I did almost all steps from this website about palladium precipitation. I added HCl to my material of palladium on a hot plate and started adding nitric acid slowly. The soloution started getting green. When the material dissolved i cooled it for a day and i started heating it again and added additions of HCl and the mixture got dark green. I made bunch of Stannous chloride tests and i think that it is positive for palladium because the colour was yellow green. When i neutralized the soloution i let it for one more day. After that a blue- green crystals were formed so i filtered them. After that I made a concentrated soloution of amonium chloride and I added it to my palladium soloution. Some precipitate was formed so i filtered it. But the precipitate was not yellow or orange. Later I make a mixture of manganese oxide and HCl to produce chlorine. I introduced the chlorine to the green mixture of palladium and then some white green precipitate was formed. My question is am I doing everything correctly and why my soloution is green and if it is wronge how can i fix it.
Dilute... 10-15% It will not precipitate, hopefully it in alreadny in metallic state and simply will not dissolve by the dilute acid.
@Sam Thank you very much I appreciate your help. I will now do a second batch but before the refining procces I am doing the recovery procces discribed in your article I think the pd will be more pure this way.
Do you mind showing us the starting material?
@Sam It is from old rotate phone scrap.
This is one out of many
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)?
Hi Sam,
I use some old phone material for test and I am sure that there is Palladium but i dont know how much. I think there is platinium and nickel or copper i think. I made a concentrated ammonium chloride soloution and some precipitate was settled. Then I made chlorine gas by mixing manganese oxide and HCl and I bubbled it in the Pd soloution and a precipitate was settled. Then I filtered the precipitate and I put ammonia and the soloution became dark blue and I poured HCl and the mixture became transperent and after some time a little bit precipitate was formed but i do not know is that what should i get and why the whole proces the soloution was green-blue and what to do. Thanks :)
@Sam Hi Sam sorry for bothering you but I would want to ask you a question about gold scrap. What type of ram ia better for gold refining and contains more gold PC rams or laptop rams? Thank you
As far as i know, the gild content is somewhat similar
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.
@Sam
I would suggest trying to work onky with MLCC at first and get to know more about the work with Palladium.
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.
@Sam So when i put HCl the pd salt will precipitate on the botton? And how dilute should the HCl be?
@Sam can you answer me
Maybe.. But very hard to say, just by looking at it.
@Sam i will do the dilure hydrochloric acid and will see what will happen. Can you tell me does the type of capacitors differ for palladium or every type has palladium.
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
Looks good. Wash the powder with boiling hot water 2-3 times and then 2-3 time with dilute HCl (don't forget to test those wash with stannous chloride), again one more time with hot water. Proceed to refining the black palladium powder.
@Sam Thank you. And do you know how many (average) rams do I need to produce good amount of gold?
@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.
The precipitate look like copper... So a the solution.... Is the solution positive for Pd? Do you have DMG?
@Sam Copper...? Hm... Yes the test is green yellow color when I put it on a paper. When I put a sample on a spoon 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
@Sam please answer
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
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
No... The precipitate should be dark bright red... Yours seems white.
What it is then and how to fix it?
Honestly, i think there's a chance that there isn't any Pd... or that the amount is very very small. You should rrally get some DMG, as it is very sensitive and will quantitatively drop Pd.
This is the sncl2 test
This picture is after the neutralization
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
Your test seems very dilute... Borderline negative. See here wht an SnCl2 looks like with a 1g/L palladium control solution.