Precipitant for palladium

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Testing!

Why run blindly?

Dissolve a tiny sample in water, and test with stannous chloride.

If you still have questions, test, also, with DMG. Test the same sample with stannous chloride after it has been tested with DMG. If there it platinum present, it won't be disguised by the palladium reaction because you will have precipitated the palladium with DMG.

READ HOKE!

Harold
 
Harold_V said:
Testing!

Why run blindly?

Dissolve a tiny sample in water, and test with stannous chloride.

If you still have questions, test, also, with DMG. Test the same sample with stannous chloride after it has been tested with DMG. If there it platinum present, it won't be disguised by the palladium reaction because you will have precipitated the palladium with DMG.

READ HOKE!

Harold

The solution contains a lot of gold, which is still not precipitated. Stannous chloride show black color due to high gold concentration. Maybe it would be wiser to precipitate gold first, not platinum and palladium?
 
lazersteve said:
Do you have a photo of the orange powder you can post?

Steve

I will post tomorrow, it is night in Europe now, and I do not have places with good illumination ...
 
Drop your gold first.
Gold has a way of masking pt and pd with the stannous test if they are in solution together.

Mark
 
Renaldas said:
The solution contains a lot of gold, which is still not precipitated.
Not a problem. Do you have any ferrous sulfate? Even if you don't use it for precipitation, you should have a small supply on hand for testing in cases just like this.

Take a drop of solution from your vessel, using a stirring rod. Place the drop in a cavity in a spot plate. Add a small crystal of ferrous sulfate. That should precipitate all of the gold, which will be evident by the formed brown powder, or even by a shiny skin of gold.

Once the gold has been precipitated, you can then test the same drop with stannous chloride. With the gold gone, you can then read the test better.

If, by chance, the remaining solution is heavy in palladium, you can eliminate the palladium by adding a drop of DMG. You can then test with stannous chloride for platinum.

Read Hoke. All of this is well explained there, although you may have to dig it out, and you may have to draw some conclusions, using logic. That worked for me.

As far as I'm concerned, it's always smartest to precipitate gold before the platinum group. You can't wash the salts of the platinum metals without losing some to the wash. Also, the concentration level may be too low to precipitate, anyway. By eliminating the gold first, assuming you have enough of the platinum group to justify the effort, you can then evaporate the solution (for concentration), then recover that which will cooperate.

I found it was generally better to just pour platinum solutions to the stock pot unless I was sure there was an abundance. That way they get concentrated so you can recover them in the future.

Harold
 
You must be 100% certain your solution is properly denoxxed before adding ferrous sulfate or ammonium chloride to any mixed gold, platinum, and palladium solutions. Below is an abbreviated list of some methods by which palladium will precipitate, pay very close attention to the last two items in the list below:

Standard Methods of Chemical Analysis said:
Palladium Detection

...

Ammonia added to a concentrated solution gives a flesh-red precipitate. PdCl2NH3, soluble in excess of ammonia. If HCl is added to this solution the yellow compound of pallad-ammonium chloride, Pd(NH3Cl)2, is deposited.

Sulfur dioxide precipitates the metal from the nitrate or sulphate solution but not from the chloride.

Cuprous chloride precipitates the metal from the sulphate, nitrate and chloride solution when they are not too strongly acid.

...[ ]...

Potassium nitrite precipitates a yellow crystalline powder, K2Pd(NO2)4.

Ferrous sulphate slowly produces a black precipitate of metallic palladium from the nitrate.

Ammonium chloride precipitates palladium as (NH4)2PdCl4 from the nitrate.

...

From the above you can clearly see that precipitants behave very differently under different conditions. This is one of the difficulties when working with PGMs for beginners who tend to be in a hurry to get results. If you cut corners and do not properly treat your solutions prior to adding the precipitants you will end up with mixed metals and your refining efforts will be thwarted.

Steve
 
lazersteve said:
You must be 100% certain your solution is properly denoxxed before adding ferrous sulfate or ammonium chloride to any mixed gold, platinum, and palladium solutions. Below is an abbreviated list of some methods by which palladium will precipitate, pay very close attention to the last two items in the list below:

Standard Methods of Chemical Analysis said:
Palladium Detection

...

Ammonia added to a concentrated solution gives a flesh-red precipitate. PdCl2NH3, soluble in excess of ammonia. If HCl is added to this solution the yellow compound of pallad-ammonium chloride, Pd(NH3Cl)2, is deposited.

Sulfur dioxide precipitates the metal from the nitrate or sulphate solution but not from the chloride.

Cuprous chloride precipitates the metal from the sulphate, nitrate and chloride solution when they are not too strongly acid.

...[ ]...

Potassium nitrite precipitates a yellow crystalline powder, K2Pd(NO2)4.

Ferrous sulphate slowly produces a black precipitate of metallic palladium from the nitrate.

Ammonium chloride precipitates palladium as (NH4)2PdCl4 from the nitrate.

...

From the above you can clearly see that precipitants behave very differently under different conditions. This is one of the difficulties when working with PGMs for beginners who tend to be in a hurry to get results. If you cut corners and do not properly treat your solutions prior to adding the precipitants you will end up with mixed metals and your refining efforts will be thwarted.

Steve

Thank you!
Maybe it is better to use sodium sulfite for gold precipitation?

I get this after adding of ammonium chloride to my solution. Gold is still in solution.
PGM-precipitate.jpg
 
Lets look at this. I think, it is silver-palladium post and core. It dissolves in AR very slowly and after some time orange coloured substance can be obtained on the surface. What do you think, may it be silver-palladium alloy?

Refining-post-and-core.jpg
 
Renaldas said:
may it be silver-palladium alloy?
A simple test with nitric acid will reveal if it is, or not. Both silver and palladium are soluble in dilute nitric. Place one in a small container with a few drops of acid and water and heat. If the items are as you suspect, the resulting solution will be a dark grown, perhaps with a green highlight. A test of the solution with a drop of HCl (or some salt) will yield silver chloride. A test with DMG will yield a bright yellow precipitate if there is palladium. It will also react with stannous chloride, yielding various color reactions. Blue, green, or various shade of brown/black can be palladium. The best test is DMG, which will remove all doubts.

Harold
 
Hello Forum
May someone can help me with some basics. I´m new to the matter. I had some black sand, mostly magnetite. I read recently that Pt or Pd come often along with magnetite, so I roasted them, washed and add nitric. I let it boil and tested with SnCl. The solution show´s a canary yellow color change. I try to precipitate with Sodium Carbonate and Formic Acid while boiling, but it´s just turned into a reddish solution and nothing comes out. May someone has experience with this type of magnetite and can give me an idea how to make it better. Thanks
 
Hello Forum
May someone can help me with some basics. I´m new to the matter. I had some black sand, mostly magnetite. I read recently that Pt or Pd come often along with magnetite, so I roasted them, washed and add nitric. I let it boil and tested with SnCl. The solution show´s a canary yellow color change. I try to precipitate with Sodium Carbonate and Formic Acid while boiling, but it´s just turned into a reddish solution and nothing comes out. May someone has experience with this type of magnetite and can give me an idea how to make it better. Thanks
You need to hide those chemicals of yours and start studying.
If and a big IF there is PGM salts they are extremely toxic and need to be handled in a safe environment with proper protection.
First you roast MLCCs then black sands.
Read Hokes book and the safety section if the forum.
Then return and ask questions before you do anything more.
 
To slow your enthusiasm a bit, that yellow is likely iron.
Pd and Pt look different and nitric does not dissolve Pt.
As said put your things aside in a safe place and study and ask if you get lost.
 

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