Is this Palladium?

I'm working on precipitating the extract from a batch of monolithic capacitors and have a question.

Is this what Palladium looks like when precipitated?:




The solution tested positive with stannous chloride (brownish purple) before the precipitation. After precipitation it tests clear.

Steve

Steve,
What did you use for precipitation?
Sodium Chlorate or Ammonium Chloride?
I have only tried dimethylglyoxime, and that
ends up bright yellow. Harold or GSP will
probably be the ones to give you an answer,
but you already knew that I am sure.
Jim

Jim,

I used ammonium chloride and sodium chlorate.

I added the ammonium chloride to the hot concentrated solution followed by the sodium chlorate, but nothing happened. I let the solution sit for a few days and still nothing. I retested with stannous chloride and again had the same orange-brown/purple result. I presumed this was a mixture of gold and palladium (from the monolithic capacitors datasheet). I decided to try and drop the gold since the palladium would not drop. When I added the SMB, the yellow precipitate immediately formed.

Here's the test result:



Here's the filtered powder:




Now the solution tests barren to fresh stannous chloride.

This test batch was from a small 25 mL sample of a much larger batch that I plan on doing a palladium video on. I always do small tests runs before I film an experiment.

Thanks for the reply. Hopefully someone will confirm this is Palladium. I would have no doubts had the original precipitants dropped the powder.

Steve

Steve,
I have about a 1/2 gallon of solution from when
I processed the hammond organ contacts. I got
the same results on it as you did with stannous
chloride, so it should have palladium in it.
I was planning on doing it tomorrow with sodium
chlorate, I will let you know what I come up with.
I had good results with gold and SMB, I think the
PGM's will be tougher to get right.
Jim

lazersteve said:

Is this what Palladium looks like when precipitated?:

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Not in my experiences. When you precipitate with ammonium chloride and sodium chlorate, the precipitate is a deep scarlet color, and is often even deeper when being precipitated from a dirty solution (lots of base metals). The only time you can expect palladium to be yellow is if the precipitated scarlet colored salt is dissolved in ammonia, then re-precipitated with HCL, at which time it is yellow. That's according to Hoke. I did it only once and got the expected results. It may be that you have achieved something similar by your process. I'm at a loss.

The color of precipitate from DMG is a very deep yellow, much darker than what you've shown. It is a test you should perform so you become familiar with how it looks.

When platinum is precipitated, the color ranges from a light yellow through a light orange color. That is an instant reaction, assuming it is going to happen at all. If the solution is too dilute, it does nothing. It is accepted that the ammonium chloride is added to the solution while it's at room temperature. Should the solution contain platinum, it is then allowed to settle well and separated from the solution before attempting to precipitate palladium or other values. The color of your precipitate could pass for platinum, but I'm not suggesting that's what it is.

The solution tested positive with stannous chloride (brownish purple) before the precipitation. After precipitation it tests clear.

Click to expand...

It will be very interesting to see what you've created!

May I suggest you dissolve a tiny amount of your precipitate in water, then test it with stannous chloride, and if you have it, DMG? Use as little water as you can, so you have a concentrated solution. You can dilute it further if necessary-----but if you have palladium salt present, it will dissolve, whereas any gold will not. I'd also suggest you test for sulfur. Could it be?

Harold

Harold,

Thanks for the information. Unfortunately I don't have any DMG. I'm going to perfrom some other tests and post more on this thread. It is possible the solution contians platinum.

I'm real curious why the SMD dropped this powder. Could this be a pH reaction?

The original solution was made by dissolving 30,000 identical monolithic capacitors in AP for several months. A white powder speckeled with fine black particles (assumed undissolved Pt) formed in the bottom of the reaction vessel and was filtered off thru a very tightly packed funnel neck (to catch the very fine particulate). The solution was then evaporated down to 1/4 of it's original volume and treated with ammonium chloride followed by sodium chlorate.

When nothing happened I tried for the gold which appeared to be in the solution from the stannous test. The powder formed.

Today I'll take a few small samples of the resultant powder and test them. I'll also test a few more small samples of the mother liquor.

Steve

lazersteve said:

I'm real curious why the SMD dropped this powder. Could this be a pH reaction?

When nothing happened I tried for the gold which appeared to be in the solution from the stannous test. The powder formed.

Click to expand...

Some time ago, both Chris and I commented on the book published by George Gadja. In it, as I recall, he talked about precipitating palladium with SO2. While everything he said, to me, was nonsense, and did not support my experiences in the least, I now wonder if the yellow salt is palladium. It may precipitate yellow by his suggested method (I never tried it that way, so don't have a clue). That's why I suggested you dissolve a tiny amount and test it with stannous chloride---the test would be conclusive.

As for looking for gold, while I'm not suggesting you didn't have any in solution, the test you showed could easily confuse as being gold, but is nothing more than palladium. That's why it's so important to have DMG---which would precipitate all the palladium when you tested, allowing you to then test the solution for other values. Tests such as this are best carried out with the use of a spot plate. If you had gold present as well, the palladium, now fully precipitated in an insoluble form, would test barren, or show gold without the palladium reaction. You must get some DMG-----it is essential to your operation and would have been the perfect way to make this determination.

The question I have now is did your procedure precipitate the palladium from what was a solution that was too dilute to precipitate, and would not have precipitated at all had you not followed up as you did. I can't tell you the number of times I had both platinum and/or palladium in solution and failed to achieve precipitation. You finally come to terms with the fact that it won't happen, and turn to recovery, routinely, in the stock pot.

If you have enough curiosity to pursue this matter further, you can try calcining a tiny amount of the salt. Hoke discusses that adequately. If it is palladium, and you work slowly, so you don't lose the metal in the fumes, when it's finished it will show beautiful peacock colors plus pink. That's the oxides that form when you reduce the salt in the atmosphere. I used to use a Fisher burner with a quartz dish for the calcining process. Don't breath the fumes!

Harold

Steve,
I just tried to precipitate the palladium out of the solution
that I had from the Hammond organ contacts. No luck.
I heated it up and added sodium chlorate and got nothing.
Maybe there isn't enough in there to precipitate, although
it tests good for palladium with stannous chloride.
The solution turned a bright blue from the dark green/blue
that it was.
Is this why they say to boil down the solution to syrup to
concentrate the palladium before trying to remove it?
Here are some links to what the palladium should look
like with the different reagents;

Is this what it should look like after sodium chlorate also?;
http://cgi.ebay.com/Palladium-Ammonium-Chloride-5-grams-99-95-purity_W0QQitemZ220099210310QQihZ012QQcategoryZ104233QQrdZ1QQssPageNameZWD1VQQcmdZViewItem

This is what it looked like when I used DMG;
http://cgi.ebay.com/Diammine-Palladium-II-Chloride-5-grams-Pd-NH3-2Cl2_W0QQitemZ220101654126QQihZ012QQcategoryZ104233QQrdZ1QQssPageNameZWD1VQQcmdZViewItem
Jim

Did you ever do any more testing on this steve ?

I too was kinda waiting to see what became of this. LOL, I think he got mad & threw it out. I know I would have!

Guys,

I NEVER throw anything out.. just ask my wife! :lol:

Seriously though, the project has taken a back seat to the Gold Filled DVD. It's eating up my hard drive and time like it was going out of style. I ran into a few speed bumps with the GF (tin nitrate I think), but I've made it past that hurdle tonight.

I'll give the Pd another go starting next week. I melted the light yellow powder and got a super tiny BB of gray/white metal so I'm pretty sure we are dealing with Pd based upon the tests and the stannous chloride results.

I concentrate the solution again since my last update on the solution and hope to succeed at the precipitation on video soon. :wink:

Until then,

Steve

We know you stay busy Steve. We were just wondering. This just gives us something to look forward to. :wink:

Thanks for the work.

lazersteve said:

Guys,

I NEVER throw anything out.. just ask my wife! :lol:

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Steve, if our wives weren't so patient what would we do?

Yeh after seeing that ebay listing for diammine dichloro palladium I am reasonably sure that is your salt. You could always dissolve the bead in nitric acid just for giggles and grins but why make yourself redo the separation/precipitation again?

Buy the way your website is AWESOME! Thank you so much for your hard work. I have started a chemistry website but it is pretty barren right now as I haven't been able to add a lot to it. You went to godaddy.com too? Pretty friendly folks AFAIK.

Welcome to the forum Chloric1,

Thanks for the complements on my site, it has slowly evolved over the last few months. I need to go ahead and upgrade to remove the top banner ad. Keep working on your site a little at a time and it will all come together. I use my text editor to make small changes on a weekly basis and it has started to shape up just recently. I have more plans for the site, but all in due time.

Steve

Those who sacrifice liberty for security deserve neither

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:wink:

i know this is really old, but from me just searching around i figure id ask if you ever found out what it was. id say in 8 years you would have to figure it out by now haha

Looks like Pt from a gold solution.

Amazing how long ago this was, about six months after I joined the forum. Back when I was cutting my teeth on Pd and Pt.

Turns out precipitate was a Pd salt. There was no gold in the solution.

If you are interested in Pd processes on monolithic's check out this post I made six years after the post you are replying to:

Pd from Layered capacitors

It's important to look for the most updated information on a subject when you are researching any process. All of us learn new techniques along the way and many of these updates get posted to the forum.

If searching the forum for a particular subject matter, be sure to sort the results by date so you are aware of the 'latest and greatest' information.

Thanks for bringing up the memories; everything was so exciting back then, a lot less like work than it is today and more like an adventure!

Steve

Yes I figured this would have been your post from probably when you first started. You could tell from this post that you have come along way. I somehow stumbled upon it and just realized you never came back with a follow up. Sometimes I just jump around your post to soak up as much as I can.

lazersteve said:

Thanks for bringing up the memories; everything was so exciting back then, a lot less like work than it is today and more like an adventure!

Click to expand...

True, and the chief reason why I sold my small business and retired. The fun of refining had long gone. It was now just work.

Harold