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Thanks for sharing your process sounds like you're working really hard on this! It looks like you're following most steps right, but the green color could mean there are other metals like copper or nickel still in the solution. That might be why your results look different than expected. Also, the pH level (how acidic or basic your solution is) can change how things react, especially when using ammonium chloride. If you're doing this as part of a project or research, getting help from a dissertation tutor in Sheffield could make things easier and help you fix any mistakes. You're doing great just keep testing and be careful!

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If you add nitric acid you can not easily precipitate Palladium use hydrogen peroxide instead of nitric acid

Thanks

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Nikel tuzu gibi görünüyor.Sam daha iyi bilir.klor gazı fokurdayınca PDCl2 solüsyonundan kırmızı PD tuzu düşer.sizin yeşil düşmüş!

Hi again. I succesfully precipitated everything from the solution. But I think I have nickel and copper in the precipitate. How can I remove them from the palladium?

Hi @Sam. I am processing another palladium solution. The stannous chloride is very positive it turns dark when I add 1 drop pd solution and 3 drops sncl2. The colour of the solution is green. When I add more HCl to neutralize the HNO3 the solution turn very dark green. I let it cool down from the hot plate and I added a spoon of zinc powder then the solution start fizzing very much and a blueish foam appears and brown gases releases. I do not know why. I decided to add aluminium foil and the same thing happens and nothing precipitates. I put the solution on a hot plate and the blue foam dissappeared and the solutiom got lighter. When I added HCl it got again dark green. I think it did not neutralized enough and if how to neutralize it completly? Should I use urea powder? And when I neutralize it what should I do to get the dark pgm powder as described in this site? I hope you will help me. Thank you in advance.

Hi @Sam. Three days ago I started processing gold so I got gold fingers from RAMs and I put them in nitric acid. The gold platings started seperating from the fingers and the soloution turned blue-green color. I decides to test it with stannous chloride and it got strong positive for palladium. So how should I process the liquid after filtering it?Should I precipitate with zinc powder or I should do something else? Thank you!

Hi @Sam if you want I will give you my number to contact better in viber or whatsapp if you want?

Your test seems very dilute... Borderline negative. See here wht an SnCl2 looks like with a 1g/L palladium control solution.

Hi @Sam. Today I filtered the precipitate and I put ammonia soloution then I added HCl and I put the soloution on a hot plate to evapurate the liquid. Then it evapurated and a yellow powder settled on the bottom. I am thinking of making the refining process again ( dissolve in AR then neutralizing, precipitating with ammonium chloride, precipitating with chlorine etc) or to calcine the powder as described in this site?

This is the yellow precipitate which formed

This is the sncl2 test

This picture is after the neutralization

What it is then and how to fix it?

Hi @Sam. I wanted to tell you what is happening with the process. So I neutralized the pd soloution on a hot plate by adding HCl. After that I let it for a night and today I made saturated ammonium chloride soloution and I added it to the soloution. I filtered it and after that I bubbled chlorine gas into the soloution and a precipitate started to form and I let it for a night now. Is everything as it should be?

This is the precipitate after the chlorine bubbling

@Sam

Hi @Sam Copper...? Hm... Yes the test is green yellow color when I put it on a paper. When I put a sample of the pd soloution on a spoon and when I add the sncl2 a dark color forms then it is gone. And no I do not have DMG. Maybe there is copper and pd?

Hi @Sam Copper...? Hm... Yes the test is green yellow color when I put it on a paper. When I put a sample of the pd soloution on a spoon and when I add the sncl2 a dark color forms then it is gone. And no I do not have DMG. Maybe there is copper and pd?

@Sam please answer

@Sam

Hi @Sam I am writting to tell you about the process I told you earlier. So I got the zinc precipitate it was dark (brick) red. I washed it with HCl and water. Then I put it in another beaker and I put HCl and I put the beaker on a hot plate. Then I started adding HNO3 in small increments until the precipitate dissolved. The soloution was yellowish but when it cooled down it turned light green. Then I put the beaker in cold water for a night and I am waiting now. Is everything as it should be? Am I doing something wrong? Oh and I made a stannous chloride test for the dissolved precipitate and it was positive (as it should be).

This picture is when the precipitate soloution cooled down.

This is when it was on a hot plate.

These two are the precipitate.

@Sam

Hi @Sam I am writting to tell you that I am doing a second batch but first I am doing the recovery process after that I will do the refining. So I put the material on a hot plate and I added calculated ammount of HCl and heated it for 1-2 hours. I let it settle for a day after that I added tap water and let it settle again. After that I made stannous chloride test and it was negative (as it shoyld be) so I put the beaker again on a hot plate and I added a calculated amount of HCl and 3% H2O2 and added little additions of HNO3 until the material dissolved and the stannous chloride was positive. The solotion was deep green color. I let it settle again and the next day I added a little bit of zinc powder to settle the pd dark powder. When I started adding the solotion turned from deep green, to light blue and some precipitate was formed. I mad pd test and it was negative. And now it it settling for a day. Am I doing everything correctly?

These pictures are from the zinc settling and the blue color

Maybe.. But very hard to say, just by looking at it.

@Sam can you answer me

Dilute... 10-15% It will not precipitate, hopefully it in alreadny in metallic state and simply will not dissolve by the dilute acid.

Very likely Nickel oxide. How hot did it get? If you got it hot enough to completely decompose and calcine the Pd salt, then, a dilute HCl will dissolve the nickel salt, leaving you with only Pd powder.

In that case, try one more roung of leaching the source material.

Thanks but I think that i have good amount of palladium and i think my problem i caused because i did not made the recovery process before the refining process. What do you think?

I would suggest trying to work onky with MLCC at first and get to know more about the work with Palladium.

Thing is...

The instructions in the tutorials relates to higher Pd concentration with few other metals present.

The amount of Palladium (and other PM) in such materials as you mention is so so small and the amount of other elements is svery high. A begginer (and even the experienced) would have a hard time seperating them or even understand what's going on.

Hi Rem,

There's a lot of missing information...

What was the starting material?

Are you sure it contains Palladium? How much?

What other metals does it contains (soudns like Ni is present)?