Palladium Complete Sequel

[necromancer]

very nice, thank you

i am running 3.5 lbs of MLCC's, your post helps

 

[RaoOvious]

your post helps

That was its purpose precisely.Good luck with MLCC's.....

 

[9kuuby9]

Very helpfull!

So if I understood it correctly, starting from (NH4)2PdCl6; you filtered the sponge red and then digested it in Ammonium hydroxide, from their you added HCl to precipitate Yellow Palladium salt (DiamminedichloroPalladium II Chloride) and then filtered the yellow sponge.

How did you reduce the Pd metal from their using Formic acid and NaOH?

and did you wash all your Pd salt sponges residuals with a cold solution of 15% ammonium chloride?

 

[RaoOvious]

So if I understood it correctly, starting from (NH4)2PdCl6; you filtered the sponge red and then digested it in Ammonium hydroxide,from their you added HCl to precipitate Yellow Palladium salt (DiamminedichloroPalladium II Chloride) and then filtered the yellow sponge.

Yes except,before adding HCl you must filter the transparent yellow Palladium Solution.And i wont name the Palladium salts as 'sponge red and yellow sponge'.

How did you reduce the Pd metal from their using Formic acid and NaOH?

Add DI water(Approx. 20 ml for 1 gram of Palladium or 10 ml for 1 gram of yellow salt) to Yellow diammine salt,then add 1 ml of formic acid for 4 gram of yellow salt or 0.5 ml for 1 gram of Pd metal in yellow salt i.e(1 gram yellow salt contains almost .5 gram of Pd metal),heat them upto to 65 C,then slowly add 6.25 M(25% NaOH solution or 250 grams NaOH per litre of water) NaOH solution such as for 1 gram metal or 2 gram yellow salt 1.7 ml of 6.25 M NaOH should be added.Suddenly after some greenish look all the yellow metal would be converted into beautiful settling Pd sponge.

and did you wash all your Pd salt sponges residuals with a cold solution of 15% ammonium chloride?

Red (NH4)2PdCl6 should be specially washed whereas Yellow Diammine can also be washed with cold DI water instead of 15% ammonium chloride.

 

[9kuuby9]

RaoOvious thank you for the answer I really appreciate it

After converting the Yellow diammine salt to Pd metal; is their any need for washes?

Or just regular Hot Di. water washes?

 

[RaoOvious]

Yes,hot DI water washes would suffice until the PH gets neutral.

RaoOvious thank you for the answer I really appreciate it

Appreciated.

 

[9kuuby9]

Is it possible to recover Pd from a solution using Ammonium Hydroxide and HCl instead of Sodium Chlorate?

Assuming I dissolved Pd using AR and denoxx it from any NO2, and then added a saturated solution of Ammonium Chloride.

Because I can not get my hands on Sodium Chlorate.

 

[lazersteve]

You'll need a chlorine source along with the ammonium chloride to recover the Pd. This can be a chlorate, hypochlorite, or even chlorine gas.

Steve

 

[9kuuby9]

Thank you for the respons Steve.

 

[RaoOvious]

Yes you can.

First make sure that the volume of solution after denoxxing is 10-15 ml/gm,add saturated solution of NH4Cl and then make sure that there are no needle shaped brown crystals of Ammonium tetrachloropalladate.Then add concentrated NH4OH(35%) and let it sit overnight.(You may sometimes need to heat and stir it to get all the Pd convert into tetraammine solution)

Filter the Palladium Tetra-ammine solution,add HCL(PH 2-3) to get purified yellow Palladium Diammine salt.

 

[9kuuby9]

Your answer is appreciated as always

When do you actually know when you have added enough saturated solution of NH4Cl? Would doubling the existing volume with NH4Cl suffice?

 

[lazersteve]

There seams to be a little confusion as to what the contents of your solution are. If you have a dirty starting solution, ammonium hydroxide will precipitate lots of other metals, not just Pd. If your goal is to purify the Pd, this is not the way unless you have a pure palladium solution.

If you are working with a dirty solution, you will need to selectively precipitate the Pd.

Steve

 

[Marcel]

Very informative.
Thanks for sharing!

 

[9kuuby9]

You'll need a chlorine source along with the ammonium chloride to recover the Pd. This can be a chlorate, hypochlorite, or even chlorine gas.

Steve

Would a solution of 14% hypochlorite be able to selectively precipitate Pd as (NH4)2PdCl6?

There seams to be a little confusion as to what the contents of your solution are. If you have a dirty starting solution, ammonium hydroxide will precipitate lots of other metals, not just Pd. If your goal is to purify the Pd, this is not the way unless you have a pure palladium solution.

If you are working with a dirty solution, you will need to selectively precipitate the Pd.

Steve

Thank you for clearing that up Steve!

 

[lazersteve]

Hypochlorite reacts with free HCl to form chlorine gas in situ. The higher the chlorite concentration the better, as Pd precipitates best from concentrated solutions.

Calcium Hypochlorite is a dry bleaching powder that will work.

Concentrated bleach (unscented and not color safe) will also work in a pinch.

Steve

 

[RaoOvious]

When do you actually know when you have added enough saturated solution of NH4Cl? Would doubling the existing volume with NH4Cl suffice?

It doesn,t work like that.For 1 gram of Pd in solution,prepare 37.1% NH4Cl solution having 1.5 grams of NH4Cl(1.5 times weight of Pd).For example if one has approx. 15 grams of Pd in Solution,then add 22.5 gm(1.5 times Pd) of NH4Cl crystals in approx. 60 ml of water,then pour in into the Pd containing solution.


22.5*100/37.1

 

[kadriver]

I am getting ready to do this experiment in another thread, showing a little more detail, and under the guidance of Rao who has helped me along very graciously.

Here is the beginning of that thread: http://goldrefiningforum.com/phpBB3/viewtopic.php?f=51&t=18907

The Pd black powder I am working with in this thread came from extractions with nitric acid from catalytic converter mixed black PGMs.

I am planning to use a gas generator just like the one in this video to dissolve the Pd black powder - except I'll be using a small gas bubbler instead of a beaker to hold the Pd black powder.

The gas generator in the video uses HCl dripped onto a slurry of trichloroisocyanuric acid (crushed up pool chlorine tablets from the hardware store).

I've used it before and it works perfectly - as long as my fume hood stays running.

[youtube]http://www.youtube.com/watch?v=Iwvt_QHeb7o[/youtube].

 

[9kuuby9]

Thx for new post kadriver

Rao really did help us quite a lot with Pd processing

Btw has any of you used Al to cement Pd from a nitrate solution? because it takes days before you see some flakes falling down; Or is it because of the extra HNO3?

(The nitrate solution contained some silver nitrate So I separated the salt using HCl to create AgCl, this reaction creates HNO3)

 

[kadriver]

Btw has any of you used Al to cement Pd from a nitrate solution? because it takes days before you see some flakes falling down; Or is it because of the extra HNO3?

Hello, I have never used aluminum to cement Pd.

I am processing some silver cell slimes to try and get a little palladium by cementing on copper.

kadriver

 

[samuel-a]

Al is practcally inert in the presence of NO3-