Refining : pt pd rh with cm hokes methode

[Abdoulapapatte]

I try with 50-gram of this alloys

I attacked the alloy with aqua regia, approximately 1300 ml of 37% HCl and approximately 350 ml of 65% HNO3. containing platinum (Pt), palladium (Pd), and rhodium (Rh). The composition of the alloy is as follows:

Platinum (Pt): 77.55%
Palladium (Pd): 14.18%
Rhodium (Rh): 8.15%

After the complete dissolution of the acids on the alloy, I obtained a deep purple, red-purple solution.


After complete digestion , I add amonium chloride with water
( satured water[ c ] = +- 10% Nh4Cl)

Results: platinum comings in yellow precipitate:




After wash with nh4cl , I reput inse hot water and dilute , before I analyse simple

Yes it's platinium now I'm shure

Once the platinum chloride salt had completely dissolved in hot water, we then formed ammonium formate with ammonia and neutralized it to a pH of 6.9 using formic acid.
The platinum will then precipitate with the action of ammonium formate. If you want to recover your powder quickly, you should add the ammonium formate slowly, minute by minute, very gently. Also, observe the color of your solution, which will change from yellow to clear and translucent.

So, you are supposed to recover this black powder, which in theory is platinum. And since we have a spectrometer, we place this black powder under the spectrometer and analyze the received spectrum.


Platinium is août of solution , I'm very disappointed, because contamination Rhaaaaaaaaaa

But fist time it's ok


If you don't mind, now I am finally interested in palladium, and I could have several options for how to refine it, knowing that the solution now contains both palladium and rhodium. So, you need to precipitate the palladium without focusing on the rhodium for the moment and leave it in solution.

I decided, and I'm not sure if it's the right choice, but I used sodium chlorate. Normally, I should achieve a red precipitate that separates the palladium from the rhodium, which remains in liquid. But, to my surprise, when I add chlorate, I get a black powder directly, which seems to be palladium. After analysis, it turns out to be palladium, 900 out of 1000.

I notice one thing in this step. It's very difficult to judge the tipping point between the appearance of the precipitate inside the beaker and its disappearance if you add too much chlorate, in my opinion. Meaning, the powder tends to appear and then disappear. To make it reappear, I add ammonium chloride. Let's not forget that to obtain this precipitate, we need to use ammonium chloride beforehand, which is present here because we precipitated the platinum earlier with ammonium chloride. So, we are sure there is enough of it. But when I add chlorate, I don't feel like I'm recovering all the palladium. So, like a fool, I add more chlorate, and the palladium powder tends to disappear again.
Maybe question about pH?
What happens in equation ?
I don't know
I will tcheck cm hook all night I appreciate you're help.

I'm sorry, but I don't have access to photos. However, it seems like you have been facing some challenges in the precipitation process with the palladium. Diluting it in hot water and adding ammonium formate should theoretically yield a black powder, just like with platinum. It's possible that you might have encountered issues with the chlorate or other factors affecting the precipitation. If you continue to face difficulties, you may want to consult with experts or review your procedure to ensure the desired outcome.


It sounds like you have a well-thought-out plan for the final step. Adding formate acetate and a bit of formic acid, and heating strongly should, in theory, allow the rhodium in the solution to transform into a black metallic powder, just like the platinum and palladium. I wish you success in this step of your process!

At one point, I took a small amount after removing the platinum from the solution that contained rhodium and palladium. I still managed to find the balance between adding chlorate and ensuring that the precipitate stays in my solution and doesn't dissolve. I have the impression it's already a palladium metal powder. I tested it with a spectrometer, and it turned out to be 900 out of 1000. I'll try to return to this step in the other solutions and extract palladium this way. I believe a secondary refining step will be necessary for palladium in any case. After recovering the palladium from a small portion of the successful chlorate test, I noticed that the solution has now turned very pink, a truly pink color. I think this is the rhodium remaining in this solution. So, in this small liquid sample, I will use formate acetate, heat it, and see what happens with a bit of added formic acid.

Friends, for those who are ahead of me in CM Hook's book, I'm talking about the platinum group metals allied with gold, etc., and the alternative methods in the last chapters. If you can help clarify the addition of sodium chlorate, whether I can check with pH, color, or quantity, if I can reach the point of precipitation, and how to do it accurately, if someone knows this step and has been working on it for a while, and if someone can tell me why I'm getting this metallic powder instead of the red precipitate I'm trying to obtain. From memory, palladium chlorate ammonium is what I need to extract palladium correctly. Thank you.

If professionnel can HELP ME FOR PLATINIUM GROUPE METAL
THANK YOU THANK YOU THANK YOU

"VINCHÉ From MASSILIA"

 

[Abdoulapapatte]

Certainly, I'll translate your messages from French to English:

"I am in the process of training to become a professional in the field. I need to acquire this knowledge and know how to refine platinum, palladium, and rhodium. I also want to know how professionals do it, and I can get the equipment. It's not a problem, but you need to tell me which path to take and which process to follow. I absolutely need to achieve 999, at least in terms of purity.

The people who entrusted me with the samples are putting a crazy amount of pressure on me. I make very pure money at 4 nines from AgCl with NaOH and sugar. Gold with SMB or FeSO4... Now it's time for me to challenge the platinum group metals. There's no time to wait; we only have one life.

Thank you, thank you, thank you. Don't hesitate to encourage me. It will make me very happy. If you respond to me, please, regarding methods or techniques, make sure you thank you. But please talk to me about things you know like the back of your hand, things you master 100%, that you've already practiced. Thank you."

 

[FrugalRefiner]

Abdoulapapatte, watch your language! I have edited your post to remove all the profanity in both languages. This is your warning. Next time, I will ban you. I don't have time to clean up unnecessary outbursts.

Dave

 

[Abdoulapapatte]

Ôk

 

[Abdoulapapatte]

Hello, I would like to know if anyone has any interesting suggestions or at least tell me if my protocol seems good to you.

Merci

 

[Lou]

I would separate the Pd and Rh from the Pt by hydrolysis. It’s detailed here on forum.

DMG will separate the Pd from the Rh or you could use DETA to precipitate the Rh.

Of course you can also take comfort in the weird quirk of cationic rhodium and separate that from the Pd.


The ammonium hexachloropalladate disappears with the over addition of chlorate (or chlorine) because you are oxidizing away the ammonium cation into NCl3.

Instead, use KCl. The Pd salt is much less soluble than the rhodate.

 

[Abdoulapapatte]

I would separate the Pd and Rh from the Pt by hydrolysis. It’s detailed here on forum.

DMG will separate the Pd from the Rh or you could use DETA to precipitate the Rh.

Of course you can also take comfort in the weird quirk of cationic rhodium and separate that from the Pd.


The ammonium hexachloropalladate disappears with the over addition of chlorate (or chlorine) because you are oxidizing away the ammonium cation into NCl3.

Instead, use KCl. The Pd salt is much less soluble than the rhodate.

Hello Lou and thank you. Where can I find information on hydrolysis to separate Pd from Rh and Pt? Will DMG not cause Pt and Rh to precipitate? Is it better to add it cold? What do you mean by "Of course you can also take comfort in the weird quirk of cationic rhodium and separate that from the Pd"? Instead of NaClO3, do you recommend KCl? Okay, but in my current process, without changing anything or after using DMG? Could you detail the steps of your process? I want to achieve a minimum purity of 999 for the three metals for commercial purposes. Thanks, and I've already written to you in private; I'm glad you're responding here. Thank you very much.

 

[Abdoulapapatte]

and what is DETA "DMG will separate the Pd from the Rh or you could use DETA to precipitate the Rh."

 

[andu]

This dude seems to have it got right, i'm no expert but here it is.

There's a second vid you'll want to watch too.

 

[Abdoulapapatte]

Hello I see this guy's but I think he shoes the wrong way