Pd purifying in pictures

[Lou]

@freechemist,

Very good! Nice to see another chemist on the board. Welcome, please stay!

What he has made is Vauquelin's salt, which as you said is the palladium analog of Magnus's green salt--he did not use enough ammonia. I find that one can add 1.2X the amount of concentrated ammonia water at room temperature, stir very well, and then heat well (80*C) to drive off some of the ammonia. It is important to make sure that some still remains and that it is basic to litmus. Then one may acidify and get the familiar yellow trans-PdCl3(NH3)3].

Cheers,

Lou

 

[61 silverman]

Lou, I just now ( reading this post ) learned why my most recent Pd button had a darkish sheen to it after melting the first time , without quenching.. I melted with a oxy- propane set-up. Just read the Pd more than likely absorbed some of the propane gas .. melting a second time then quenching in cold water left a very light ash like, substance floating on top of the water. and the button has more shine to it.. Can the quenching at the right time improve the button's appearance or purity by blocking the carbon absorbtion.

 

[HAuCl4]

Can you post a large version of your gold micky avatar?. It's just too cool.

 

[Barren Realms 007]

Can you post a large version of your gold micky avatar?. It's just too cool.

He has before search his post's.

 

[lazersteve]

What was the source material of the Pd Mark?

Nice work on the button.

Steve

 

[Palladium]

Can you post a large version of your gold micky avatar?. It's just too cool.

http://goldrefiningforum.com/phpBB3/viewtopic.php?f=60&t=983&hilit=Watch+bands

 

[61 silverman]

Steve; I'm sorry It seem that every time I need too respond to a question from you too me, I don't get too it... MY APPOLAGIES.. Now to finally answer your question. The palladium button pictured is more of the palladium I had recovered from Dental scrap, I have melted two sepperate buttons , before I read that it isnot wise too melt it unles a hydrogen torch is used.. I did not have really any trouble at melting either these buttons or the Platinium button I pictured in an earlier post ( incinerated colore powder ) all in total to this point I have recovered 95.5 grams of twice re-refined gold, 2 melted buttons of palladium weighing 6.7 grams also 36 grams of reduced Pd powder ( zinc reduction ) I had weighed 3.0 grams of the powder to do a test melt return weighed 2.8 to 2.9 grams i feel it is 2.85 , that is a 5% loss compared too a 3% expected.. There is also 2 buttons of Platinium One of them has too be refined again converted powder was not clean ; dummy melted it DUH!! the amount of Pt. so far is close to 8grams.. this batch of dental scrap had 89grams of yellow crowns and such items with 158 grams of white and off white material.. I know I have not recovered all the values, I have an Embarassing amount of stock pot material too process.. say 1 1/2 cups of settled material rinsed clear . I used a combination of copper wire - yes SLOW - as time went on I started using zinc, worked out a system of removing the copper from the blacks , it was basically cemented from a earlier solution w/zinc, finely divided,approaching the end of the material my slightly pregnant solutions incompled precipitations, started going staight to the stock pot essentially removing the available copper too cement pgm's and possibly Au, My collection of blacks are truly that BLACK.. I will post a picture when I transfer to process,View attachment 2 I will have too add the results from my stock pot in the future, The dentist I refined this material from truly expect very little in return.. Not free but not far from it. Unbelievable . :shock: 8) :mrgreen: Mark

 

[kroutonz]

Are you sure thats only .2 grams of pd? I incinerated my material recently it looks just like that but is significantly smaller in amount and weights 2 grams.. Just curious.

 

[61 silverman]

Are you sure thats only .2 grams of pd? I incinerated my material recently it looks just like that but is significantly smaller in amount and weights 2 grams.. Just curious.

If you look again you will see the palladium button is 2.8 grams not .2 grams.. started (in that melt as a purity evaluation ) 3 grams of Pd powder. Some very small BB's were left from blow away that is un-weighed.. I will know soon what the purity of that button along with 38 more grams is.. Mark

 

[kroutonz]

Sorry, I was referring to kjavanb123, the original poster. Just seems like a decent amount of powder for only .2g that the jewelers said.

 

[kjavanb123]

Sorry, I was referring to kjavanb123, the original poster. Just seems like a decent amount of powder for only .2g that the jewelers said.

well, i combined the metallic Pd from this post with some other Pd i produced from processing 9 combs, after melting it weighed only 0.68grams. you can see a pic of it below.


My mistake was in temp of solution during Pd percipitation. I think it was too hot so when i added ammonium chloride solution to it, i had a spilliage and lost most of the solution. For my future project i am gonna use a vase between my beakers and the heat source.

 

[kroutonz]

Ah, nice. I thought it seemed a little more than .2. In my 2 pd precipitations(lol) i've found that temperature doesn't matter atleast for pd. I also had no boiling/foaming whatsoever with the addition of the sodium chlorate/ammonium to cold solution. However it may be a different matter when its concentrated more.

 

[Inter Refiner]

The pink residue on the filter shown in your picture series is the result of an incomplete reaction of your palladium salt with ammonia. It's chemical composition is the same as that of the yellow diamminepalladium(II)chloride, but it's structure is very different. The rose precipitate actually is a double salt, built up from [Pd(NH3)4]2+ cations and [PdCl4]2- anions, which is only very sparingly soluble in water. An analogous compound in platinum chemistry is the well known green Magnus salt.

Hello friends,
I am processing some cats that contain pt, pd, rh. the process is leaching in aqua regia- cementing with zinc or ammonium formate- redissolving pgm black in hcl/h2o2- precipitating platinum with ammonium chloride- precipitating mixed palladium and rhodium salts by bubbling chlorine gas through the solution- I get a brown sponge of mixed pd and rh salts- dissolve pd salt in ammonia and get the insoluble rhodium salt. every thing went well till the last step of ammonia, I have a pink precipitate that I didn't know if it was rhodium salt or undissolved palladium. the pink salt is extremely insoluble in anything that I tried, please help me with knpowing what that is and how to get my rhodium for next times and this time, and how to avoid forming this pink salt, how much ammonia is needed to dissolve the brown pd salt.

thank you very much

 

[kjavanb123]

Hi

Ammonia should be added and stir the solution, you should do this till all pink residue dissolved, if not then filter the clear solution add hcl the yellow Pd salt will percipitate.

 

[Inter Refiner]

I did all of that but the pink precipitate still refuses to dissolve, I recovered palladium from ammonia but the pink residue is still there


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[kjavanb123]

If my memory is correct that pink residue is either a compound of Palladium or impurity.
I guess Lou can elaborate on that.

 

[Inter Refiner]

The pink residue is hard to dissolve in aqua regia and in hcl/h2o2 and hcl/bleach


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[Lou]

Pink residue (more mauve I guess) is vauquelin’s salt. Needs more ammonia then dissolves to colorless terammine Pd complex.

 

[Lou]

https://www.technology.matthey.com/article/20/1/21-24/

It is binuclear complex.

 

[Inter Refiner]

thank you lou,
I would like to ask you some questions about rhodium,
after precipitating platinum with nh4cl will rhodium precipitate with palladium by bubbling chlorine to the solution?
what would be a proper test for rhodium?

I am asking because I have very minimal info about refining rhodium and I need to get familiar with it to process cats

appreciate any help
thanks in advance