Ammonia Soluble Hexachloropalladates (IV)

[kadriver]

In a short amount of time some yellow powder began to appear floating on top of the liquid in the beaker.

As time progressed the yellow salt began to accumulate on the bottom of the beaker.

Since I have no experience with this, I can only assume that this yellow salt is the platinum.

It is quite yellow in appearance.

 

[kadriver]

My next task is to get the rest of the un-dissolved salt to dissolve by adding in a little HCl.

Then I'll filter out the yellow powder and add the filtrate to the main solution and re-concentrate to about 46ml.

Then filter out any more Pt salt that forms.

Then, if all goes well, chlorinate the solution with chlorine gas to form the ammonia soluble hexachloropalladate (IV).

kadriver

 

[Lou]

Looks more like mostly a Pt gig.

 

[kadriver]

The liquor does look orange. I'll know more later today.

 

[kadriver]

I had forgotten all about this post.

I still have the beaker sitting somewhere in my shop - probably dried to a crisp by now.

I need to get this back out and start working on it again.

 

[kadriver]

I jumped out of bed and went to my shop.

Sure enough, there was the beaker up on a shelf long forgotten.

It is dry as a bone, how should this be re-hydrated?

It already has 15% ammonium chloride in with it, just add a little distilled H2O?

I have some more15% ammonium chloride solution.

 

[Lou]

Mix of complex Pd/Pt salts and chloroplatinates, by visual appearance and correlating with what I said before up thread before you forgot about it.

You can digest it all in aqua regia and rid it off ammonium chloride, and start over.

Lou

 

[kadriver]

That's what I'll do Lou, thank you.

 

[kadriver]

I got this dissolved again and I will start it all over again.

I also have some more PGM from DMG precipitations out of silver digestions.

I am going to throw it all together (unless someone here tells me not to).

I also have a platinum ring that I may dissolve and throw in the mix - unless this would be unwise (the ring XRF'd at 93.5% Pt)

 

[Lou]

You better roll that ring out or you'll be dissolving it til the cows come home.

Usually we melt with copper for bulk metallics, sample, off to the races.


You need to make a game plan and follow the flow sheet.


Lou

 

[kadriver]

Lou,

I've got a friend who has a metal roller and I'll get him to help me roll it real thin.

I remember trying to dissolve a piece of Pt the size of a match head - it took about 6 hours and still wasn't completely dissolved.

I am using old knowledge from doing this the last time, it seems much easier this time since I've done it before.

Starting over was a good suggestion.

I got the salts dissolved in hot AR

Edited once to correct photo

 

[kadriver]

I added zinc turnings after filtering.

The solution was concentrated and the zinc turnings turned almost instantly into black powder.

Edited once to correct up-side-down photo

 

[kadriver]

I had a bunch of filters with DMG precipitated Pd so I put them in a beaker and dissolved in hot AR - filters and all.

Edited once to correct. Up-side-down photo

 

[kadriver]

After everything dissolved I put some ice in to cool the solution so it would not blow a hole in the filter paper.

Edited once to correct up-side-down photo

 

[kadriver]

Stannous test to verify I had metal in solution.

 

[kadriver]

I filtered the solution to remove solids then put the solution back in the cleaned beaker

 

[kadriver]

I then combined the two batches into one beaker and added more zinc turnings to get the PGMs to cement out as black powder.

 

[kadriver]

The zinc was getting dissolved fast by all the excess acid so I added a little sodium carbonate to get the pH adjusted up. I should have done this first before adding the zinc to pH 2 to 3. Still learning.

 

[kadriver]

The PGM blacks were coming out of solution nicely.

This is as far as I got this evening.

I have about 5 pounds of pure zinc that I ordered. My friend has a big milling machine and he is going to let me use it to make turnings out of these bars in the morning at 9am so I got to sign off and get some sleep.

More to follow.

kadriver

 

[mls26cwru]

thank you for restarting this thread... I think i am going to be dealing with Pd soon, so i am going to be following this thread closely! thanks again!