Pd purifying in pictures

[kjavanb123]

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

 

[lazersteve]

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

 

[kjavanb123]

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

 

[Lou]

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

 

[kjavanb123]

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

 

[lazersteve]

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

Steve

 

[kjavanb123]

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

 

[lazersteve]

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

 

[kjavanb123]

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

 

[lazersteve]

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

 

[samuel-a]

Good job kjavanb123.

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

 

[kjavanb123]

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.

 

[patnor1011]

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.

 

[HAuCl4]

Nice picure show kj. 8)

 

[kjavanb123]

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

 

[Lou]

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.

 

[Palladium]

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.

 

[Palladium]

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

 

[freechemist]

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.

 

[kjavanb123]

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.