow addition of an aqueous solution of sodium chlorate (NaClO3)

ClO3(-) + 5 Cl(-) + 6 H(+) => 3 Cl2 + 3 H2O
H2O2 + 2 H(+) + 2 Cl(-) => Cl2 + 2 H2O

The elemental chlorine formed will oxidize the Pd to Pd(II) in PdCl4(2-), and, eventually to some Pd(IV) in PdCl6(2-). It is important, that you always have excessive HCl in the reaction mixture. I am recommending the HCl/chlorine-method for dissolving Pd-sponge or Pd-black, because in my hands dissolution in aqua regia in most cases turned out to be a messy reaction, only difficult to control, which often lead to extensive cleaning/recovering-actions of the work place under the fume hood.

Regards, freechemist
 
thanks Freechemist for your complete explanation-----when the problem arises again,i will try your method------although Suchos method worked perfectly---
regards and thanks
Arthur
 
freechemist

I have incinirated Pd-DMG before, more or less by the same order you have described. i vowed to never repeat that mistake again.
It tends to ignite and mess up the entire oven with a fluffy yellow deposite and the loss of metal was too much for me to bare.
The fluffy deposite will be there even if it does not catch fire... dare you to blow some air on it, a cloud of fireflies will cover the room and chase you down the hall...

Just a heads up for anyone wishes to try that.
 
Any chemists or otherwise knowledgeable folks want to speculate on how well hot concentrated sulfuric acid would work on redissolving the palladium from the dmg complex?
 
Ok I tried heating up the sulfuric acid and Pd-DMG complex, but I stopped too soon. Although the complex dissolved it reformed on dillution. Maybe more heat was needed.
 

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