# is that could be palladium powder ?



## bastinado (Dec 24, 2016)

is that could be the color of palladium powder or it should be more gray than this white?


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## FrugalRefiner (Dec 24, 2016)

It might help to know a little more.

What was the original material?
How did you process it?
How did you precipitate it?

Any details you add will help members to answer your questions.

Dave


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## bastinado (Dec 24, 2016)

FrugalRefiner said:


> It might help to know a little more.
> 
> What was the original material?
> How did you process it?
> ...


 MLCC's

HCl + H2O2 

precipate with copper ( Few black layer on th copper ) 

i left the remain solution for several days then i found this as white to gray precipitate and it become as per photo after drying

i suppose that palladium chloride have been decomposed over time is that possible?


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## nickvc (Dec 25, 2016)

It looks more like cemented silver to me, dissolve a small sample in nitric and test for any Pd using stannous, palladium will be the last to cement out so test your original solution too.


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## bastinado (Dec 25, 2016)

nickvc said:


> It looks more like cemented silver to me, dissolve a small sample in nitric and test for any Pd using stannous, palladium will be the last to cement out so test your original solution too.



id didn't use nitric acid to dissolve silver i used Hcl with h2o2 only so there is non solvent silver chloride and i already filtered my solution very well before the precipitation 

when i redissolve the powder it take very long time with (hcl + h2o2 ) and the solution color is yellow to orange 

i cant get nitric acid in my country 

i ll try to made some sttanos chloride to test but the powder well take very very long time to re dissolved completely 

i have had look under microscope i didn't see any crystals 

i added NH4cl to check if this is Cucl but there was no reaction


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## Lino1406 (Jan 2, 2017)

Palladium chloride does not decompose. Did you make NH4Cl alkaline?


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## bastinado (Jan 2, 2017)

no nh4cl i added to the precipitated powder not the solution 

but i have add some hcl with non ionic surfactant , i think that is the reason for precipitating the palladium if this is palladium

there is some of reductive compounds i have added without intention , which have make this powder and not the copper


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## bastinado (Jan 2, 2017)

now after days i think i have understand what is the reasons for diffrant palladium precipate colors

some time white ( this should be hte normal ) 

some time gray ( white with some black palladium oxide ) 

some time canary yellow ( white with yellow stain from the yellow color of pure palladium chloride solution )

some time red ( white wit red stain from either mix of palladium and other metals solution )


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## Lino1406 (Jan 3, 2017)

The 100% palladium is black. I recommend Dimethylglioxime for identification. 
Also making NH4Cl alkaline will identify copper by blue hue


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## bastinado (Jan 3, 2017)

i see

Black but when u get from Nitric acid solution i mean palladium nitrate so during precipitation palladium is going to be oxidized so it become black

when my solution is chloride and all of H2O2 have broken to water so there is no oxidizer and palladium is pure white metal

Nh4cl have not make any reaction with my powder 

also concentrated KOH have now reaction

last taste i tried to melt with propane gas and it have turned into gray without any melting ( if this was silver it should be melted )


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## g_axelsson (Jan 3, 2017)

A few short questions.
- How much MLCC:s did you start with?
- What is the weight of the gray powder?
- Have you saved the solids?

This doesn't look at all like palladium powder to me and I have always cemented the palladium from chloride solutions.

Göran


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## Topher_osAUrus (Jan 3, 2017)

Lou had a post with a pic showing gray palladium powder, but it was the formate method, not cementing.


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## bastinado (Jan 3, 2017)

Göran

are you cementing with copper ? or other method ?

some of my palladium which was on the surface of copper plate was black

but the other which have precipitated with kind of non ionic surfactant 

i have had around 4 kg of mlcc 

the total amount of this powder which i have tell now is around 50 grams and i still precipitate some extra

the solution in the begging is red or brown and after precipitation it become dark green and some extra powder fall then it become normal green


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## bastinado (Jan 3, 2017)

some thing important i remind to mention

this color of powder is after washing without washing the powder is yellow


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## g_axelsson (Jan 3, 2017)

I cemented with zinc.
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=51&t=18564

The resulting powder after drying.



I have also tested cementing solution from MLCC:s on copper wire:



Did you test your washing solution with stannous?

You could easily test the dissolved powder with stannous to see if it is palladium.

Göran


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## bastinado (Jan 3, 2017)

this powder is palladium oxide (black)

i don't have pure tin to made stannous 

i have take some of my solution and precipitate with aluminum foil i have black powder but may include other metals


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## bastinado (Jan 3, 2017)

i have put my powder under propane or boutan (i dont know exactly ) flame and it turns to gray

i put the gray powder in hcl to remove some borax i have added i found the powder in the solution black also

i ll re dry it and put the photo after drying


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## Topher_osAUrus (Jan 3, 2017)

g_axelsson said:


> You could easily test the dissolved powder with stannous to see if it is palladium.
> 
> Göran



...that would be easy, almost *too* easy..



bastinado said:


> i don't have pure tin to made stannous



You don't need pure tin, some fellows on the board even just use pewter dissolved in HCl. Or solder.


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## Platdigger (Jan 3, 2017)

What is this " kind of non ionic surfactant" you keep mentioning?
Also what are these? "there is some of reductive compounds i have added without intention"
And, what did you rinse the yellow powder with?


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## bastinado (Jan 3, 2017)

i dont know what exactly but my Hcl was not pure it have had non ionic surfactant , it may be ploy Etheline glycol or another type

here is the photo of the same sample powder the gray one was white and i opened flame on it it turn to this gray 

then i wash it with hcl and water and re dry it it become gray du to the effect of the oxdizer flame

and that confirm my theory the palladium powder is originally white and the gray color is comong from some of palladium oxide

if it 100 % palladium oxide id become totally black

now is in the lower is color of palladium powder ?

if it is so this is the white one and it is also palladium


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## bastinado (Jan 3, 2017)

am preparing stannous and when it complete i ll inform u the test result


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## Platdigger (Jan 3, 2017)

You need your metal in solution to test with stanus.


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## Thetodor (Jan 5, 2017)

From my experience, this looks like (NH3)2Cl2PdCl2, diamminedichloropalladium(ii) chloride. The appearance is described as: "(Color) Faint Yellow to Yellow and Yellow-Green" 
It is sparingly soluble and precipitated with the addition of HCl to your previous solution of Pd(NH3)4Cl2, tetraamminepalladium(ii) chloride.

Depending on the series of reactions some people get a dark brown solution of (NH4)2PdCl4 ammonium tetrachloropalladate(ii), this is characteristc of tetrachloropalladic(ii) acid. Even further oxidation gives hexachloropalladic(iv) acid. With ammonium chloride it precipitates a red (NH4)2PdCl6, diammine hexachloropalladate(iv). I have not been able to get this one... possibly due to adding too much ammonium chloride very early on. 

I say, seperate it from the silver chloride, there's bound to be some.. after precipitating, try dissolving in only nitric acid, then add very little hcl or salt to the clear solution. adding too much Cl- will re-disolve some silver as AgCl2- ion


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## Lino1406 (Jan 5, 2017)

Sorry, the conditions for getting that diamine were not existing


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## bastinado (Jan 6, 2017)

I didnot add Nh4CL to my solution to have this compound 

90 % probability that my powder is pure palladium with no palladium oxide

when there is mixture of pure palladium and palladium oxide the powder is gray , and if the powder is 100 % palladium oxide it become totally black

this is my deduction 

if i found place to melt my powder and have as alloy i ll check by xray and no exactly what is and i intend to inform you


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## bastinado (Feb 1, 2017)

this is the powder after melting with oxyacetylene

it is black as per this image 

so what could be this powder ? is that palladium ?


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## Lino1406 (Feb 1, 2017)

Could be since palladium on cooling back from 1545C at 1000C the oxide becomes stable. Returning backwards: Take a sample, dissolve and check with DMG


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## Platdigger (Feb 2, 2017)

Are you sure this is not silver chloride somehow? You said there was some black pd that cemented to the copper, and then later this powder appeared. Have you tried to dissolve a small sample of the powder with ammonia?


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## g_axelsson (Feb 2, 2017)

So, what did stannous testing give?

It still doesn't look like palladium to me, more like a slag. For example tin oxides could be created when working with MLCC:s and tin(IV) oxide melts at slightly higher temperature than palladium. Silver chloride is also a possibility.

When you melt a metal in a melting dish it has a very different appearance compared to slags. It should have been obvious if you had a metal or other metal salts creating slag.

Testing is always more reliable than deduction.

Göran


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## bastinado (Feb 2, 2017)

there was no reaction with ammonium chloride 

my solution was filtered so it is free of any insoluble silver chloride

i assume the black is metal because i know palladium well be mixed with carbon which is main component of acetylene and also it well be oxidized so it may looks black 

the was no borax during melting trial 

i failed to make stannous i started weeks ago ad i still see my tin wire in the solution


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## Topher_osAUrus (Feb 2, 2017)

...maybe it's just me

But, if I couldn't even make stannous chloride, I sure wouldn't be trying to melt some unknown powder I "think" is palladium.


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## bastinado (Feb 2, 2017)

Melting is not at my house 

i went to jewelery workshop for melting ( they only work in silver and gold ) they don't have induction furences melt over than 1200 c , they don't have even oxy hydrogen because acetylene is enough 

for me melting palladium is problem rather than selling , 

my Hcl is less than 30 % concentration 

i know how to make stannous the problem is in the low concentration and the rusted or un pure tin , and even if i use stannous it well confirm there is palladium , and am sure there is palladium and some thing impossible to dissolve high grade MLCC and there is no palladium in

what i want to know is this palladium by meaning th most of powder is palladium or it might be palladium with other metals ? 

i do all chemical tests which confirm this powder have no tin , no copper , no copper mono-chloride 

and it is impossible to have silver chloride because i already remover it during filtration of my red solution as powder 

so what would be remain is one of the precocious metals which are used in MLCC it is not nickel and not copper and not tin and not silver , so it is either Palladium or platinum or ruthenium


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## mls26cwru (Feb 2, 2017)

To be blunt... Stop guessing at what you have! Either do the tests that the members here have suggested, or take it and have someone professionally analyze it....you are going to get the cold shoulder if you continue to ignore the advice that has been given to you.


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## bastinado (Feb 2, 2017)

ok 

thanks for all members who have give an advice 

i see no one have expertise such as this powder looking or this black color after acetylene melting but many thanks

i have not ignore any advice , DMG is not available for me , Stannous Chloride result is negative or i failed to prepare it ( may be the low HCL concentration or the bad oxidized tin )

i cant imagine Hi grade MLCC from servers and telecom boards and photo copiers have no palladium 

physically and chemically the powder is not salt or tin or tin oxide 

chemically it is impossible to be silver or silver chloride 

chemically it is impossible to be zirconium or zirconium oxide 

what am sure 100 % this powder is Either precious metal but not silver or acid resistible oxide for metal i don't know but it have been used to make ceramic material in the MLCC


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## Lino1406 (Feb 3, 2017)

Sorry I forgot to point out that if you rub the black oxide, as mentioned,
a white metal appears below - if it is palladium


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## patnor1011 (Feb 3, 2017)

Bastinado your HCl is as strong as it gets. HCl does not come stronger than what you have. I do not understand how you can fail doing basic easy thing like preparing stannous yet you think you are processing palladium. 
For stannous all you need is to heat your HCl and tin will dissolve with ease. 

There is plenty of DMG for sale on ebay and if you want to work with palladium you cant cut corners and play guessing game. You either do have palladium there or not. Get yourself some DMG and find out.
http://www.ebay.com/sch/i.html?_from=R40&_trksid=p2050601.m570.l1311.R1.TR1.TRC0.A0.H1.Xdimethylglyoxime.TRS0&_nkw=dimethylglyoxime&_sacat=0


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## Thetodor (Feb 3, 2017)

Your not reacting the black metal with the stannous chloride, right? You need to react the solution made from the black metal (after it is dissolved in aqua regia or nitric acid) with stannous chloride in solution or solid form


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