Mixed Black PGM Powders

[kadriver]

Here is a shot of the platinum salt that was precipitated with saturated ammonium chloride after the liquid was filtered off.

Edit one time to add a picture

 

[kadriver]

Since there was palladium in the solution, I decided to add sodium chlorate to see if the palladium salt would form.

The video posted above shows the sodium chlorate being added the the solution.

This is a shot of the resulting precipitate that formed, and what the solution looked like after adding the sodium chlorate.

The precipitate was black - again, not what I was expecting.

 

[kadriver]

Before filtering, I did a stannous test.

It was a very faint orange - A tiny bit of platinum still remained in the solution.

There was no indication of palladium with the stannous test.

 

[kadriver]

Something definately looks wrong here.

This was my first go at platinum, and these procedures are all experimental in nature.

I have no clue what that black material is.

 

[kadriver]

Here is what I collected in the filter -

 

[kadriver]

This is supposed to be palladium salts - but it does not look like any that I have seen anywhere on the forum or in any publication.

I must have made a mistake somewhere - but I did gain some valuable experience with all these experiments.

 

[kadriver]

Top left = palladium salt ready for calcining.
Top right = Palladium DMG salt, needs further treatment.
Bottom left = the black precip from the NaClO3 precip (supposed to be palladium salt).
Bottom center = sparingly ammonia soluble brown colored (NH)4PdCl4(Ammonium terachloropalladate).
Bottom right = platinum salt precipitated with saturated ammonium chloride.

kadriver

 

[RaoOvious]

Looks like u have also dissolved and thus precipitated Rhodium along platinum thereby causing the platinum precipitate to have a greenish look instead of of fine canary yellow.

 

[kadriver]

I agree - the platinum salt did not look very clean, but there is a procedure to repurify - I'll try that to see if I can get it clean.

What really baffled me was the amount of palladium that was still there.

I did 5 nitric acid treatments to remove the palladium.

My last DMG test on the 5th nitric treatment showed little if any palladium.

Where did it come from? Just goes to show how difficult (for a novice like me) that PGM refining can be.

This did not turn out like I thought it would, but I gained much experience and knowlege.

I look back and see that the palladium refining was the most fun - it yielded some clean salt and pure metal.

Thanks for looking - no wonder not many people are eager to try platinum.

I have more material to work with - more to follow.

kadriver

 

[kadriver]

FYI, the dilute "lazersteve" method of separating Pt from Rh and Ir works remarkably well. I call it the lazersteve method because I saw Steve employ it on some iridium containing med material and then saw the resultant platinum product. If time is not an issue, it is the pre-eminent way.

Low and slow!

I searched the forum for hours and still could not find this post.

I even searched only Steve's posts.

Can someone point me in the right direction.

kadriver

 

[lazersteve]

Lou is referring to a visit he made to a job site where I dissolved a small batch of mixed platinum alloys from medical scrap.

I have not made these methods public because they are a source of income for my family that is vital to my livelihood. The last thing I want to see is another one of my methods being publicly cloned and spawned all over the internet. If this method where to be made public it could adversely affect my income and hence my family's welfare.

For this reason, I won't post about it on a public forum. I hope you can understand where I am coming from on this one.

Steve

 

[kadriver]

Absolutely Steve, no problem. I can clearly see how these processes are very valuable.

I don't blame anyone who does not want to reveal their hard-won techniques on a public forum.

I salute you for all that you have already given.

Aa far as I am concerned this will conclude this post - I got a great education and provided a path for others to follow.

Thank you!

kadriver

 

[lazersteve]

Kevin,

PM me if you have any further questions, I'm happy to help with what I can.

Steve

 

[RaoOvious]

Kevin really enjoyed ur fabulous series.Just concentrate on the main processes and u wod have ur answer,the secret lies in careful examination of things,which u already have done.

I would also stress that Lou should have guided u properly because his process has proved to b unfruitful,cause the whole chemistry changes when u have pt.pd.rh as blacks,and both nitric and sulfuric washes dissolve pt black as well.Just like silver alloyed with platinum and nitric wod dissolve both of them practically,same is the case with pgm blacks,one follows the other though its not supposed to follow theoretically.

Kevin great job,I would love to see another series by you.

 

[Lou]

Sulfuric washes do not dissolve appreciable platinum metal at all at any concentration ever.

NItric may dissolve platinum black, particularly if chlorinated tap water is used to dilute the solution.

Rhodium black won't appreciably dissolve in room temperature sulfuric or aqua regia. Given great heat, it will dissolve in both.

Probably enough to say that the processes aren't quantitative (they really never are in PGM chemistry) and can be done a hell of a lot faster. In some instances, it is beneficial to do it much faster so that less other metals get involved.

 

[Oz]

I would also stress that Lou should have guided u properly because his process has proved to b unfruitful,cause the whole chemistry changes when u have pt.pd.rh as blacks,and both nitric and sulfuric washes dissolve pt black as well.Just like silver alloyed with platinum and nitric wod dissolve both of them practically,same is the case with pgm blacks,one follows the other though its not supposed to follow theoretically

By all means I would love to hear you expand upon "your" knowledge of this separation and share what you know. I would enjoy hearing how you would have done this differently. Perhaps you could help Lou and I both in getting clean .999 seperations of mixed PGMs.

 

[RaoOvious]

"By all means I would love to hear you expand upon "your" knowledge of this separation and share what you know. I would enjoy hearing how you would have done this differently. Perhaps you could help Lou and I both in getting clean .999 seperations of mixed PGMs".

Oz

Sorry i cant share that valuable info on this public forum.

 

[samuel-a]

Now... isn't that convenient...

You knew you would be challenged, then why say anything at all?
If you are expecting others to show thier cards, be ready to show yours.

 

[RaoOvious]

I think there has been lots of meddling regarding this matter(I cited the observation rightfully and not to have a tug regarding showing cards ) which has been settled privately with the concerned person,and he has recognized the fact that all regarding PGM chemistry can be unfruitful and unpredictable sometimes as happened with the current scenario.

"Now... isn't that convenient...", And by the way i didn,t started a thread about something unpredictable at the first place so no need to show mine,if i wod have to i wod share wid him personally.

Its not about being bully or something,it was an honest(may be got infuriated) input at something that was going no where. Hope everyone would get it.

 

[Noxx]

Quick question concerning the mixed black PGMs powder.

What are you guys doing with it ? I have some that I wish to sell.

Is it better to have it assayed first ?


Thank you