# Osmium, Iridium and dealing with toxics



## Adaptation (Jan 16, 2014)

I have some concentrate bound in SiO2 slag, thats not really the point here because I have a smallish sample that has been ultrasonically pulverised to almost a dust consistency so I'm hoping most of the cash is not bound in glass. 

I have read up on just about every source I could find about refining using acid. My plan is to dissolve out the non pgm's with sulfuric and later nitric acids in a two step wash to hopefully make collecting the silver easier. Then hit the PGM's and gold with AR and selectively pull out the gold with SO2 the Pt with NH4Cl. 

I have a small issue with the iridium, I just don't know if it will dissolve or not. It's 20.4% of my precious metal content. I will have a decent amount of SiO2 left so I can't just assume the andy remainder is iridium. If I get the go ahead to go full scale with the recovery I could use HF to wash the SiO2 out but at that point I could afford to hire a real chemist to help me. I may try to cook the crap out of it with AR or try to use density to separate it (panning or iridium anyone). 

On to the real question, I'm not finding much on osmium refining. I know this stuff is hella toxic and I have it in powder form that loves to turn into OsO4 great (-_-') I'm not a real chemist but I know it's supposed to be resistant to AR but I don't know when or how to kick it out of solution or if it will wash away as OsO4 with my early steps. It represents 13.4% of my precious metals. OsO4 melts at 40°c and boils at 130 so perhaps I should try to convert any elemental Os to OsO4 and distill it as a first step before I wash the non platinums out and later convert it to a metallic state. 

My non precious has 1% Pb, pritty sure I know how to kick that out of solution and I can sell it but it also has 1% As and I dont know how to kick that out or what to do with it once it's isolated. If I was smart enough perhaps I could make technical grade arsenic sulfides and sell them.

Sorry I drone on too much I really should learn to keep my questions few and simple.


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## nickvc (Jan 16, 2014)

It seems to me you have an ore concentrate which while containing values also has some very toxic elements in its makeup. Before any treatment I would fully check out any risks to you or anyone else and be prepared to contain such hazards and keep everyone safe. Many ores simply aren't a backyard proposition and I'd advise taking some professional help and advice before you do yourself or anyone else some harm. You don't sound a complete novice so I'm hoping you understand my concerns and while the osmium may have some value it's not widely used in industry so spending time and money to refine it may be a no go. Lou is our resident expert on PGMs so his view would be well worth having on this whole topic and I would follow any advice he cares to give.


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## Lou (Jan 16, 2014)

I'd advise forgetting about the whole thing. You're not working with something easy to work with, and really, given the materials, if you have to ask how to do it, you should not be doing it.

Hate to be a downer, but it's only (_potentially_) money--money that you might not enjoy if it sends you or worse yet, others to an early grave.

Save yourself a million dollars in frustration and stop with it.


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## g_axelsson (Jan 16, 2014)

OsO4 or osmium tetroxide is REALLY DANGEROUS! Yeah, I'm yelling, sometimes it's motivated.

OsO4 might have a melting point at 40°C but before that it sublimates , ie turn into gas. It is so volatile that it is delivered in glass ampoules that have been melted together. One major usage is in staining samples for electron microscope. The ampoule is broken inside a fume hood and just put beside the sample, the vapors is enough to do the job.
One of the major organs that OsO4 attacks is the eye, depositing osmium metal in the cornea, you lose your sight from metal that is covering your eyes! And if that isn't enough it can kill you if you inhale it even at a level that you don't smell it.

If you haven't realized it yet, one of the most scary chemicals I know of is osmium tetroxide.
http://en.wikipedia.org/wiki/Osmium_tetroxide#Safety_considerations

That arsenic you have is child's play in comparison.

Göran


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## Adaptation (Jan 16, 2014)

Yah it's bad but it's not the worst, I'm far more afraid of plutonium, polonium and HF but what scares me the most is Dimethylmercury I wouldn't touch that stuff if my life depended on it. OsO4 definitely bad stuff probably worse than hydrazine. I have a fume hood, face shield, pvc gloves, pvc apron and was considering a tyvek suit but I will add a respirator and goggles. I take safety seriously which is part of the reason I did not want to mess with HF just yet. 



> if you have to ask how to do it, you should not be doing it.


Don't really agree with that attitude, askling is one of the fastest ways to learn. Should or should not I'm going to try my best. I wish I had a glove box but I think I can be adequately safe with what I already have. 

I just don't know whether it's better to reduce it early on and process it with the rest of the AR (and would it stay reduced?) or intentionally oxidized it and process it out first. Or perhaps there is a superior method I am unaware of. I may like to forget about it but it is a major enough constituent that it must addressed somehow. 

Yes Göran I have read the wiki and other documents regarding it, I found osha's page on it most useful. 
http://www.cdc.gov/niosh/docs/81-123/pdfs/0473.pdf


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## FrugalRefiner (Jan 16, 2014)

Adaptation,

Since you've been here for less than half a day, I understand you don't yet know the people who have posted in response to your questions. I can't say I really know Göran's professional background, but he is very knowledgeable. nickvc spent many years as a professional refiner working for Johnson Matthey. Lou currently makes his living as a professional refiner specializing in the platinum metal group. If these men say you should forget about it, I would recommend following their advice.



Adaptation said:


> Lou said:
> 
> 
> > if you have to ask how to do it, you should not be doing it.
> ...


That only works if you follow the advice you're given. In this particular case, Lou is right. This isn't something you should be learning how to do from bits and pieces you read on the internet.

This forum is seven years old. There are nearly 200,000 posts on over 18,000 topics. There is a reason you won't find any information here about what you're proposing to do. If you have enough of this material to make it financially worthwhile, then you have enough of it to send it to a professional refiner.

Dave


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## nickvc (Jan 16, 2014)

Dave I did work for JM but my refining was all done with my own company and similar to Harold I learnt from scratch but without that wonderful book Hoke, I'm sure I lost some values by not having a full understanding but hey I made money from my endeavours.
I have learnt more here perhaps than in my time professionally refining certainly enough to spot things to avoid and definitely whose words you can count on as been as the final ones, with that comment in mind,as I previously said Lou will know the answers to the OPs questions and if it were me personally I certainly would take serious notice of his comments and advice, even if they were not what I wanted to hear.
Seriously Adaptation listen to Lou even if you don't listen to me, I know it sounds like we are killjoys but the reason is this material is seriously hard to recover let alone refine and with its toxicity problems it could do some serious damage if not processed correctly. This material is maybe fine for multi million dollar set ups with the correct emission controls and professional chemists but not in your back yard with a few buckets and beakers.


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## FrugalRefiner (Jan 16, 2014)

Nick,

Thanks for the clarification. I didn't know the exact details of your professional refining career, but I knew you had mentioned spending some time with JM.

Dave


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## Adaptation (Jan 16, 2014)

Well I guess what I will do is wash it in hot water a few times to start with and assume whatever is left is in metallic form and will come out the other pgm's at some point.


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## Lou (Jan 16, 2014)

Why don't you get a small sample, contact a reputable company that does such things, send it to them, work out terms, and save yourself a lot of trouble?

I will not give any suggestion on how other to do it than to contact a business that has the proper systems in place to manage the material.

Given the rarity of Os/Ir, there's more than a 99.9999% chance that what you have doesn't have those elements in significant enough amounts to even be valuable. You throw percentages out there, but how do you really know? Do you have a copy of the assay report? If so, how was it done?

Slow down.


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## Adaptation (Jan 16, 2014)

The assay was performed by total acid digestion followed by icp spectroscopy. It was performed on a few chunks of from a large pile which may not be homogenous. The values from the assay represent more than 3% of the total with Pt representing 35% of that. Very rich stuff and there is quite a bit of it. I looked into Johnson Matthey but for a number of personal reasons I don't wish to go that rout. I plan on doing a small scale operation to bootstrap a large scale one in the near future.


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## nickvc (Jan 16, 2014)

If one of the reasons was cost then I think that gives you another pointer to the difficulty of processing your ore, I'm sure they would be using the best available equipment with all the necessary environmental controls to process this material, another possibility for refining this may be Inco who are specialist PGM refiners but I expect turnaround times may well be months.
Please be very cautious if your going to try this, I still think your wrong and personally I wouldn't waste the time or take the risks involved especially after Lou said exactly that.


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## Harold_V (Jan 17, 2014)

Adaptation said:


> The values from the assay represent more than 3% of the total with Pt representing 35% of that.



And that doesn't send up a red flag for you?
I'm going to play the devil's advocate for a moment. 
You just told me that you have an ore that contains 306 ounces/ton platinum. 

Platinum is considered to be 1/10 as common as gold. To my knowledge, it isn't found in large percentages, with rare exception. And you happen to have over 300 ounces/ton?

What does a fire assay show?

If I've misunderstood what you've said, please correct me. 

Harold


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## Adaptation (Jan 17, 2014)

I did not say it was raw ore.


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## Harold_V (Jan 18, 2014)

Adaptation said:


> I did not say it was raw ore.


I stand corrected, and you have my apology.
Now, what does a fire assay show?

Harold


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## Platdigger (Jan 18, 2014)

So, is what you have slag from a smelting operation?
And, there was no fire assay, right?


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## g_axelsson (Jan 18, 2014)

FrugalRefiner said:


> I can't say I really know Göran's professional background, but he is very knowledgeable.


Thanks Dave!

I have a Master of Science degree in physics but read a lot of extra math, computer science and some chemistry, worked as an army telecom engineer and also with helicopters, I've run my own computer and electronics consultancy for a couple of years. Then ten years as a research engineer on the university and now I'm working for a small company that develops and sells measurement systems, doing all different things from electronic design to climbing 100 meter masts during service jobs.
Refining is a hobby just as the two electron microscopes I have, one SEM (450 kg) and one TEM (1800 kg). That way I've been introduced to osmium tetroxide as it is used as a stain for biological samples in electron microscopy. Other hobbies I have is mineral collection, coin collection and I'm collecting old computers.
... oh, and I love scrapping stuff.

Try to put a label on that! :mrgreen: 

/Göran


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## FrugalRefiner (Jan 18, 2014)

g_axelsson said:


> Try to put a label on that! :mrgreen:
> 
> /Göran


No problem. You're a renaissance man like many on this forum. 8) 

Dave


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## g_axelsson (Jan 18, 2014)

FrugalRefiner said:


> g_axelsson said:
> 
> 
> > Try to put a label on that! :mrgreen:
> ...


You got me there, that is in fact how I sometimes think of my self!
Probably why I like this forum so much.

8) 

Göran


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## royalrefiner (Mar 3, 2014)

I can tell you from experience that there are false readings of high amounts of iridium when there is sio2 present. Also, bismuth reads iridium on xrf if it isnt specifically calibrated for it. Also, if your sample is from a smelting operation and is not homogenous there is no reason to do anything until you have a proper assay. If Lou is telling you to forget it then forget it. I know he is very skilled and not to sound like one of his groupies but Im sure he could refine that material himself and if you can get that much pgm from that material why wouldnt you have a large refinery run it for you or ask someone on this forum to.do it or recommend someone. Anyway, I wish you well and if everything turns out good, you might be the next millionaire/billionaire, goodluck. Just remember, I could always use a donation if everything pans out!!!!!


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## Iridium chaser (Dec 26, 2018)

Well,as for SiO2 my own personal solution if it is present in anything that gets into my hands and contains enough precious metals will always be HF and nothing else in the world.However you must never apply it until you removed all the pnictogens including arsenic and bismuth or you will ruin your process and possibly end up dead in case you make it without proper protection but anyway you will have a sudden and vigorous reaction which will emit some of the most dangerous stuff in the world and turn all your material into a pile of toxic viscous and disgusting goup with all your PGMs converted into hell-knows-what from which even JM will have a hard time precipitating anything so even if you have the best chemical protection in this universe-you still have to deal with your pnictogen content first!
As for osmium tetraoxide yes,it's not a pleasant stuff but it is as for me quite a simple process to leach osmium:you can on opposite,put everything in one vessel,heat that up with applying the hot current of pure oxygen and so the only thing that you will leach will be pure osmium tetraoxide which you will have to condense somewhere and so you can further reduce it to osmium sponge with very little effort and to melt it down using either vacuum EAF or just with some really refractory flux like cryolite which however will also evaporate and even boil in the process but at the temperature above it's boiling point you will have your sponge already partially molten and also above the temperature range of osmium tetraoxide so it will decompose immediately upon forming so you will smelt everything in a bead and preferably cut the oxygen supply to the sample so it will not get oxidized upon cooling and so I did several times already..
Your real problem is presumably a bunch of pnictogens in your sample but there should be some process of leaching them out.


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## anachronism (Dec 26, 2018)

Assuming you're in a proper lab and not working in your back yard that's fine. Especially working with the acid that eats your bones, whilst juggling it with the chemical that make you blind. 

I guess that at least when you can't see enough you won't see the splashes of acid that melt the bones in your fingers. 

Don't make out it's easy working with this stuff. It isn't. There's people on here that shouldn't be trusted with hot water let alone this kind of stuff.


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## Iridium chaser (Dec 29, 2018)

It's anyway possible to design a quite primitive apparatus which will be completely sealed and also the reaction vessel made of for example titanium lined with tungsten like the entire apparatus and being one of two things that will be detachable so the general design would be simple as nail:the reaction vessel with welded pipe from which oxygen will come in,and the simple receiving vessel which will be cooled down with either liquid nitrogen or just with an ice bath:that's it!So just apply heat and pure oxygen while only holding the pressure with an outside supply-obviously without venting and therefore losing any oxygen so simply without any holes and so just you will start with your osmium bearing material and end up with the same material without any osmium left in the reaction vessel and all the pure osmium tetraoxide distilled into the receiving vessel which is obviously trivial to reduce after that by simply applying hydrogen gas and heating them both to get a beautiful osmium sponge under the water and that's it!However it is really pain in the b*tt to smelt osmium sponge even with vacuum arc furnace(I personally had never succeedaed smelting it less than in three times regardless of the weight)-and without one trying to smelt osmium sponge with any torch-like machine is actually only possible if it is made by serious people with serious chemical protection and made with a single purpose:to prove that they can-which is really an unlikely and very stupid thing for them because first of all the actual setup consisting of special custom torch preferably using for example pair of dicyan gas C2N2 and pure oxygen(insanely hot combination:it is burning at 4600°C+),also tanks,crucibles,fluxes,protection,upgraded fume hood preferably strong enough to pull somebody careless into it,and so on-which will most likely cost more than a proper vacuum EAF and also it is inevitable that at least some losses will occur always during this act of mocking over any logic and any common sense but it is anyway not something that you can do on the backyard ever!Especially with sponge:I noticed when I got an access to vacuum EAF and melted the osmium sponge that I extracted from various sources,there was always in the end some evidence of the fact that during melting all the remaining miniscule amount of oxygen in the melting chamber got completely and greedily mopped up by hot osmium so you are right that osmium is really not something that backyard refiners should process on their own-but if all the required precautions are cared about-that is actually a possible affair but it is really dangerous as probably no other naturally occurring element when it comes to smelting..
Yes and also about the ruthenium smelting:it is also a huge pain in the same place but not that huge as for osmium;I really once not too long ago had some sintered ruthenium pieces and I decided to smelt around one gram with a simple oxygen-mapp torch and I did that,but it was incredibly tedious and odious in fact much harder than smelting iridium metal even though it has the higher melting point it is vastly easier and unlike ruthenium it is completely safe to melt it down in any possible way which is almost the opposite thing for ruthenium but surprisingly the loss during melting of ruthenium was miserable and not more than 1-2% by weight..However still not for backyard refiners anyway!


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