Ammonia Soluble Hexachloropalladates (IV)

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kadriver
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Re: Ammonia Soluble Hexachloropalladates (IV)

Postby kadriver » September 29th, 2014, 1:28 am

Here is a photo of the precipitate mentioned earlier (top photo).

I've been so busy with other refining tasks that I have not had time to do anything with this.

But I am starting to see more PGMs coming through my shop.

The bottom photo; stannous tests taken from solutions that dissolved some jewelers filings and clippings.

Those orange test strips where taken AFTER the gold had been precipitated.

The test came from the green solution in the middle photo after the gold was precipitated with SMB.
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Re: Ammonia Soluble Hexachloropalladates (IV)

Postby kadriver » February 4th, 2018, 2:40 pm

I'm getting ready to refine the Pd salt from my silver cell slimes that I just posted. Believe it or not, I've still got the solutions of palladium that I was working with in this thread!

I've completely forgotten how to do it because it was several years ago. But now I'm ready to shoot a video of the entire process.

i may have to do this in several parts.

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Re: Ammonia Soluble Hexachloropalladates (IV)

Postby Lou » February 4th, 2018, 6:53 pm

Would you like any advice?


There are some methods you can use that are not the traditional [PdCl4]2- to [Pd(NH3)4]2+ method that most use. That method largely but inadequately separates Pd from Pt.

In that method, one boils the freshly oxidized solution...Pd(IV)-->Pd(II) + Cl2 while Pt remains Pt(IV) and can come down as X2PtCl6 and is rinsed with ammonium or potassium chloride that is slightly acidic. The liquor is then made ammoniacal and the pink salt dissolved up. Pure Pd yields a colorless solution. Filtration from any hydroxides and then acidification with HCl to a pH of 2 yields Pd(NH3)2Cl2, the yellow salt often found as an end product of conventional Pd refining.

If you're interested Kevin, we can talk about about the bromide method. In my opinion, the bromide method makes as good as Pd as any other!
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Re: Ammonia Soluble Hexachloropalladates (IV)

Postby Lino1406 » February 5th, 2018, 10:59 pm

Wouldn't be the same result if dropping the TCCA (or KClO3) inside?

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Re: Ammonia Soluble Hexachloropalladates (IV)

Postby Lou » February 6th, 2018, 8:18 am

Can you elaborate Lino?
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Re: Ammonia Soluble Hexachloropalladates (IV)

Postby Lino1406 » February 6th, 2018, 12:54 pm

I watched the system that produces chlorine and drives it into the system. Instead, I know the KClO3 method, which by dropping KClO3 into the solution produces chlorine in situ and I assume TCCA will do same.

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Re: Ammonia Soluble Hexachloropalladates (IV)

Postby Lou » February 6th, 2018, 4:33 pm

I see.

Much better to use TCCA (method on sciencemadness.org) as no risk of ClO2!
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Re: Ammonia Soluble Hexachloropalladates (IV)

Postby kadriver » February 7th, 2018, 5:15 am

Lou wrote:Would you like any advice?


There are some methods you can use that are not the traditional [PdCl4]2- to [Pd(NH3)4]2+ method that most use. That method largely but inadequately separates Pd from Pt.

In that method, one boils the freshly oxidized solution...Pd(IV)-->Pd(II) + Cl2 while Pt remains Pt(IV) and can come down as X2PtCl6 and is rinsed with ammonium or potassium chloride that is slightly acidic. The liquor is then made ammoniacal and the pink salt dissolved up. Pure Pd yields a colorless solution. Filtration from any hydroxides and then acidification with HCl to a pH of 2 yields Pd(NH3)2Cl2, the yellow salt often found as an end product of conventional Pd refining.

If you're interested Kevin, we can talk about about the bromide method. In my opinion, the bromide method makes as good as Pd as any other!


Thanks Lou. I'm looking to go the easiest and least technical route. I did some before and got some metal. I dissolved the brick red Pd in ammonia, then acidified with HCl, filtered out the Pd salt and calcined It in a fuzzed quartz dish. It made 992 palladium. It worked well for me and seemed straight forward.

What's the pay out for palladium. If I sell it, can I just send you the sponge? Thank you.

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Re: Ammonia Soluble Hexachloropalladates (IV)

Postby anachronism » February 7th, 2018, 4:56 pm

To quote a very well respected Australian forum member:

"The only reason I am still here at my ripe old age is because I let other people play with PGMs. Most of them are dead now."
If you keep on doing what you've always done then you'll just keep on getting what you've always got.

"If you can bear to hear the truth you’ve spoken twisted by knaves to make a trap for fools, or watch the things you gave your life to broken, and stoop and build ‘em up with wornout tools" -- Rudyard Kipling

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Re: Ammonia Soluble Hexachloropalladates (IV)

Postby NanoCat » April 3rd, 2018, 5:43 pm

Lou,
so what is your non traditional method for the Pt/Pd separation?
I have mixed PGMs that came down as primarily Canary Yellow with some deep orange. I have hit it with KClO3 getting it hot to 77C and the pH is 1.8.
The oxidizer is slowly going off and the yellow layer in the beaker diminishing.
The supernatant is mostly clear pale yellow. Again all the PGMs are in that mix but if I can get even the Pd and Pt isolated that will help me get those to the refiner.

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Re: Ammonia Soluble Hexachloropalladates (IV)

Postby kadriver » April 17th, 2018, 2:15 pm

I finally got my palladium refined.

I've turned this post into a video

here is the link to the video:

viewtopic.php?f=52&t=26855

any comments would be welcomed

Thank you

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Re: Ammonia Soluble Hexachloropalladates (IV)

Postby kadriver » April 19th, 2018, 3:08 pm

Here is a picture of the pure palladium button 3.6 grams from the video
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Re: Ammonia Soluble Hexachloropalladates (IV)

Postby kadriver » April 21st, 2018, 3:54 pm

kadriver wrote:Here is a picture of the pure palladium button 3.6 grams from the video



It sold for $150 through my eBay store.
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Re: Ammonia Soluble Hexachloropalladates (IV)

Postby VK3NHL » April 25th, 2018, 9:44 pm

Great Video's as usual Kevin... Thanks for sharing..
regards
Tony


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