Palladium purification problem
Using the process described in Hoke's book on pages 176,177 (purifying Palladium)
I had redissolved Palladium Chloride (red salt) in 20% Ammonium hydroxide solution,
filtered it and precipitated it by adding HCL . Got lots of Palladosammine Chloride
(Yellow salt) so far so good.
Because I had started with a mixture of metals containing Palladium and my goal was
Pure Palladium I needed one more step to achieve this .I vacuum filtered it and washed it several times with distilled water .
Now I redissolved the Yellow salt in more Ammonium Hydroxide (with some heat ) and again added HCL . This time it took a lot more HCL to precipitate the Yellow salt (this is where I think I goofed) I should have used a pH indicator instead of just adding HCL . Anyway the Palladosammine Chloride formed as expected however the solution began to turn dark red??? The yellow salt remained (later washed and heated to make Palladium Sponge ) but the solution still contained a substantial amount of Palladium (tested with Stannous Chloride) .
My question is how do I get my Palladium back from this solution ?
It already has a lot of HCL in it . I did try some Ammonium Chloride but it just redissolved and turned red clear again.
Any suggestions?
Using the process described in Hoke's book on pages 176,177 (purifying Palladium)
I had redissolved Palladium Chloride (red salt) in 20% Ammonium hydroxide solution,
filtered it and precipitated it by adding HCL . Got lots of Palladosammine Chloride
(Yellow salt) so far so good.
Because I had started with a mixture of metals containing Palladium and my goal was
Pure Palladium I needed one more step to achieve this .I vacuum filtered it and washed it several times with distilled water .
Now I redissolved the Yellow salt in more Ammonium Hydroxide (with some heat ) and again added HCL . This time it took a lot more HCL to precipitate the Yellow salt (this is where I think I goofed) I should have used a pH indicator instead of just adding HCL . Anyway the Palladosammine Chloride formed as expected however the solution began to turn dark red??? The yellow salt remained (later washed and heated to make Palladium Sponge ) but the solution still contained a substantial amount of Palladium (tested with Stannous Chloride) .
My question is how do I get my Palladium back from this solution ?
It already has a lot of HCL in it . I did try some Ammonium Chloride but it just redissolved and turned red clear again.
Any suggestions?