UPDATE : Can someone please help with copper pgm seperation

[Slaughlin79]

I solved my problem with help from another member and is working well so far. After dropping everything from solution with the zinc, and was having copper show up, I just re dissolved all the material and since there was copper already in solution I just used copper I had dropped from a nitric solution I had used to dissolve a bunch sterling silver. It worked and Ive got mor than I thought. I added the copper and turned up the heat and kept the solution acidic with additions of HCl and all the copper turned black. Here’s a couple pics of about half of what I’ve got. The plastic bowl is a test batch and the Büchner is a large batch. Thanks for all the help. And I quit using the aluminum and won’t ever used again if I decide to refine converters in the future again.


I started a batch of catalytic converters and dpf’s a while back and when dropping with zinc and aluminum “zinc is much better” I have gotten copper like I would not have believed.

I actually dissolved the copper pgm precipitation, evaporated, filtered and then added my ammonium chloride solution and got a orange yellow drop. “More yellow than orange” I let that settle for a bit and came to find a thick layer of green which would be the copper.

So after I filtered I didn’t even rinse the platinum/copper precipitation into the solution of now mostly palladium solution just so I didn’t accidentally dissolve some of the copper to put back in solution. After, I present the solution with chloride gas and the red palladium comes out.

Now I understand that now I should dissolve with ammonia and that should leave only the palladium in solution and then I can filter than precipitate with HCl.

Here’s my problem. How do I separate the copper from platinum? If I just add water both will dissolve and If I add diluted 10% ammonium chloride nothing happens just like with the platinum. Will low heat dissolve it? I read a lot on a lot of different subjects and I know to search for answers but all I can find as far as copper platinum seperation is electrolyticly which I’m not interested in doing. This is the first time im doing this but does anything have an answer that’s not pointing me in a direction? I need to get this stuff finished up bc it’s been going on for almost a year

 

[Platdigger]

pm sent

 

[anachronism]

pm sent

Not to cause a squabble here but I've been pulled up for offering to give someone advice via PM in the past. Correct Dave?

 

[Lino1406]

Separating Pt and Cu is easy. I'd like to mention that ammonium chloro palladite could be green

 

[snoman701]

pm sent

Not to cause a squabble here but I've been pulled up for offering to give someone advice via PM in the past. Correct Dave?

I don't know anything about this, but I don't know why we don't take greater issue with people who are leaching cats in a amateur environment.

I have nothing against the original poster. I understand the desire to try things for educational purposes. But when it turns in to a profit motivated venture, one has to be more controlled.

Here would be my suggestion. Stop processing cats. Buy a quarter ounce of platinum and palladium. Keep your amounts small, use only as much acid as is needed. Learn to do the separation on small volumes. ONLY when you have mastered that, do you move on to cats.

If you are cooking down leached cats without a sealed reactor, you are killing yourself, creating toxic waste and could be polluting your work environment to a point that it's going to be cheaper to demolish it than proper remediation of the danger.

 

[ChemGeek]

@snoman701,
Actually what does it mean for you "cooking down leached cats"?
Leached means already free of PGM.
If so, then what's the point to "cook them down", whatever it means?
Leached cats are of no further use and one should dispose them off.
Or do you mean "concentrating solution of PGM produced by leaching cats"?

 

[snoman701]

@snoman701,
Actually what does it mean for you "cooking down leached cats"?
Leached means already free of PGM.
If so, then what's the point to "cook them down", whatever it means?
Leached cats are of no further use and one should dispose them off.
Or do you mean "concentrating solution of PGM produced by leaching cats"?

Yes, concentrating.

Disposing of aqua regia leached cats isn't that great of an idea. Batch them in sealed barrels. Cats leached in aqua Regia will still have a lot of value in them as you won't get a majority (if any) of the rhodium and a sizeable amount of the palladium.

 

[ChemGeek]

@snoman701,
Chlorine or bromine based leaching solutions are more successful than aqua regia for this process and also more user friendly. Most of rhodium will go into solution as well. After such treatment catalyst has very little values left.
http://citeseerx.ist.psu.edu/viewdoc/download?doi=10.1.1.459.4122&rep=rep1&type=pdf
There is also no need to concentrate large volumes of PGM present in leaching solution as these can be precipitated with suitable reducing agents like zinc, water phase decanted or filtered off and metals refined again in smaller volumes.
But I agree that a person who has already contracted platinosis would find life miserable, if his kitchen and bathroom is contaminated with platinum salts.
Mind you, during my working career I went through several kg of hexachloroplatinic acid and much more of palladium salts while processing spent industrial catalysts and no platinosis.
Allergies are funny though, one of workers was a company "azide detector". His face was turning into horrible red-purplish colour whenever even minute quantities of hydrazoic acid were present. He was a good evidence showing limitations of industrial fumecupboards. It was *impossible* to work with azides in his presence without making him miserable, so he was getting a time off whenever such work needed to be done.

 

[Geo]

Have you tried small amounts of copper metal dust on the first dissolution?

 

[snoman701]

But I agree that a person who has already contracted platinosis would find life miserable, if his kitchen and bathroom is contaminated with platinum salts.
Mind you, during my working career I went through several kg of hexachloroplatinic acid and much more of palladium salts while processing spent industrial catalysts and no platinosis.
Allergies are funny though, one of workers was a company "azide detector". His face was turning into horrible red-purplish colour whenever even minute quantities of hydrazoic acid were present. He was a good evidence showing limitations of industrial fumecupboards. It was *impossible* to work with azides in his presence without making him miserable, so he was getting a time off whenever such work needed to be done.

I helped clean up a mess, that's all that I'll say. It left me with a serious paranoia about what I could have messed up if I had developed platinosis.

It's not just kitchen and bathroom. It would be life, if proper industrial hygiene were not adhered to. Does this person have an area that is wet mopped daily. Do they have refining specific clothes and boots. Do they take showers before putting their head on the headrest in their car. If not, cleaning up the low level contamination that could make one miserable is simply impossible.

That is my reason for having little patience for "i tried processing cats in a bucket". I was the guy that cleaned up the mess.

 

[anachronism]

But I agree that a person who has already contracted platinosis would find life miserable, if his kitchen and bathroom is contaminated with platinum salts.
Mind you, during my working career I went through several kg of hexachloroplatinic acid and much more of palladium salts while processing spent industrial catalysts and no platinosis.
Allergies are funny though, one of workers was a company "azide detector". His face was turning into horrible red-purplish colour whenever even minute quantities of hydrazoic acid were present. He was a good evidence showing limitations of industrial fumecupboards. It was *impossible* to work with azides in his presence without making him miserable, so he was getting a time off whenever such work needed to be done.

I helped clean up a mess, that's all that I'll say. It left me with a serious paranoia about what I could have messed up if I had developed platinosis.

It's not just kitchen and bathroom. It would be life, if proper industrial hygiene were not adhered to. Does this person have an area that is wet mopped daily. Do they have refining specific clothes and boots. Do they take showers before putting their head on the headrest in their car. If not, cleaning up the low level contamination that could make one miserable is simply impossible.

That is my reason for having little patience for "i tried processing cats in a bucket". I was the guy that cleaned up the mess.

And this is why you have people incinerating stuff in a pan in their back yard. Without having a clue about what contaminants may be there. Cadmium, Beryllium, all kinds of things going up in the smoke. Most of which is inhaled by not only the person doing it but their families and neighbours.

Absolutely crass ignorance and stupidity. And yet we support it.

People here cry loudly and scream nasty words about how evil Cyanide is. It's a lot safer than this shit that you're advocating.

 

[ChemGeek]

I would also notice that sieving chip ashes is actually *deliberately* making airborne fine dust often containing beryllium in addition to one carried out with smoke and I won't even go to details, what sort of niceties careless heat gun/sand bath treatment of PCB-s can release.
Main reason why I will never run this "technology" at my home or in my garden. Why beryllium should be any healthier than platinum?
I is obviously *not* the case and beryllium related problems, should they develop, are far worse.
Ending "further exposure" does not resolve berylliosis as is usually the case with platinum allergy.

Honest advice about home refining is such:
If you don't organize your lab at least to semi-industrial standard (means $$$$$) and you don't have sufficient scientific and practical knowledge how to operate it properly, you are likely to harm yourself and your family, particularly if your adventure is not one off trial but regular activity. Probably you will also harm your neighbors if you run cowboy like approach full throttle.
If you get there or/and your neighbours suspect something and further investigation showed unusual and harmful chemical elements in *their* gardens and source could be traced to you, then your legal liability and compensations paid could ruin you for life.
You are also constantly infringing various environmental regulations, small scale but still.
About all what amateur can do (assuming basic knowledge) safely is separating gold from gold plated pins and fingers.

But everyone is free to become new radium girl as s/he pleases.

 

[Slaughlin79]

How is buying a half ounce of fine platinum and dissolving that going to teach me a single thing about catalytic converters? I get it that some people have all the money they need to have their sealed system and you should be happy with that but that my question. I don’t understand how I can read through so many of these threads and see so much negative comments persuading people to not refine when this website is here to learn about and get help with refining and nothing is done about it. You people,the ones that have the money to buy all the fancy stuff that the little guy would love to have,and only the ones that try to bully people out of doing refining are the ones I’m talking it because not all are bad, must have been born with a silver spoon in your ass and not understand where hard earned come from. Not all people as lucky to have the funds to buy all the latest equipment. Im on a site that I cant abbreviate bc and have to use the actual because word but you jerks “I want to call you something else but I for one have respect for other people” can come on here and gripe a person out on a website that’s just for what the hell they are asking about. If you don’t have a helpful answer and just got on here to tell me to stop bc I don’t have a million dollars for the right equipment “if I had a million a could throw away I would be on a ranch right hunting by the way” then I ask you to not reply to my thread. So if no one else ever replies of what I just said so be it because this is the last refining I probably will ever do. But thank you for not giving one useful piece of information.

 

[snoman701]

How is buying a half ounce of fine platinum and dissolving that going to teach me a single thing about catalytic converters?

By learning the processes of individual metals, and mastering a simple system, prior to trying to master a complex system. It's the same advice Hoke gives. Start simple.

Did you read Lino's advice?

I'd like to mention that ammonium chloro palladite could be green

 

[Slaughlin79]

Look man no offense but I have a mom,a sister and a niece with a crap dad I have to support so buying an ounce or half of platinum just to play with us out of the question. Thank you to the people who helped me with answers I really do appreciate it.

 

[Slaughlin79]

For the people who actually don’t mind helping this question is for you. Is pgm black always a grayish color? I ask for one, no matter what I search I can’t find any reference except for being black which is deceiving
,and two because I have some that is dark gray and some that is black? I used copper I got from a copper nitrate solution that was left over from some silver I had refined a while back. So what I did was used zinc to precipitate the copper and washed it and added to my pgm solution.

 

[Geo]

Now that you have your PGM material concentrated, you can redissolve the PGM blacks in the least amount of acid needed. The safest way is to use HCl and chlorine gas, since you are dealing with a powder. If you have the experience, a gas generator works well. You will have a purer form of chloride solution. Simple heat and evaporate to concentrate and remove any excess chlorine.

Ammonium chloride is added as a saturated solution to precipitate Pd. This should be a dirty drop. Collect the brick colored salt and add it to a beaker. To this add ammonium hydroxide and stir. Add small amounts and stir and wait. When you add solution and no more solids dissolve, filter the solution and rinse the solids with ammonia.

Once you have a clean, yellow solution, add HCl a couple ml's at a time and more pure, yellow Pd salt will precipitate. Keep adding HCl until the solution is acidic. Now you have a very nearly pure form of palladium chloride salt.
Compliments of lazersteve and ms Hoke.

 

[FrugalRefiner]

Slaughlin, if I may offer a friendly word of advice, I'd suggest dialing back your attitude a bit.

While you may not have liked snoman's suggestion, they were intended to help. Experimenting with small amounts of pure metals is a well accepted method of learning this art.

Many members can't afford the latest equipment. I am a frugal refiner and I make do with what I can. Others can afford better labs and equipment, and they should be able to discuss that here as well. We can all learn from each other. I may never have the level of equipment that some have, but I can learn things from them that I can make a frugal version of to suit my needs.

You seem to have a dislike for those who are more fortunate than you. That's a shame. Like many of our members, I have seen my share of tough times, when I had no food and didn't know where I would get money to buy my next meal. I've had to avoid my landlord when I couldn't pay the rent. But I never resented those who's lives weren't as hard as mine.

No one here knows your personal circumstances unless you mention them. So some posts and suggestions may not be appropriate for you. We suggest using nitric acid all the time, but we know it is expensive and difficult to find for many. It doesn't mean we shouldn't suggest it, and it doesn't mean that those who can't get it should become irritated at those who suggest it.

When someone offers me a suggestion, I try to thank them for their advice, even if I can't use it.

Dave

 

[g_axelsson]

I totally agree with what Dave just wrote. I just want to add a couple of thoughts...

There are two kind of refiners here on the forum. The ones that does it as a way of earning their income, putting food on their tables. They might still have a burning interest for the art of refining but in the end the decisions on how to process and what to invest in is based on an economical reality. Then there are the ones that is pursuing this as a hobby, not relying on refining for their salary.

If you are pursuing refining to make an earning then you have to do some investment. Sure, you might start slow but every month you haven't started your business is another month of salaries lost. If an ounce of platinum is too expensive to buy to learn the trade then you seriously lack the cash to equip a lab and purchase material to refine. If you can't get an ounce of platinum back into metallic form then you won't be able to do it with material collected from scrap. You should be able to sell the ounce back after you have learned to refine PGM:s. If you can't sell it how can you expect to sell your product later on.

You might not need a full ounce, just a few grams would be enough for experimenting. It's an investment in knowledge and you only need it for a while.

Göran

 

[ChemGeek]

Look man no offense but I have a mom,a sister and a niece with a crap dad I have to support so buying an ounce or half of platinum just to play with us out of the question. Thank you to the people who helped me with answers I really do appreciate it.

We are not asking you to buy most modern eqiupment to do small refining.
However initial $10000 in your labware allowing you to work with PGM without contaminating surroundings, next $10000 into premises separated from your main property, well ventilated and maintained is a must.

You should also have your own land and dont drop more than minute amount of waste stream down the drain or you will get an attention of authorities (and incure fines) soon enough. You must either electrolytically recover other metals or treat it with lime + 10%of gypsum (what makes them harmless and sent to licensed landfill site.
Assuming that you are skilled DIY person and keen chemist & engineer and a person who diligently look for 2nd hand items on different auctions, you will set a reasonable small scale operation at budget of $20000 or so. That is if you already have a suitable *land*.
By doing so, with time you could claim some invention (not so difficult in urban mining area), find sponsor, make patent application, base on this apply for government grant and end up with proper refining business, small scale but still.

If you live in flat/terraced/semidetached house with your mom, sister and dad this activity is not for you. Once you have contaminated your property with platinum salts and one of you got platinosis, you will need to abandon it or your life will be hell. If you harm neighbours properties, legal claims can ruin you. It is not worth.

And if you don't have $200 for a quarter of ounce of platinum to experiment with, then forget it entirely.
$200 I am spending every 2 months on dog food.

I am not trying to be malicious but one has to recognize his limitations when they are there.

Mind you, many professionals here will deter you deliberately, because market is already not easy and they fear new competition coming.
They hate 3rd world, cowboy like practices, which are destroying their legitimate business and at the same time are damaging to environment and workers/bystanders health.