Inquart mixed PGM's?

[nickvc]

Know the man well and I had similar problems with him
If your material is metallics and not salts you should be able to melt them depending on the PGM content and an xrf on several surfaces should tell you how good a melt you got.

 

[Justincase]

Yep, interesting how this secrecy and practically divided monopoly evolved around PGMs. Why not the other metals.

That was why I invested so much time and effort to elaborate the PdPtRh "separation - recovery" method with acceptable losses. And failed miserably, to be honest. Then stuck with health issues, so I am out for several months and cannot perform experiments on PGMs. And I was relatively close to tuning the NH4Cl precipitation that way it do not drag too much Rh with it. That was the annoying step, so much Rh was trapped in the precipitates of ammonium platinate (nearly 40 % sometimes, from that 1-2% starting Rh content). Later steps were pretty much straightforward - cementing the PdRh remaining solution on zinc, boiling the precipitates with water to get rid of chlorides (practically) completely (AgNO3 test pass) and then digesting the cement with HNO3. Filter palladium nitrate and get enriched Rh cement fraction.

If I was ever to accomplish the recovery of more than 50% of the contained Rh to some enriched fraction, it will go straight here to the forum, for free and for anyone.

The problem is not one of recovery or refinement.
Tho that would maximize returns and eliminate the inaccuracies of the assay system.
The doorkeeper of that trade is one of quantity until you are over the required lower limit,
the only show in town J.M. will not talk to you.
Quite fascinating the world of catalytic screens for industrial use.
But because of their excellence and monopoly of the world's most P.G.M.-dependent industry, they set the standard.
Until you get above that entry-level you are stuck.
Even national-level labs do not have a controlled atmosphere tube furnace or an induction equivalent.
Just got to save until you satisfy them and cash in for close to spot.

 

[Justincase]

Know the man well and I had similar problems with him
If your material is metallics and not salts you should be able to melt them depending on the PGM content and an xrf on several surfaces should tell you how good a melt you got.

I have a tube furnace, But will not have any tubes made until I have enough space to give it a dedicated area to live in, dam expensive hand made quarts tube apparatus.
I have never felt comfortable with trying to melt Pt and Pd even with a hydrogen torch.
First, you would need a pill press to form the black into something that would not simply fly out of your melting dish secondly getting a normal dish up to heat can be a challenge so upping that by six or seven hundred degrees centigrade strikes me as outside that tools productive operating level.
I would like a vacuum chamber with an induction coil, any metal can then be put into a carbon mold, brought up to its melting point under vacuum, and left to cool.
Should yield nice clean bars of all elements, but particularly facilitate Pt and Pd.
Even with that, I would still have to hand what was left over to J,M. But luckily with the value of Rh that should not be too large a lot.
Until then I will just squirrel away.

 

[MicheleM]

Probably this is a stupid comment but, what about the idea to separate different platinum group metal salt solution via centrifugal force? Like in nuclear industry, they used to separate UF6 different isotopes. I mean if chemically is too difficult , maybe physically could be a viable option.

 

[Geo]

I have a tube furnace, But will not have any tubes made until I have enough space to give it a dedicated area to live in, dam expensive hand made quarts tube apparatus.
I have never felt comfortable with trying to melt Pt and Pd even with a hydrogen torch.
First, you would need a pill press to form the black into something that would not simply fly out of your melting dish secondly getting a normal dish up to heat can be a challenge so upping that by six or seven hundred degrees centigrade strikes me as outside that tools productive operating level.
I would like a vacuum chamber with an induction coil, any metal can then be put into a carbon mold, brought up to its melting point under vacuum, and left to cool.
Should yield nice clean bars of all elements, but particularly facilitate Pt and Pd.
Even with that, I would still have to hand what was left over to J,M. But luckily with the value of Rh that should not be too large a lot.
Until then I will just squirrel away.

I make a saturated solution of borax and distilled water. Little more liquid than a paste, I dampen the PGM blacks with this before melting. I use a propane/oxy cutting torch and it melts PGM's like a charm. I melt in a Wesco highback melting dish exactly like this one.

 

[Justincase]

I make a saturated solution of borax and distilled water. Little more liquid than a paste, I dampen the PGM blacks with this before melting. I use a propane/oxy cutting torch and it melts PGM's like a charm. I melt in a Wesco highback melting dish exactly like this one. View attachment 49583

It is not that I do not understand how it might be just about achieved.
It is more that I am unsatisfied with such crude methods that will result in waste and potentially Organic platnouse compounds if melted with a carbon-based torch.
People do a lot of things, but few stop to think if they should be doing so.

 

[Geo]

I understand that. I wish I had the same options you have on philosophy. My philosophy is, use what you have, when you can.

 

[Justincase]

I understand that. I wish I had the same options you have on philosophy. My philosophy is, use what you have, when you can.

If in an escape and evasion mode I can see them being valid tactics.
But I hope you are not in a pure survival mode.
If given the time and space I see no reason to compromise your methods.

 

[Justincase]

Probably this is a stupid comment but, what about the idea to separate different platinum group metal salt solution via centrifugal force? Like in nuclear industry, they used to separate UF6 different isotopes. I mean if chemically is too difficult , maybe physically could be a viable option.

I think you will find the technology that can separate closely related elements by their mass centrifugally is very demanding and controlled.
You have mentioned why that is. to prevent the proliferation of nuclear devices.
The tolerance of such centrifugal separators is phenomenal, I do not know anyone capable of building such a system.
not to mention the power requirements for such systems.
A few years ago the CIA destroyed the enrichment facility of another nation simply by infecting their lynx-based systems with a small bit of malware which pushed a decimal point one or two places out.
The result was all their centrifuges ran over speed and BOOM!
I can think of a number of people who would pay you just about anything you can think of if you can demonstrate a working unit.

 

[orvi]

Agreed. Small scale business is vanishing, not only from PGM industry. Naturally or forcefully.
I was just upset when I heard our 2% Rh in material wouldn´t be paid. Knowing that they will certainly be paid for it, when sell to bigger refiner who actually refine the mixture. Straight rip-off.

 

[orvi]

I make a saturated solution of borax and distilled water. Little more liquid than a paste, I dampen the PGM blacks with this before melting. I use a propane/oxy cutting torch and it melts PGM's like a charm. I melt in a Wesco highback melting dish exactly like this one. View attachment 49583

When I was melting Pt or Pd, I was using MgO cupels. Cheap, easy to handle, resistent to the temperature required for melting... And there is no possibility of carburizing the metal when melting. Also you can purchase MgO powder and press one on your own. Cheap stuff, but many times you need to contact larger facilities - they may not be willing to sell you one 25kg sack. Here, I tried two, and one was keen to sell sack for 75 euros. Not great not terrible. Last you a lifetime

 

[orvi]

I think you will find the technology that can separate closely related elements by their mass centrifugally is very demanding and controlled.
You have mentioned why that is. to prevent the proliferation of nuclear devices.
The tolerance of such centrifugal separators is phenomenal, I do not know anyone capable of building such a system.
not to mention the power requirements for such systems.
A few years ago the CIA destroyed the enrichment facility of another nation simply by infecting their lynx-based systems with a small bit of malware which pushed a decimal point one or two places out.
The result was all their centrifuges ran over speed and BOOM!
I can think of a number of people who would pay you just about anything you can think of if you can demonstrate a working unit.

Idea is interesting. As organic chemist, I was more interested in chromatographic separation of these elements because it is stated in literature, and it works. However, not for hundreds of grams... But that ease of separation is so tempting - took a syringe with soluble complexes of the PGMs, inject them to the column of stationry phase, start pumping mobile phase (buffered water) and you separate individual PGMs salts as fractions. When you have transparent glass or plastic column, you can clearly see bands of different colours going down. If you get the mobile phase right, you get 99+% separation/purity.

With centrifugal separation, I have no idea how big the force must be to start moving up molecules eg in solution. I will need to calculate it... Also very clever idea - Pt is nearly twice as dense as Pd. So this separation could be accomplished more easily (I assume) than uranium isotopes. But I´m staying rational and trust the old NH4Cl could do something for me

 

[kurtak]

Hmmm - let's see if we can get back to solving Geo's problem - which is (first) the recovery of "all" the PGMs (including the Rh) from the 9 pounds of filter ash

It would be nice if it was as simple as leaching the ash - but it's not due to the difficulty of trying to dissolve the Rh out of the ash with wet chemistry

As we know - Rh (even finely divided) is resistant to AR --- for (complete) wet chem leaching of the Rh Chlorine or Bromine would be required - the problem there is keeping those elements in solution "long enough" for complete dissolution of the Rh - I believe the leach needs to be done under pressure or vacuum (don't remember which)

As a side note; - I am FAR from being an expert on all things PMG - what I do know is that wet chem dissolution of Rh is at best a difficult task

This brings us back to smelting for the recovery of the metals in the ash (including the Rh)

It has already been pointed out that silver is not a good collector for Rh

However - as Lino pointed out -----------

I agree that copper is more suitable

& as Lou pointed out in this thread -----------

How this is done industrially is with cryolite as the flux and fine chopped copper wire inside of a furnace you could drive a small truck into.

Note here; - cryolite is only needed in the flux when ceramics are involved as cryolite dissolves ceramic at "high" temp

So - IMO - (& if were me) smelting with copper is exactly what I would do to recover the metals (including the Rh) from this ash

As another note; - based on the report Geo posted - yes there is "some" silver in the ash - BUT - it is so very low (2.9 %) that it will have NO effect on the collection of the Rh - silver is only a problem (for the collection of Rh) when it (silver) is the predominant metal in the smelt

Once geo has recovered his metals from the ash by way of smelting with copper as his collector he should be able to get very near complete separation of the metals from his smelted dore with wet chemistry

So this is what I'm fighting.

Geo - IMO - smelting your ash with copper (as collector) is the first step in the recovery of the metals (including Rh) from your ash - once the metals are recovered (collected) from the ash we can go to wet chem separation on the dore

With proper ash/flux/copper ratios & proper flux ingredients you should be able to achieve 97 - 98 % recovery of your metals with your only real losses being small beads of metal that hang up in the slag of your "first" smelt pour - & those beads are recoverable

One more note; - you want your copper to be "fine" so it mixes in well with flux/ash for proper collection - as in "fine" chopped wire - or powder (clean copper cement would certainly work)

If you need help with ash/flux/copper ratios &/or flux ingredients let me know & I will be more then glad to help

Kurt

 

[orvi]

Hmmm - let's see if we can get back to solving Geo's problem - which is (first) the recovery of "all" the PGMs (including the Rh) from the 9 pounds of filter ash

It would be nice if it was as simple as leaching the ash - but it's not due to the difficulty of trying to dissolve the Rh out of the ash with wet chemistry

As we know - Rh (even finely divided) is resistant to AR --- for (complete) wet chem leaching of the Rh Chlorine or Bromine would be required - the problem there is keeping those elements in solution "long enough" for complete dissolution of the Rh - I believe the leach needs to be done under pressure or vacuum (don't remember which)

As a side note; - I am FAR from being an expert on all things PMG - what I do know is that wet chem dissolution of Rh is at best a difficult task

This brings us back to smelting for the recovery of the metals in the ash (including the Rh)

It has already been pointed out that silver is not a good collector for Rh

However - as Lino pointed out -----------



& as Lou pointed out in this thread -----------



Note here; - cryolite is only needed in the flux when ceramics are involved as cryolite dissolves ceramic at "high" temp

So - IMO - (& if were me) smelting with copper is exactly what I would do to recover the metals (including the Rh) from this ash

As another note; - based on the report Geo posted - yes there is "some" silver in the ash - BUT - it is so very low (2.9 %) that it will have NO effect on the collection of the Rh - silver is only a problem (for the collection of Rh) when it (silver) is the predominant metal in the smelt

Once geo has recovered his metals from the ash by way of smelting with copper as his collector he should be able to get very near complete separation of the metals from his smelted dore with wet chemistry



Geo - IMO - smelting your ash with copper (as collector) is the first step in the recovery of the metals (including Rh) from your ash - once the metals are recovered (collected) from the ash we can go to wet chem separation on the dore

With proper ash/flux/copper ratios & proper flux ingredients you should be able to achieve 97 - 98 % recovery of your metals with your only real losses being small beads of metal that hang up in the slag of your "first" smelt pour - & those beads are recoverable

One more note; - you want your copper to be "fine" so it mixes in well with flux/ash for proper collection - as in "fine" chopped wire - or powder (clean copper cement would certainly work)

If you need help with ash/flux/copper ratios &/or flux ingredients let me know & I will be more then glad to help

Kurt

I have experience with copper "inqartation" of PGMs (in my case 87%Pt 13% Rh to the final mass of 20% PGMs in copper). It alloys OK, drive past 1200°C and it is fine. Still copper-ish colour, but whitened considerably. Reaction with nitric is much more tame than plain copper. Dissolves very easily in nitric, but nitric also dissolve some platinum to the juice. But precipitate formed cannot be filtered easily.
When you have Cu dore with PGMs, it will be very easy to dissolve it in AR. Sponge produced from Cu inquart is extremely fine, particles so small that they refuse to settle completely even after one week, and were inert to my trials of efficient flocculation. So taking this and putting it straight to AR would bring Rh to solution relatively easily, i assume.

I can imagine next putting the copper bar into the bucket of AR solution (not sure if it is necessary to de-nox, since Rh form nitrito complexes... but these should be reduced also), aerate and precipitate the PGM cement. This could be workable for next chemistry, sponge could be dissolved in HCl/Cl2 and you have no salts in solution, evaporate chlorine and majority of HCl and you are prepared for Pt drop with NH4Cl - no NO complexes of Rh, no excess nitric, no excess of HCl (lower the solubility of not only ammonium Pt salts but also Pd and Rh ammonium salts).

 

[Geo]

Most of what was in the report is not a mystery to me as how it got in there. Zinc and iron is understandable as I have used both to cement with. Zinc turnings and steel wool. All the rest are found in electronics except for bismuth. I have never used it before and it's never been reported in any other metal I've recovered. Is bismuth in solder? If not, what components, if anyone knows, in electronics that contains bismuth?

 

[Justincase]

Idea is interesting. As organic chemist, I was more interested in chromatographic separation of these elements because it is stated in literature, and it works. However, not for hundreds of grams... But that ease of separation is so tempting - took a syringe with soluble complexes of the PGMs, inject them to the column of stationry phase, start pumping mobile phase (buffered water) and you separate individual PGMs salts as fractions. When you have transparent glass or plastic column, you can clearly see bands of different colours going down. If you get the mobile phase right, you get 99+% separation/purity.

With centrifugal separation, I have no idea how big the force must be to start moving up molecules eg in solution. I will need to calculate it... Also very clever idea - Pt is nearly twice as dense as Pd. So this separation could be accomplished more easily (I assume) than uranium isotopes. But I´m staying rational and trust the old NH4Cl could do something for me

The first part sounds more like the purification of LSD than any metallic use I can think of, very effective for small samples but not very scalable.
The second, even the engineering for a centrifugal concentrator is beyond most all but the best available engineers.
Once you take that concept down to the molecular level that is strictly governmentally controlled technology the same as Exploding Bridgewire and flash detonators.

 

[orvi]

Most of what was in the report is not a mystery to me as how it got in there. Zinc and iron is understandable as I have used both to cement with. Zinc turnings and steel wool. All the rest are found in electronics except for bismuth. I have never used it before and it's never been reported in any other metal I've recovered. Is bismuth in solder? If not, what components, if anyone knows, in electronics that contains bismuth?

Bismuth is found in some exotic solder mixtures, but not very often. Lead-free solders are practically pure tin with very small percentage of antimony, copper or silver. It is also used in thermal protection fuses - non-reversible ones, where an low melting alloy wire is used. Bismuth is sometimes in this composition. I bought bismuth once from Aliexpress for like 20 bucks a kilo (intended to use it as collector metal instead of lead). Very brittle and crystalline metal.

 

[snoman701]

The problem you will have is PGM refining is still very much a closed shop and not all refineries actually refine it but concentrate and pass onto one that does who can set their own terms as to returns and what they will pay for, nice for them bad for the small refiner.

I feel like it depends. Good for the small scale refiner, bad for the small scale collector / assay / seller

Agreed. Small scale business is vanishing, not only from PGM industry. Naturally or forcefully.
I was just upset when I heard our 2% Rh in material wouldn´t be paid. Knowing that they will certainly be paid for it, when sell to bigger refiner who actually refine the mixture. Straight rip-off.

Was it ever there in the PGM industry?

This volatility doesn't exactly help either. It's considerably harder to hedge small amounts that a little guy without a $1,000,000 bankroll can buy...the guys trying to hustle with $10,000 don't stand a chance, and the guy with $100,000 is going to struggle.

 

[Justincase]

I feel like it depends. Good for the small scale refiner, bad for the small scale collector / assay / seller


Was it ever there in the PGM industry?

This volatility doesn't exactly help either. It's considerably harder to hedge small amounts that a little guy without a $1,000,000 bankroll can buy...the guys trying to hustle with $10,000 don't stand a chance, and the guy with $100,000 is going to struggle.

You are only looking at the size of an operations float, that is free capital.
That is not the hardest part, The hardest part is the investment in facility and infrastructure that will let you turn over your float safely.

 

[snoman701]

Not necessarily. Being small can be quite the advantage. What is "safe" for a single man operation is negligence for an environment where you have employees. Mind you I am not talking about processing of Ru, Ir, Os....the only one of those worth chasing for a little guy is Ir, and you better be getting it free because the premiums on the sale are going to eat your profit quick.

The biggest setback is the cost of entry for analytics for the pgm's. Lou will tell you that the quantitative chemistry always wins, but you'll need ICP spectrometry for efficiency. You simply can't do it with AAS, and XRF is too inaccurate.

In Geo's case here, the first thing I'd do is send it out for a proper nickel sulfide fusion / assay to make sure he actually has the anticipated amount of Rhodium present and isn't chasing a $35,000 dream.