# aquired 3428g of mixed pt salts...help needed



## DNIndustry (Jan 19, 2012)

I recently aquired 3428 grams of dried platinum salts. they came from catalytic converters. i also aquired some palladium salts. (See below)
I know the process the person used however there are some things i need to figure out process them. 
They used AR. DRopped Pt with NH4Cl. Pd with sodium chlorate. They said they didnt think qny Rhodium is in it.
Ive watched steves dvd several times.(nice work...thank you)
Ive played with some to test. Here are some things ive delineated
They are water soluble. 
There is Pt in them.
The person dried them..with out knowing the method and temp i feel comfortable saying most of the ammonium is evaporated however they are still the hydrated versions. im going by color(lack of yellow, orange and red mostly). these i believe are a mixture of Pt(II and IV). I dont belive they oxidized twith H2O2 before dropping. 
I believe there is also Pd and Rh contamination.
I hate Zinc chips
Id like to be able to go down several paths in testing then choose what is best for me.
Im going to try calcining, reducing with iron powder(not zinc), tributylphosphate solvent extraction, and rerefining them.
i did purchase a few 120mm quartz calcining dishes and a hydrogen torch rig.

what temps do the volitilizations occur. with ammonia. pt(IV)->pt(II)->pt?
Should i rig up a chilled vapor column to cut any losses?
Can i used hydrogen gas/vaccum to aid in the process/lower the temp?

To reconstitute and either redrop with nh4cl or reduce with iron
shoukd i use water or hcl?
What ph? How concetrated? What temp?
Should i oxidize with h2o2 so all is pt(IV)?
Should i use KCl instead or can i use hydrogen gas.
it likes to redissolve when i use zinc. how much free chlorine should there be?

Any one selling and induction heater or vaccum electric furnace for a good deal?

Thanks for the help in advance! Any advice is greatly appreciated. Im sure ill have more questions.
-Donovan


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## DNIndustry (Jan 19, 2012)

Pic


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## samuel-a (Jan 19, 2012)

DNIndustry 

Seems like you are overcomplicating things here.


Calcine the powders slowly under a stream of H2.

Leach what is possible with hot 50/50 nitric acid, wash and treat with AR.

Then go on as per Steve's DVD.


From my perspective, It is that simple.


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## awbrew (Jan 19, 2012)

Woundn't you be better off putting all the platium together and having it assayed at this point. And the same with Palladium at this point? Im Just a New be to.. But if you melt it together, isn't just going to have to be re-dissolved and then assayed ? before proving it...? There a real good thread about using a Umpire as a third party, before selling it. It is a bullet Proof, plan for not getting cheated... It might be under thread about "I been cheated by two different refineries.".

As for your question About Refineing to a pure state. That would be Chapter 14 In Hoke, Although You should probably read the entire book all the way threw and understand it before trying...

Anyone seeing anything wrong in what I said please correct me...

P.s. I looked for the thread, I was talking about and can't find it.. Maybe Palladium can help ?? I was trying to give the link to this thread but can't find. I cut and pasted it to a txt file on the desk top, I just pasted It back here...

Not sure who wrote it ? Any help...

" I hear a lot of complaints about being ripped off by refiners but it seems that few people know how to prevent it. How many of you would go into a bank with a pile of money and tell the teller that you don't know how much is here but if they will count it and credit your account you would appreciate it. You know sooner or later you'll get ripped off. Going to a refiner and handing them a pile of scrap to pay you for is the exact same thing. If you don't have the capabilities to melt the material go to the refinery and witness the melt, don't let it leave your sight. If the melt was large enough they will take a dip sample, make sure the melt is molten and stirred before sampling. If it is a smaller melt, still make sure it is molten and stirred before they pour it. Inspect the bar and the slag after the pour. If the slag has alot of beads put it in a bag and take it, it contains your metal. Now they will either drill your bar, make sure if it is a drilling they take it from both the top and bottom, if they took a dip sample they will cut it into small pieces. Both the cutting of the dip sample and the drilling will be done in front of you. They will package up 3 small samples of at least 1 1/2 grams each (1 pennyweight) I would request more sample, at least 3 grams so you have extra in case you need to run another assay. You take 1 sample, they keep 1 sample, and a 3rd is for an independent assayer in case you don't agree with their assay. I like to request the right to take my bar back if we don't agree on assay, so since all bars tend to look alike, sign the bar on both sides with a marking pen. Also sign the seal of the umpire sample. If you follow these steps they will know you have been around the block before and your settlement will be treated with respect.
Now before you leave take a receipt with you which states the weight they will be paying you for. It should be the weight of the bar plus the weight of their sample, plus the weight of the umpire sample.
Now it's just like you counted the money before going into the bank and you have a receipt. You now have recourse if you don't like the result!..Of course you have a written list of what the charges will be for the refining services, what metals they will be paying for (don't let them keep your silver either) And you had it before you went to the refiner in the first place. To be fair to the refiner, because there are refiners who do legitimate business and are entitled to make a reasonable profit, you will be paid a percentage of all metals refined and if some metals do not reach a minimum deduction you will not be paid for them. There are also things like splitting limits which means if your assay differs from their assay by more than a defined percentage (never over 0.25%) you will use the umpire 
sample to determine who is right. If you are within the splitting limits you split the difference. Umpire assays are not cheap and the looser pays the tab. Shop a few refiners, read their terms and do what I wrote above and you should be OK for melt-able scrap. Find a decent assayer and have your sample assayed, in the event of a difference, keep track of who wins, if your assayer looses too often, find another. A good assayer is like a good heart doctor except they don't make as much money.

If you follow the procedure above you will leave the refiner with no cash in hand, but you will have receipts which are legal documents. Send out your assay sample ASAP and when you have a result call the refiner to exchange assays. In most cases they will tell you their assays first, if their number is higher accept it and go to the next metal. This process will take a few days longer if PGM's are in the bar but you can usually settle gold and silver within 2 days. When you settle you tell them which day you want them to price your metal and they will cut a check for you on that day.

There are similar precautions for non melt-able scrap and if anyone is interested just ask. It isn't fair to complain about being ripped off if you didn't go into the refinery prepared.

Burning crushing and sifting. Sampling material that needs incineration and sweeps preparation is never a 1 day deal. When your drums arrive at the refiner, with your seals on them, they will call you to schedule your visit. Always let them know when you intend to come or would like to come and schedule delivery so the material isn't at the refinery too long. Who knows what can happen, you've safeguarded the scrap this long so be safe. They will put the material into the incinerator and start a burn cycle. If they say it will need raking during the process be there when the oven is opened. Usually they burn overnight so seal up the oven until the morning. Your material is ready for crushing in the morning, usually after a rake to see if it's still smoldering, if it is let it burn out. Before the material is put into a ball mill, check to see that there are only balls in the mill. Have them install the dump grate and spin the mill to make sure no left over material is in the mill. 
Add your material to the mill and let it crush for the required time, usually 1 hour. They will then dump the mill into the enclosed housing and take your crushed powder to the sifter. Again have them spin the mill to assure it is empty. Some representatives make the refiner weigh the material out of the incinerator so they can track the weight and be sure it is all there after milling and sifting. (Not a bad policy) Finally the material is sifted, the majority of the fine powder represents your greatest values, this is where your samples will come from using the sampler the same as in the previous post. They rarely dry a sample after incineration because it hasn't had time to pick up moisture. There is oversized material in the sifter, it is your material and it almost always contains values. Have it put in a 5 gallon pail and put a seal on it and take it home. When you accumulate enough of this stuff bring it back for crushing and sifting again. Usually there are 3 fractions coming off the sifter, the oversize is broken down into magnetics (low value) metallics (higher value, usually there's bigger pieces of gold in there) and chunks of wanna be powder that didn't crush. You want it all. If there's a large fraction of metallics the refiner may suggest melting it. Finish with your sweeps samples and rep the melt just like the method described for melt-able scrap. Again you will leave with paperwork stating the settlement weight, you will have sealed up an umpire sample and you have your sample. And you have seen it all processed before your eyes. The last type of material to watch at a refiner is e-scrap, my next post will detail that sampling process, I have to rest my fingers.

The last and possibly the most popular type of scrap (for this forum) to send out to a refiner is e-scrap. From what I've read on this forum a-lot of our members get this scrap and cherry pick the good stuff for refining or do some sort of preparation so they can recover the metals from the higher yield components themselves. This will always leave some kind of lower yield material that is ripe for sending out, providing you can get paid fairly for what's in there. Again the only way to tell what is in there is to sample the material and the sample has to be representative. This material is generally stream sampled. What that means is they chop, shred, grind or pulverize the material into uniform sized chunks so they can draw off a proportional sized sample. A stream sampler will sample shredded paper as well as it will sample lead shot, and therein lies its weakness. It is up to you, the generator of the material, to separate the material into grades of like density scrap. 
This is a bit of subjective sorting here but let me explain. The material which has been processed into like sized pieces is moved along a conveyor and dropped into a chute as a steady stream of parts, the machine is programmed for say a 25% sample, by switching some diverting arms the sample streaming down the chute is diverted into different lines, one line goes to the 75% accumulating pile, and the other to the 25% pile. It is amazing to watch and I have watched it and weighed the fractions coming off and it's pretty dang close to right on. This procedure will then be repeated on the 25% fraction to produce a fraction which is 6 1/4% of the original and so on. They continue until you have a representative, manageable sample of the entire lot. This sample is either incinerated, crushed, sifted, and the oversize melted with copper, or it's melted directly with copper. The benefit is the smaller sample is produced into an assayable sample while you watch.

Now for the glitch...... ........if the material is a mixture of say steel relay headers with gold pins, and depopulated PC boards, the sampling will not be so great. The heavier steel headers fall faster than the light circuits so the stream isn't as dense consistently. Now if you have enough headers to run separately, and enough boards to run separately, the densities will be similar and the sampling is very good. The refiner doesn't know if a bad density mix will work in his favor or in your favor so he isn't too anxious for sampling of poorly sorted materials either. So the sorting is the job of the collector, you, before you ship for stream sampling.

The material which you have pre sorted is received at the refiner where they will decide if it will be best to granulate, shred, ball or hammermill this material before stream sampling. Whatever they decide, you will be part of the decision, and with your nod the material will go through the tortuous process. You will know your start weight and verify the finish weight. From looking at the parts they will also let you know if it will need incineration (likely if it was PC boards) or straight melting. Now it's off to the stream sampling machine. I've brought in 20, 55 gallon drums of plated connector scrap and had it reduced to 3, 5 gallon pails. Now you get to do eenie meeney miney mo and pick one for processing. The other two are sealed up in case another sample is needed.

If the material has to be incinerated, you will end up with a powdered sweep portion which is sampled for assay just as described for sweeps processing, the only difference is the rather large metallics fraction. Actually they mix magnetics and metallics together for a melt with copper. You will witness the melt and just as before with meltables come away with samples and a sealed umpire. If the job didn't have to be incinerated, it goes directly to the melt room.

In both cases you have come away with samples which you witnessed and are reasonably sure represent your material.

This last type of processing is only done by rather large refiners and if they will not let you witness everything, say thank you and find another refiner who will. If you do enough of this type of recovery, and keep records about different materials you will generate enough data to feel confident that you are getting your just return. Just don't get confident enough to let them process it without you there.

There are others on this forum who have witnessed materials as I have and I invite all comments concerning what I have said or more importantly about what I may have missed.

I received an e-mail with a question about the post on melt-ables which is worthy of repeating. The question was what about the small pieces of steel that end up on the top of the melt? Good question!
A-lot of jewelry has spring wire in it for clasps or other reasons. First of all when you are buying the stuff you should check if it is magnetic. If it is sometimes it is plated so you don't buy it, sometimes it is plumb karat but the magnet sticks to the end with a catch or some clasping mechanism. Here you have to make an educated guess about how much weight to deduct because something in there isn't gold. Now you're at the refiner and your bar is melted and you notice magnetic pieces on the bar. (Surprise! your refiner has a magnet too) You can estimate the weight and subtract it from the bar weight, but that's a guess and they guess high and you guess low. If the refiner really knows his stuff he will have some phosphorous copper on hand. Great stuff, it will take magnetics into the bar 
and make it nice and homogeneous so there is no issue. Remember your bar will gain weight so the assay will go down..... same amount of gold is still there. The phos-copper comes in nuggets and 2 ounces added to a 100 ounce karat melt will dissolve maybe 1/2 ounce of steel. I would pull out all of the pieces with magnetic tendencies and do a separate melt. I would be doing this before going to the refiner. Make sure your refiner has phos copper for this purpose and when you have enough for a melt with magnetic karat run it together. If the refiner doesn't have phos copper, regular copper will work but you will have to add more copper because it doesn't get the phosphorous boost to help the melt. Having the melt without floating magnetics is a better way to get a good return but remember you have to pay the customer less for the piece when you buy it too. Be kind, the springs don't weigh that much!



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Active Member 


Posts: 1371

Joined: April 5th, 2009, 8:05 pm

Location: northeast USA



April 24th, 2009, 1:46 pm 

XRF good for buying scrap, bad for settling with a refiner

I have been reading on the forum about members using or wanting a XRF for gold assays. For buying gold from a customer selling a few pieces it can't be beat, it is quick and it definitely beats testing 
on a stone for qualitative analysis of other metals present. If you are buying gold and selling it to a refiner you should never accept an X ray result. Let me explain why. You go to a refiner who only 
charges you 2%, no melt fees or assay fees. The real selling point is quick same day settlement, how can you go wrong? The way you can go wrong is that the XRF machine is a calibrated machine. That 
means if you start with an alloy which you know is plumb 14K, you've had it fire assayed so you're sure, you sample this alloy when setting up the calibration and tell the machine this is .5833 gold 
(assume plumb). This is great for a manufacturer who uses a bunch of different alloys and programs them into the device, now all he has to do for quality control is a quick scan and he knows what his 
alloy is. The problem lies in the fact that a refiner doesn't know the starting alloy so at best it is an approximation. But what if the refiner puts in a piece of plumb 14K and tells the machine it's
13.5K. If you do the math the difference between 14k and 13.5K is 2.08%. If your total melt had a content of 1 kilo of fine gold and was 14k to start, the machine assay, if it was calibrated to read 
lower, will cost you another $600 at $900 dollar gold. True you saved on costs because you didn't pay for the assay or the melt, but you got beat for at least $500 ! After you leave the refiner will 
always run a fire assay before he puts it in production because he needs to know the real answer before he refines it. If you had waited for a day or 2 and settled on a fire assay, this can't happen. 
Now it is true that if the machine is calibrated 1/2 k off the refiner is only charging you 4.08% for 14k material, but the calibration can be off by more than that as well. But his claim was 2% no other
fees.

If you do this kind of buying and send out your refining here is a little trick you can put up your sleeve. Save your extra dip samples from your previous lots, you know the assays because you sent them 
to a fire assayer and you also know the numbers you settled on. If your current lot is say close to 14K, bring a pin sample that is similar. Now when they are ready to read your new sample, whip out your
pin and say "can you read this sample first?" If they do it, usually they get flustered and give some lame excuse, compare the reading they give you with the assay you know to be true. If it's close
you've found an honest refiner. (don't be too surprised, they are out there!) If it's off humor them while they give you an excuse and say it's OK, we'll settle with a fire assay! By the way, if you do 
the little check this pin trick first and then settle on a fire assay, you should only pay the rates you were quoted (if in writing) but guaranteed the next time you refine with them, you'll get new 
rates!

The lure of the fast settlement is often the tip-off to hidden charges



The difference between stupidity and genius is that genius has its limits. Albert Einstein
1. Refining Precious Metal Wastes C.M. Hoke http://tinyurl.com/mfnyhs
(REV) (Free Download)
2. Get the (FREE) Gold Refining Forum Handbook VOL 1 here >> http://tinyurl.com/nyutnp
3. Get the (FREE) Gold Refining Forum Handbook VOL 2 (Final) here >> http://tinyurl.com/y9w5y73
4. Chemistry Handbooks Here (FREE) >> http://tinyurl.com/n27pqu
ALL FREE-----ALL THE TIME


Ha guys, as soon as I find the link to this, I can delete it back out..
Thanks


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## lazersteve (Jan 21, 2012)

I would simply convert the salts together with zinc turnings/HCl or ammonium hydroxide/hydrazine to the mixed PGM metal blacks.

After that separation of the blacks is easy using dilute nitric acid to remove the Pd (as Sam suggests) then heat in AR to put the Pt into solution, followed by precipitation of the clean Pt with ammonium chloride and finished up with zinc turnings/HCl or NH4OH/hydrazine of the canary yellow Pt salt. 

You may have luck with putting the enitre lot in 10% NH4OH to separate the Palladium from the Pt salt. As described under my post here:

Purifying Pd Colored Salt

Steve


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## DNIndustry (Jan 22, 2012)

Thanks everyone for the responses
anyone have a source for hydrazine...the damn chemical i dont have.


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## samuel-a (Jan 22, 2012)

DNIndustry said:


> Thanks everyone for the responses
> anyone have a source for hydrazine...the damn chemical i dont have.



I think Hydrazine Sulfate is sold in the US as food supplement.


Formic acid is another option you can use to collectively reduce all PGM's.

If all else fails, HCl and zinc.


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## lazersteve (Jan 22, 2012)

DNI,

PM sent.

Steve


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