# 4.5 cats recovery/refining pics



## kjavanb123 (Feb 27, 2011)

All,

Just recieved a free pack of 4.5 2-piece cats from a friend who trade this stuff, about 500-700 cats per weeks. French made, I dissolved them one by one in AR solution, 1500ml HCL + 500ml H2O + 150ml HNO3. heat it gently at first, then boiled it for last few mins, shaked each of them and rinsed them with boiling water back to the beaker before putting a new one in. I have done 4 combs so far, the solution looks almost dark, tested with stannous and you can see the result in pictures. how can i know the AR solution is saturated enough with PGMs and can't take anymore? Is there any sign? can i just dilute it with water, and add more combs? During processing this 4 combs, I would just add enough HCL to cover the entire comb. no extra nitric was added.

the load i began processing



1st one after almost an hour of gentle heating then boiling for last few mins.



2nd comb in same AR solution



4th comb in the same AR solution



stannous test result from the 4th comb AR solution. the left swap, the right part is from the first comb in AR solution.



Thanks and regards,
Kev


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## skippy (Feb 27, 2011)

I would think that rinsing back into the beaker is a bad idea - you will be hurting your AR strength, which is important for good dissolving. Keep the rinse separate. 

There's not going to be any sign that your solution is 'saturated' with PGMs There will be a point where it will become inefficient to use the same weakened leach. Ten combs works for Steve, so why not stick with that? 
You might eventually find it more efficient to use the same solution to leach more or less material, depending on how complete you want your extraction to be, whether you're going to do follow up leach/leaches, and likely a half a dozen other variables. There's no one complete answer to the question of how to leach catalytic comb. 

Also is that your kitchen? No one has ever accused me of being a worry wart, but the PGMs are dangerous, comparable to other heavy metals like lead or mercury. It's a seriously bad idea to be handling them where you prepare food.
Also I wonder about the effectiveness and long term consequences of using your fireplace as a fume hood! Don't be in such a rush that you damage your home and or health.


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## Lou (Feb 27, 2011)

Put a sand bath underneath that beaker if you must heat it with an open flame.

Also, as skippy said--do NOT do this anywhere near where food is done. I'm not going to help if that's the case--platinum and rhodium both are extremely poisonous. Remember how sick people get from things like cisplatin for chemo treatments? They're powerful skin sensitizers and can give you dermatitis that does not go away.

Your solution doesn't look that concentrated to me.


Lou


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## pgm (Feb 27, 2011)

i think for 4.5 cats you should have covered with water and then added hcl 125ml/250ml and HNO3 only 20ml or until there was no reaction....i am doing smilar amount and this is how i would do it...HNO3 is added in 1-2ml at a time and plenty of mixing...you only stop adding in HNO3 if there is no reaction.

How long are you leaching for? 5 hours / 7 hours

LOU and skippy are right about the RISK in work area. You have to be careful, money can not buy health. 

i have 3 systems running today and i have the same problem in loading the liquid with as much as possible. I was thinking of sticking with water to cover and then boil down the liquid. so i will have a beaker which is always on boil down and each time i leach it is a new batch of acid less acid. this gives me a big problem with lot's of liquid...

i dont know but does anyone know how long does a boil down take say 10 liters 1000kw hotplate ?


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## kjavanb123 (Feb 27, 2011)

All,
Thanks for your concerns, but this is a vacant apt that no one lives in, plus I do have a filtered mask, and goggles, so I barely smell or feel any of the smokes coming out. and no one will be moving in anytime, soon, plus this is just temp place for my testing, once i finish with this cats, i am moving to a small lab with all the fume handling equipments installed.
pgm,
I followed Steve's recipe for AR, but instead of 1000ml water, i added only 500ml, 1500ml hcl and 150ml of hno3 added when hcl + water was added and heated. i stopped adding HNO3 for the next combs. Just HCL was added to cover the comb. for the first comb, I heated gently for 1.5 hrs, for the 2nd one i heated for 1hr then boiled it for 20mins, and boiled 3rd and 4th for half of an hour. in Steve's DVD in part he dissolves the mixed black powder in AR, he heat gently at first, then boil it later, all in half and hour range, if i remember correctly, that was 8.8g of PGMs. So maybe less time to boil for each comb is needed.
Thanks
Kev


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## jimdoc (Feb 27, 2011)

kjavanb123 said:


> All,
> Thanks for your concerns, but this is a vacant apt that no one lives in, plus I do have a filtered mask, and goggles, so I barely smell or feel any of the smokes coming out. and no one will be moving in anytime, soon, plus this is just temp place for my testing, once i finish with this cats, i am moving to a small lab with all the fume handling equipments installed.



You could be doing serious damage to the apt. Acids can ruin the wiring and cause fire hazards as well as the other obvious effects of acids. I wouldn't be doing that in anybody's apartment vacant or not. I would find a shed or garage.

Jim


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## kjavanb123 (Feb 27, 2011)

This is more like an abandoned apt, which will be renovated from ground up, believe me, it will be no harm to this place, plus when heating the AR, i put a glass led on it, so it won't produce much smoke. I will post more pics today. 

Kev


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## kjavanb123 (Feb 28, 2011)

ok this is getting soo annoying, I tried to rinsed and clean the mixed PGMs powder from 4 combs today, and i don't know what happened. here is what i did in picture. After zinc percipitation, i tried to clean and decant the remaining black powder with boiling water 3x. as you can see from the pic below.



then i went ahead and added NaOH, stirred it, and added some more boiling water to it, stirred, and i got this flufy looking powder like piece of shredded paper in water... ?!?! what is this? can i proceed or did i somehow lose most of the black powder clinged to the NaOH with zinc?!


and



I can't believe i am stuck in such basic stuff, I went from A-Z and now i am back to square one again. 

Kev


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## pgm (Feb 28, 2011)

kjavanb123 said:


> All,
> Thanks for your concerns, but this is a vacant apt that no one lives in, plus I do have a filtered mask, and goggles, so I barely smell or feel any of the smokes coming out. and no one will be moving in anytime, soon, plus this is just temp place for my testing, once i finish with this cats, i am moving to a small lab with all the fume handling equipments installed.
> pgm,
> I followed Steve's recipe for AR, but instead of 1000ml water, i added only 500ml, 1500ml hcl and 150ml of hno3 added when hcl + water was added and heated. i stopped adding HNO3 for the next combs. Just HCL was added to cover the comb. for the first comb, I heated gently for 1.5 hrs, for the 2nd one i heated for 1hr then boiled it for 20mins, and boiled 3rd and 4th for half of an hour. in Steve's DVD in part he dissolves the mixed black powder in AR, he heat gently at first, then boil it later, all in half and hour range, if i remember correctly, that was 8.8g of PGMs. So maybe less time to boil for each comb is needed.
> ...



Steve has been doing this for a long time and has a very good understanding, older and wiser....You sound like in a hurry...like a man with a car and no control over the brakes....Slow down and start to think and relax and it will all be OK....i think you should leach for 6-8 hours and mix every 30 minutes this should make sure whatever is inside comes out. You should be doing this everytime..i bet if you re-leach again you will get more pgm..forget about getting 8.8g for now....in a few months/years you will be ready to get that much out but not today....baby steps....


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## kjavanb123 (Feb 28, 2011)

pgm,

I am not in a rush, just lil frustrated as for zinc percipitation got messed up after i added NaOH, i am guessing now, that i should have made a 20% NaOH solution and rinsed the black powder with that. 

in Steve's DVD, when he was processing the beads, he uses dilute AR, and run it for 3hrs almost, later in that section he mentions the Pt on beads can be extracted fully with concentrated AR. so i presumed from this, for combs, i gotta use concentrated AR that way both Pd and Pt can be extracted the same time.

You mentioned 6-8hrs is that for one honeycomb or 4 of them?

Thanks
Kev


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## pgm (Feb 28, 2011)

kjavanb123 said:


> pgm,
> 
> I am not in a rush, just lil frustrated as for zinc percipitation got messed up after i added NaOH, i am guessing now, that i should have made a 20% NaOH solution and rinsed the black powder with that.
> 
> ...



honeycomes....i have tested....you do the test and you will learn alot more....


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## lazersteve (Feb 28, 2011)

Kev,

PGM is right on the money. You keep making mistakes because you are not following the directions to the letter. For example, in the above photo you added dry NaOH instead of 20% solution as Lou dictated. 

Rome was not built in a day, stop jumping between processes and follow one process through from the beginning to the end. Stop trying to shortcut to the end. If you have to leach twice or three times to you get all the PGMs then you are doing fine. Don't try to double guess the reactions, follow through with each step. If you don't see the same reaction as what myself and others are getting, simply stop and ask.

I've also noticed you mentioned urea in another thread. Please don't add urea into the mix of chemicals you are dealing with, it's only going to make your problems worse. 

You need to *process a single cat* from start to finish, with multiple extraction cycles (if required) to get the yield numbers for your French made cats. Make that your first goal. Don't worry over the Rh, if it's there, it's not going anywhere. Besides if you don't learn the basic PGMs like Pd and Pt you won't succeed at processing Rh.

This may put things in perspective for you:

I spent a year and a half learning and filming the Fundamental of Pt and Pd DVD. I made many mistakes along the way, but only after processing known samples of Pd, Pt, and Rh in test tubes, was I able to successfully process PGMs from cats. Since making the DVD I have continued to research and find new ways to process the same material. With the help of others and a lot of patience I have been able to become proficient at refining PGMs. Refining PGMs is not like making a cake, it's more like an art all to itself.

Are you keeping a lab notebook with your reaction times, masses of chemicals used, etc?

Steve


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## kjavanb123 (Feb 28, 2011)

Steve,

I learned my mistake in lye addition, that is why i only tried 4 combs, so i don't repeat them with next set of 4 combs. I already tried with one honeycomb, and believed i got it fully. So i scaled up lil to get better yield and be able to melt it easily.

I just can't stop thinking about alternative methods sometimes. for instance for Pd. why can't we just digest each of the honeycombs in nitric acid first, from what i learned so far, that should dissolve all the Pd and base elements like iron etc? it won't touch the Pt and Rh. 
Also concentrated sulfuric leach after that to take care of Rh. I mean pricewise, i think doing these 2 leaches separately won't be much diff than combine price of HCL and Nitric acid.

I haven't done it but has been keeping my mind busy since yesterday.

Thanks
Kev


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## lazersteve (Feb 28, 2011)

Leaching the Pd from the combs directly in dilute nitric may not be a bad idea if you have good fume controls and plenty of cheap nitric. You still need to control your nitric additions and deal with the large volumes of solution once the Pd is in solution. 

Using large volumes of boiling concentrated sulfuric acid is not an easy task to accomplish, not to mention it is extremely dangerous. 

In my mind it's much more economical and safe to use a cheap method (eg: HCl-Cl) of recovery of the PGMs then zinc them all out together and separate on a small scale. This saves reagents and produces less waste in the long run. I for one don't want to be handling large volumes of pregnant nitric acid or concentrated sulfuric acid, these chemicals are scary enough when handled on a small lab scale.

You are trying to recover and refine in one step. It's not too often you can safely, economically, and successfully do that with scrap of any type.

If you choose to combine steps and try to accomplish everything in one 'fell swoop', you should at the very least get your lab in order and have the proper safety measures in place. It's not a matter of if an accidental spill will occur, it's a matter of when. On a lab scale you can contain accidents easier than on an industrial scale.

My preference has always been to recover first then refine.

Steve


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## skippy (Mar 1, 2011)

I agree with Steve on the difficulty of using sulfuric acid for extraction. A good percentage of the cat itself dissolves in the hot sulfuric, which means high consumption of the acid. The dissolving reaction produces water, which has to be removed from your sulfuric to keep the action strong. Bulk sulfuric is cheap, but I think you would be further ahead working to achieve good Rh extraction in an AR or HCl/Cl2 solution.


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## kjavanb123 (Mar 1, 2011)

Steve,
Thanks for the input, I was thinking the method theoritically speaking. I am sure with your experience in this field, i don't wanna re-invent the wheels. Back to this refining experience, specially with my last 4 honeycombs, i filtered the AR leach and this morning i noticed a gray mud in the filter paper, and this is from AR leaching part, i haven't tested it but it looks like Rh salt, this is first time i see Rh from AR leaching. I thought they come from dissolving the mixed black powder in AR. How is that possible? Here is the picture of rinsed what it seems to be Rh salt.




Thanks
Kev


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## skippy (Mar 1, 2011)

This is the result of of filtering your leach? No neutralization or precipitations? It's extremely unlikely (read that impossible) that you freed up the rhodium from the cat and that it then nicely dropped into your filter. The gray mud is most likely dust from the surface of your converter. If you ground up your catalytic converter real fine you would find a heck a lot of that grey mud, and it still wouldn't be Rhodium  

If you had grey rhodium powder it wouldn't be a salt, it would be metallic rhodium.


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## skippy (Mar 1, 2011)

There's microscopically fine metal locked in that ceramic, and it's gotta dissolve out and then you have to precipitate it. It doesn't wind up in your filter just because.

I know a lot of people here say that refining is more technical than academic,
but I think not having the knowledge to understand the difference between a salt and a metal http://en.wikipedia.org/wiki/Salt_(chemistry)
is going to be a real impairment, especially if you want to do PGM work, and especially if you are trying to develop your own technique of doing PGM work!
Not trying to slight you Kev, that's just how I see it. Keep on working on this stuff by all means, and keep on asking questions, I just think you would be ultimately putting yourself way
ahead by getting at least the most basic chemical knowledge.


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## kjavanb123 (Mar 1, 2011)

Skippy,

I came to PGM refining with no chemistry background, it was help and tips from Steve, Lou, and the rest of helpfull members here who got me to finally produce the Pd, Rh in metallic form. I refered to gray mud as Rh salt since last time I dissolved my black powder in AR and I got the same residue as you in the picture. I haven't tested the gray mud in the beaker with anything just by look of it i was wondering how did it get there at such earily stage if it was Rhodium.

Thanks
Kev


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## pgm (Mar 1, 2011)

kjavanb123 said:


> Skippy,
> 
> I came to PGM refining with no chemistry background, it was help and tips from Steve, Lou, and the rest of helpfull members here who got me to finally produce the Pd, Rh in metallic form. I refered to gray mud as Rh salt since last time I dissolved my black powder in AR and I got the same residue as you in the picture. I haven't tested the gray mud in the beaker with anything just by look of it i was wondering how did it get there at such earily stage if it was Rhodium.
> 
> ...



Like steve has said MASTER 1 CAT - Just ONE - then move onto 4 or 5....i think you will learn how to do the process but at what cost i dont know....if you have not had an accident with chemicals you are very lucky but it will happen sooner or later....it happens to the best of us.

i have made a flow chart and this helps me to asses my postion....i never try to do the whole process in one go....you should think about this....We all make mistakes but you can learn and master them...


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