DMG and unknown Pd amount

[Barren Realms 007]

Lou it's British humour, I know you know more than I ever will and your scope of knowledge is staggering, do I have to kiss butt all the time :shock:

No, just most of the time.

 

[kjavanb123]

Hi Lou,

Thanks a lot for your info. My nitrate solution does not contain any gold, only copper and palladium. Do you know if they ship to UAE? And what is the minimum quantity I can order?

Regards
Kj

 

[Lou]

Do not know those details. I can get you a contact if you're serious. They have installs in Africa so I don't see why not.

 

[kjavanb123]

Lou,

Please kindly advise the person I should contact regarding purchasing and shipping. My solutions keep growing and zinc cementing or DMG is pain filtering the canary yellow powder.

Regards
Kj

 

[Lou]

Send me PM.

Thanks

 

[mls26cwru]

do you know how much Pd you ended up getting from the whole batch?

 

[kjavanb123]

Hi,

I recovered 84g of Palladium sponge from all those batches.

 

[kjavanb123]

Hi

I just did some experiment which relates to usage of DMG hence I added to this old thread.

I smelted a mix of solders and SMDs from small socket PC boards, using lead oxide.

The produced lead dore was cupeled in Portland cement hearth, and it produced 30 grams of copper beads and some small amount of lead as the cupelation was not completed due to lack of fuel.

The result copper and lead were dissolved in warm dilute nitric acid, copper nitrate solution was filtered from lead sulfate which I already precipitated using sulfuric acid,


Addition of HCL to the copper nitrate solution did not produce any silver chlroide.

A DMG solution was prepared by adding 4 grams of lye to 100ml hot distillled water and to that 5.35 g of DMG was added and stirred.

Upon filtering and adding the DMG soltion the following turned to green color precipitatant


Both of these tests indicates I couldn't recover the Pd or Ag from mix of solders and SMD during smelting.

 

[FrugalRefiner]

Upon filtering and adding the DMG soltion the following turned to green color precipitatant

The green color could be due to a combination of the yellow palladium glyoxime precipitate and the blue from the copper nitrate. Have you tried filtering out the precipitate and washing to remove the copper nitrate solution?

Dave

 

[Yggdrasil]

Hi Kjavanb
How did it go with the original solution?
Did you ever get to try out Superlig?

 

[kjavanb123]

Upon filtering and adding the DMG soltion the following turned to green color precipitatant

The green color could be due to a combination of the yellow palladium glyoxime precipitate and the blue from the copper nitrate. Have you tried filtering out the precipitate and washing to remove the copper nitrate solution?

Hi Dave

Thanks for your comment. I am filtering and washing it right now and green powder turned into very pale yellow not the canary I expected.

Dave

 

[kjavanb123]

Hi Kjavanb
How did it go with the original solution?
Did you ever get to try out Superlig?

Hi

No I never tried that as I did recover palladium from my batch using DMG.

Best regards
KJ

 

[kjavanb123]

Here is the filtered light yellow powder,


Rinsed that to a glass jar, as it can be seen below,


Sprinkled a tablespoon of zinc powder and mixed it well with light yellow Pd powder,


To that 20ml of dilute hcl acid added and swirled the jar so the light yellow is nixed with zinc ans hcl, this is what was left.


I left it until tommorow, so the hcl left over there dissolve zinc powder and will check for black powder tommorow.

Thanks and best regards
KJ

 

[kjavanb123]

Hi

Finally recovered 0.22 grams of black Pd powder from the solution and very pale Pd dimo powder.


So if addition of DMG solution to Pd nitrate solution didn't turn canary yellow, just filter ans wash the bulky powder and cement with zinc.

Best regards
Kj

 

[rickzeien]

Hi

Finally recovered 0.22 grams of black Pd powder from the solution and very pale Pd dimo powder.


So if addition of DMG solution to Pd nitrate solution didn't turn canary yellow, just filter ans wash the bulky powder and cement with zinc.

Best regards
Kj

How was the PD nitrate solution obtained from the circuit board smelting? Thanks

Sent from my LG-H872 using Tapatalk

 

[kjavanb123]

Hi

Finally recovered 0.22 grams of black Pd powder from the solution and very pale Pd dimo powder.
image.jpg

So if addition of DMG solution to Pd nitrate solution didn't turn canary yellow, just filter ans wash the bulky powder and cement with zinc.

Best regards
Kj

How was the PD nitrate solution obtained from the circuit board smelting? Thanks

Sent from my LG-H872 using Tapatalk

Hi

After depopulation, all SMD components were mixed up with molten solders.

So I collected and sieved that mix from rest of components, then melted them into a solder dore.

At first I tried dissolving that dore bar in warm hcl then dilute sulfuric acid and both seems very slow.

I smelted the solder dore bar with 300 grams of lead oxide and same amount of flux as there were some plastics and small ICs in the mix.

Cupeled the lead dore and got 30 grams of impure copper shots.

So this Pd is from SMD components (include capacitors, and other small components) and solders.

Best regards
KJ

 

[rickzeien]

Thanks

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[DylanCaldwell]

Some other factors you may find useful.

Platinum dropped with ammonium chloride (NH4)2(PtCl6) factor 0.4395

Palladium dropped with sodium chlorate Cl4H8N2Pd factor 0.37431

Would rhodium also drop from solution in this case after the addition of ammonium chloride and cl2 gas from sodium chlorate?

 

[MapishPepperush]

All,

I have a palladium nitrate solution that the amount of palladium per liter is unknown. Can DMG method be used to find out how much Pd I have in it?

Freechemist (R.I.P) mentioned 2.5g DMG will drop 1 gram of Pd. So if I take 500ml of Pd nitrate solution, and make DMG solution by dissolving 2.5g DMG dissolved in 100ml of water, and add it to 500ml Pd nitrate solution, filter the canary yellow, incinerate it then melt it to find out how much Pd was in 500ml solution to calculate gram per liter for Pd?

Best regards
Kj

I don't recommend to use the calcinate method you will definitely lose some material, try to redissolve the DMG/pd in nitric acid then boil the solution to evaporate the nitric and rehydrated with HCl , now your solution is free of nitric you can check if trace of platinum is present by adding small amount of ammonia chloride dissolved in water and after start bubbling chlorine gas to get reddish pink precipitate wich is palladium salt, filter this salt and dissolve in ammonia , filter the ammonia solution and add HCl acid to precipitate a yellow white salt wich is pure palladium salt, filter this salt and suspend in small amount of water and heat ,when is start to boil just add little formic acid and stir when you will see a black colour in palladium salt suspension you can start adding little by little formic acid until you will get a clear solution and a nice black palladium, wash this palladium with water and melt you will get 999 palladium ,
You can use DMG just mixed with hot water to drop palladium and ATENTION is not necessary all dmg to be dissolved in water to drop pd you must just add all undissolved DMG with water to main solution stiring and all pd ions will precipitate
I don't recommend to try dissolving DMG with Noah because if is nickel in solution will react making a pink nickel salt(adjusting ph and etc. is a waste of time is more easy to add just hotcwater mixed with DMG powder to main solution to drop all pd)

 

[Yggdrasil]

I don't recommend to use the calcinate method you will definitely lose some material, try to redissolve the DMG/pd in nitric acid then boil the solution to evaporate the nitric and rehydrated with HCl , now your solution is free of nitric you can check if trace of platinum is present by adding small amount of ammonia chloride dissolved in water and after start bubbling chlorine gas to get reddish pink precipitate wich is palladium salt, filter this salt and dissolve in ammonia , filter the ammonia solution and add HCl acid to precipitate a yellow white salt wich is pure palladium salt, filter this salt and suspend in small amount of water and heat ,when is start to boil just add little formic acid and stir when you will see a black colour in palladium salt suspension you can start adding little by little formic acid until you will get a clear solution and a nice black palladium, wash this palladium with water and melt you will get 999 palladium ,
You can use DMG just mixed with hot water to drop palladium and ATENTION is not necessary all dmg to be dissolved in water to drop pd you must just add all undissolved DMG with water to main solution stiring and all pd ions will precipitate
I don't recommend to try dissolving DMG with Noah because if is nickel in solution will react making a pink nickel salt(adjusting ph and etc. is a waste of time is more easy to add just hotcwater mixed with DMG powder to main solution to drop all pd)

Calcining is perfectly safe if you make sure it is not overheating.
Formate reduction is also perfectly safe.