about platinum precipitation!

[samuelbaldwin010]

The color is not right. Check if crystals dissolve easily in water

By you saying "check the crystals " I am assuming that you are referring to the ammonium chloride crystals? I believe that they do. It's my opinion that they do through my own observation. Also I feel like the recipe for ammonium chloride is so simple it would be difficult to mess up, just hcl and ammonia, heat to evaporate, scrape up crystals. But I guess stranger things have happened..

To answer clearly, yes I believe that they dissolve easily but more so if heated a little bit. I made it with a ratio of 3:1 (ammonia to hcl) roughly.

 

[samuelbaldwin010]

First and foremost, drop the spot plate.
Use cotton buds or pieces of paper.
Much less liquid used and much easier to interpret.
I have not used Ammonia Chloride myself, but I think you need to make sure it is in its highest oxidation state first.
Bubble Chlorine through it it or add Sodium Chlorate.
Then Ammonia Chloride.

Is the sodium chlorate the same effect as the pool shock I accidentally added? It does produce chlorine gas. But also I thought that as per Hoke that you had to add ammonium chloride first to drop the canary yellow salt of platinum, then add the sodium chlorate or chlorine to get the brick red precipitate of palladium and from what I remember, please correct me if iam wrong, is that it must be in that order otherwise it will not work and you will end up dropping the platinum and palladium together right?

 

[samuelbaldwin010]

Don't feel bad....I tried that home made ammonium chloride several years ago and it didn't work for me either. I think the Pt solution has to be at a certain concentration.... not sure.

I think that it may have worked just not as fast as I thought or hoped. What I have seen and read was that a yellow platinum salt appeared instantaneously and there was no mistaking what it was.
I waited awhile and I got something yellow but not alot and it appears that I contaminated it heavily with ammonium chloride salts.

That was for the aqua regia solution, as for the hcl and peroxide solution, I definitely got what I believe is the red palladium salt. I will show pictures. What strikes me as odd though is that when I did the first solution with hcl and bleach, I got a very strong stannous result for platinum but no palladium and after I did the next solution of the black pgm powders with hcl and peroxide, I am only getting positive results for palladium.

But also, on the bottom of my bulk solution, there is alot of a black metallic like substance. Could it be somehow that this is all of my platinum that didn't go into solution somehow? Then that would explain why I was only able to get a positive for palladium. But I don't understand why that is?

If anyone has any ideas please don't hesitate to let me know.

Thanks in advance
-Samuel

 

[Yggdrasil]

First off, thank you for your timely and prompt reply.
I am using rubber gloves( the really thick yellow ones for washing dishes and such..) and/or regular nitrile gloves (depending if I am dealing with nitric at the time), I don't have a fume hood, nor do I have anywhere to put one or I would have just made one by now, so I am doing everything outside.

Sometimes I will use a respirator mask if there's quite a bit of fumes, but mostly I just try to stay up wind of the fumes. since I have also read somewhere that the masks don't actually help much, if at all, anyway, but in case it does help, I will wear it as an extra precaution.

As for the wastes I have made, I have my stock pots separated by ones that have contained gold plus non ferrous base metals, gold plus ferrous base metals,
Pgms plus ferrous, pgms plus non(no metal) ferrous base metals.
I have been just storing them in plastic jugs for now,

My plan thus far is to: after I process stock pot(s) and recover the precious metals (if there are any present), I will then cement out whatever copper there is with either zinc or aluminum, then neutralize acidic solutions, and lastly dispose of solutions in a environmentally friendly and legal manner.

For filter papers, stannous chloride test q-tips, etc. I have them being stored separately in the same manner (categorized) as my stock pots, when I get enough saved, I will process as per Hoke.

And that's pretty much it. Hopefully this answers any questions and hopefully i am using acceptable practices here.

-Samuel

I just wanted to give you heads up on the PGM salts they are extremely toxic.

 

[Yggdrasil]

Is the sodium chlorate the same effect as the pool shock I accidentally added? It does produce chlorine gas. But also I thought that as per Hoke that you had to add ammonium chloride first to drop the canary yellow salt of platinum, then add the sodium chlorate or chlorine to get the brick red precipitate of palladium and from what I remember, please correct me if iam wrong, is that it must be in that order otherwise it will not work and you will end up dropping the platinum and palladium together right?

Depending on what the Pool shock contains, maybe.

 

[Lino1406]

By you saying "check the crystals " I am assuming that you are referring to the ammonium chloride crystals? I believe that they do. It's my opinion that they do through my own observation. Also I feel like the recipe for ammonium chloride is so simple it would be difficult to mess up, just hcl and ammonia, heat to evaporate, scrape up crystals. But I guess stranger things have happened..

To answer clearly, yes I believe that they dissolve easily but more so if heated a little bit. I made it with a ratio of 3:1 (ammonia to hcl) roughly.

I meant the orange-brown crystals, neither platinum, nor palladium color

 

[Yggdrasil]

I meant the orange-brown crystals, neither platinum, nor palladium color

My guess would be some Iron salt.

 

[samuelbaldwin010]

I am not entirely certain. I don't think it's iron as the materials were from catalytic converter ceramic substrate,
But I suppose stranger things have happened. How would I go about ruling it out from the point I am at now?

And oh, yeah, the pool shock is 10% sodium hypochlorite. And it does produce chlorine gas, so it should be fine right?

 

[samuelbaldwin010]

This is the pic of the solution that I suspect somehow didn't take platinum into solution but did take the palladium into solution, probably hard to see but on the bottom there's alot of sparkling metal specks on the bottom and the stannous test shown starts off as a reddish purple then slowly turns a very dark green.
My plan is to siphon most of the palladium solution and attempt to put the suspect platinum into solution with hcl and bleach again.

 

[samuelbaldwin010]

This is the other solution showing positive results for palladium, I believe...

 

[samuelbaldwin010]

I hope this is the brick red palladium salt that I think it is..

 

[samuelbaldwin010]

And this is platinum? Maybe iron? Heavily contaminated with ammonium chloride salts?

 

[Yggdrasil]

I am not entirely certain. I don't think it's iron as the materials were from catalytic converter ceramic substrate,
But I suppose stranger things have happened. How would I go about ruling it out from the point I am at now?

And oh, yeah, the pool shock is 10% sodium hypochlorite. And it does produce chlorine gas, so it should be fine right?

Is it liqid?

 

[Golddigger76]

You would be surprised at all the different metals in catalytic converters, it is rarely just palladium or platinum and sometimes they have no platinum group metals.

 

[samuelbaldwin010]

And once again, I think I may have screwed up here.. in an attempt to boil down the bulk aqua regia solution, I got distracted and ended up having a boil over and got this yellow cake like substance everywhere. Idk what it is but in an attempt to salvage the potential values lost, I scraped it all up and put it back into what liquid remained.

Not sure what I should do about this from here. So if anyone else has any ideas, please feel free to chime in at any time. Thanks

-Samuel

 

[samuelbaldwin010]

 

[samuelbaldwin010]

Also I may have boiled down my hcl bleach solution too far down as it looks like metal is floating around in it now. And as for the other one where I suspect the platinum didn't go into solution, I put it into a new leaching solution and low and behold, the stannous test was positive for platinum. Just when you think you started getting this all figured out, a curve ball outta nowhere

 

[samuelbaldwin010]

Is it liqid?

That's a negative. It's a filter paper containing what I hoped to be platinum salt.

 

[Yggdrasil]

That's a negative. It's a filter paper containing what I hoped to be platinum salt.

Is the pool shock a liquid?

 

[Yggdrasil]

That's a negative. It's a filter paper containing what I hoped to be platinum salt.

I recommend you to stop what you are doing, you do not have the proper tools to do this.
PGM salts are very toxic and most professional refiners do not even touch it.
So you should stop and store your stuff in closed containers,
at least until you have acquired proper glassware, safety gear and protective systems to contain your mess.
Have you read Hokes and the safety sections in the forum?