# Pd purifying in pictures



## kjavanb123 (Jan 27, 2011)

All,

Thanks to Steve and other helpful members here I finally got my first Pd salt from the Pd solution, it feels soo awesome after so many failed tries. Here are some photos of cleaning up the Pd salt. I got this pink residue though. what could it be?

Here is the photo of




After adding AR to the black powder following.



After adding ammonium chloride saturated to the below boiling Pd solution a strange dark gray foam formed on top surface?



Dropping the Pd with sodium



Adding ammonia to the Pd salt from previous part. 



Now could this pinkish residue be sister PGMs?

Thanks
Kev


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## lazersteve (Jan 27, 2011)

The salmon colored residue still could be undissolved Pd salts. Add some more NH4OH and stir to see if any more of it dissolves. If not, you'll want to separate it out with a vacuum filter and do more tests on it.

The solution should have your Pd in it, simply add HCl to convert the Pd dissolved in the liquid to the nice canary yellow powder with your Pd in it.

The gray is probably from the solution being overheated and dehydrated and/or decomposed. Next time don't evaporate so far down.

Looks like you are finally on the right track now.

Steve


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## kjavanb123 (Jan 28, 2011)

Steve,

Thanks for your help. I haven't gone back to the lap yet, but would heating the pinkish ammonia solution help Pd dissolve faster?

Thanks
Kev


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## Lou (Jan 29, 2011)

Kev,

Aqueous ammonia is a gas in solution. Heating ammonia will actually drive off aqueous ammonia and make it less efficient and less effective. Recall that hot soda pop will go flat much quicker than a cold pop--gases always have more solubility in a cold solution because there is less molecular motion to kick out gas molecules.


Lou


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## kjavanb123 (Jan 29, 2011)

Steve, Lou

Thanks a bunch for ur support through here. This is what I did to finally produced the canary colored Pd salt. :lol: 


Clear solution with tinted yellow containing the Pd and ammonia



Added muratic acid to the above solution and..



Filtered canary Pd salt to be incinerated



Filtering the undissolved pink residue in ammonia



That pink residue from above is being dissolved in AR while being heated.



well now i am gonna go ahead and heat the canary Pd salts in quartz dish.


Thanks
Kev


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## lazersteve (Jan 29, 2011)

What does a stannous chloride and DMG test show for the AR liquid used in the extraction of the pink residue?

Steve


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## kjavanb123 (Jan 29, 2011)

This is the stannous result on solution from dissolving pink residue into AR




Also this is the undissolved materials in AR from the pink materials



Now, I rinsed the canary color Pd salt into a quartz dish to dry and be incinerated today, and it turned out to be like this.



I will post updates today

Kev


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## lazersteve (Jan 29, 2011)

Two things:

1. Your dissolution of the original Pd salt in NH4OH was incomplete as evident by the second test swab indicating Pd. You need to use more NH4OH or you had made a salt of Pd that was not soluble in NH4OH.

2. Your incineration of the yellow powder was not successful as the color of the powder is not gray. If the second photo is of the powder before the incineration, then disregard this statement.

Steve


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## kjavanb123 (Jan 30, 2011)

All,

These are incineration process, as following

Pd salt



Pd salt being incinerated



Pd metallic powder I guess



Steve, can oxygen torch be used to melt the Palladium powder or only hydrogen torch?

Thanks again for walking me through this recovery/refining

Kev


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## lazersteve (Jan 30, 2011)

Well done on the incineration.

Melt the Pd with an oxy/hydrogen flame or leave it in the sponge form for easy dissolution by the end user.

Steve


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## samuel-a (Jan 30, 2011)

Good job kjavanb123.

If you could melt it, i would sure love to see the resulting button.


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## kjavanb123 (Jan 30, 2011)

I tried to melt is locally, and two places that deal with Pt Jewlery making, didn't want to do it since it is only 0.270grams of Pd. I am gonna compress the powder to make them stick together in form of pill, that way when tourching they don't get out of the cruible.


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## patnor1011 (Jan 31, 2011)

Make sure that powder will be totally dry as if you compress that in pill and try to melt it you may experience steam explosion. That may send powder flying everywhere.


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## HAuCl4 (Jan 31, 2011)

Nice picure show kj. 8)


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## kjavanb123 (Jan 31, 2011)

Thanks all,

I was thinking a small type of furnace with aluminum black color crucible in it, would that work to melt the Pt or Pd? 

Kev


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## Lou (Jan 31, 2011)

No, it's not that easily melted. I wrote a post about melting Pt and Pd, it should be easily found with the search engine; if any case, I'm going to be making a very big post on PGMs in the coming days. Preferably do not melt it.


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## Palladium (Jan 31, 2011)

Lou said:


> I'm going to be making a very big post on PGMs in the coming days.



I'm like a kid in a candy store when you tell me things like that.


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## Palladium (Jan 31, 2011)

If you're trying to melt it, get a high back alumina crucible and preferably go at it with an oxyhydrogen torch. Any oxyfuel torch will easily make enough heat to melt platinum or palladium. It just depends on tip and flow rate. That's why I recommend a high back alumina melting dish so that it's much harder for your powder to blow away. 

The reason why, the true reason, that carbon-based fuels like MAPP, acetylene, propane, and natural gas aren't recommended is this:

Palladium oxidizes. Platinum does not. You can usually get away melting platinum with oxyacetylene if you keep it lean at all times. You can't with palladium. Palladium has a problem that's kind of like silver's--it absorbs oxygen and fuel gases when molten and tends to spit if you don't know what you're doing. Remember well that these metals are catalytic--so any gas in a rich flame that hits the palladium is going to be split into hydrogen and carbon on the surface of the palladium. The carbon will migrate into the piece and give it a shiny gray-black look. Palladium has to be cooled below red heat in a reducing flame, and the only flame suitable for that is a hydrogen flame.


Lou
http://goldrefiningforum.com/phpBB3/viewtopic.php?f=39&t=8814#p83250


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## freechemist (Feb 1, 2011)

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.


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## kjavanb123 (Feb 1, 2011)

Freechemist, thanks for the chemistry insight. i like to know the chemical formula behind these processes.

I have to wait to process few more cats to produce few grams of PGMs in order the Pt jewler can melt it.


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## Lou (Feb 2, 2011)

@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


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## 61 silverman (Feb 5, 2011)

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.


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## HAuCl4 (Feb 6, 2011)

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


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## Barren Realms 007 (Feb 6, 2011)

HAuCl4 said:


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



He has before search his post's.


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## lazersteve (Feb 6, 2011)

What was the source material of the Pd Mark?

Nice work on the button.

Steve


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## Palladium (Feb 6, 2011)

HAuCl4 said:


> 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


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## 61 silverman (Feb 9, 2011)

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


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## kroutonz (Mar 16, 2011)

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.


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## 61 silverman (Mar 16, 2011)

kroutonz said:


> 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


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## kroutonz (Mar 17, 2011)

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


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## kjavanb123 (Mar 17, 2011)

kroutonz said:


> 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.


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## kroutonz (Mar 17, 2011)

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.


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## Inter Refiner (Jul 10, 2020)

freechemist said:


> 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


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## kjavanb123 (Jul 10, 2020)

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.


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## Inter Refiner (Jul 10, 2020)

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 (Jul 10, 2020)

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


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## Inter Refiner (Jul 10, 2020)

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


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## Lou (Jul 10, 2020)

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


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## Lou (Jul 10, 2020)

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

It is binuclear complex.


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## Inter Refiner (Jul 10, 2020)

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


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## Lino1406 (Jul 12, 2020)

Rhodium test:
Take a liquid sample, add sodium acetate to saturation (buffer). Add carefully solid sodium nitrite, NaNO2 or 60% solution, until end of brown fumes evolvement. Yellow/green color should develop. Heat over a plate or in a hot air flow for an hour. Add carefully ammonium hydroxide solution. A yellow/brown precipitate should form. Formula: (NH4)3Rh(NO2)6, ammonium hexanitro rhodate.


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## Inter Refiner (Jul 13, 2020)

Thank you lino that is very helpful 


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