# starting catalytic converter test with pics



## pgm (Dec 19, 2010)

hi

here is my test the last one for gold i did with everyone on the forum and everyone was very helpful....so i thought i might i do the same thing again for cat's

Ok i have taken 1 kilo of honeycome and crushed it then added it 3000ml beaker and added in 2liters of hcl and 0.5 liters of nitric

then i have placed it on a hot plate with a foil and sand to stop the thermal heat from breaking my beaker (i have broken 3 beakers but the sand should stop pyrex beaker from snapping) heated for 3 hours @ 80-100'C


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## rusty (Dec 19, 2010)

The procedure is right except he forgot to mention that it should be conducted using a FUME HOOD.


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## pgm (Dec 19, 2010)

rusty said:


> The procedure is right except he forgot to mention that it should be conducted using a FUME HOOD.



sorry my friend ohhh Dear rusty.....safty is a must i forgot you have already mentioned this twice to me.....people rusty is 110% correct be safe and use a fume hood......Thank you Rusty


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## pgm (Dec 19, 2010)

so i have now filtered the solution and i have a green colour solution not orange or red but green....more pics


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## lazersteve (Dec 19, 2010)

You are using way too much HCl and nitric. Try covering the comb in tap water then add enough AR (5:1 HCl:HNO3 muriatic:nitric) to dissolve about five grams of PGMs (25mL HCl : 5 mL HNO3). Double the amounts if you are processing cats from high end foreign model vehicles. I usually use more HCl than 5 times the nitric so the solution is a little more acidic. You can double or even triple the amount of HCl, *but not the nitric* and still get good results. 

Add the nitric in 1-2 mL additions at 60-90C and stop adding if you don't see any tiny bubbles coming from the material with each added dose. The crushed material has to be stirred also to expose the fine grains to the acid. You should notice the color of the solution darkening as the PGMs are extracted. Test periodically with stannous chloride and DMG to monitor the reaction progress.

Steve


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## pgm (Dec 19, 2010)

now i have done a stanous with i did this 2 time one was a light dip and the other was a big dip inside the pgm liquid

please wear gloves....safty first

more pics


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## lazersteve (Dec 19, 2010)

Looks positive, now you can use the same liquid to extract 20 more cats or you can evaporate it down after filtering it free of sediment to remove the 500 mL of nitric you used.

Steve


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## pgm (Dec 19, 2010)

lazersteve said:


> Looks positive, now you can use the same liquid to extract 20 more cats or you can evaporate it down after filtering it free of sediment to remove the 500 mL of nitric you used.
> 
> Steve



how much shall i evaporate....200ml of total liquid or when it becomes slug (thick)


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## lazersteve (Dec 19, 2010)

Evaporate to syrup like consistency then rehydrate (do not allow to dry out) with HCl. Repeat two more times or until no more brown fumes are seen.

Steve


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## pgm (Dec 19, 2010)

lazersteve said:


> Evaporate to syrup like consistency then rehydrate (do not allow to dry out) with HCl. Repeat two more times or until no more brown fumes are seen.
> 
> Steve



thankyou Steve for the info i will post more pic's when this is complete..


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## pgm (Dec 22, 2010)

ok i added the zinc and then i filtered...........i did a stanous test and no change but i think i added just a little too much zinc...but not sure...

so here are the pics these are when i think the zinc has done it's job and dropped out the pgm....


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## pgm (Dec 22, 2010)

ok these are the pics of the filtering....while i was filtering into another beaker...i took these...it looks like some reaction is still happening even after the stanous is showing no change in colour.....something is bubbling in the acid..

what do you think steve?


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## lazersteve (Dec 23, 2010)

Let the solution settle for several hours and see what color the liquid is. 

The mixed PGM powder will be on the bottom of the beaker.

zinc metal + muriatic acid = zinc chloride + hydrogen gas

Steve


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## pgm (Dec 23, 2010)

lazersteve said:


> Let the solution settle for several hours and see what color the liquid is.
> 
> The mixed PGM powder will be on the bottom of the beaker.
> 
> ...



Steve i have a black liquid with a tint of lime green ...now i have done a sharman filter and the liquid has gotten lighter but i can see at the end of every filter at the bottom some pgm still get's through the process.....i re filter after 5 hours and ther always is something at the bottom very fine but i can see it...

sorry i didn't get pic today but will take some tommarrow..

the first filter has pgm that dropped in it...this is black....the filter paper has also gone brown/orange where i have sprayed to the filter paper to move the pgm's down the filter paper...will take pic's to show again tommarow..

shall i dry the pgm in the filter......? i can then re AR the powder but this time use nitric 1ml at a time......i really wanted to follow the dvd.my fault too much nitric..got everything for it too...


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## pgm (Dec 24, 2010)

ok here are the pics of the filter.....last night i had put all the liquid into one big beaker and today i decanted into a another beaker and there is a thick black bottom layer this got through this filter....these are 6 coffee filters...the only other filter i have is wattmans 4 ashless filters.....i am going to try these next but this will take time 5.5cm filters.....i used these when i did gold filtering....it did the job...

or do i need another type of filter....?

any help is welcomed....


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## Barren Realms 007 (Dec 24, 2010)

You might want to try a charmin plug thru a funnel. And when you filter your solution if you still get material passing thru refilter with the same plug. As the plug gathers your PM's it will fill the voids that some of your material might be passing thru and recover more of your material. The filtering will get considerably slower but you will recover more of your material.


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## pgm (Dec 24, 2010)

Barren Realms 007 said:


> You might want to try a charmin plug thru a funnel. And when you filter your solution if you still get material passing thru refilter with the same plug. As the plug gathers your PM's it will fill the voids that some of your material might be passing thru and recover more of your material. The filtering will get considerably slower but you will recover more of your material.



thanks barren..... i will try this..... you think i should wash with hcl to wash away any zinc.....i was thinking of rinsing at the end with hcl....but not done it yet


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## Barren Realms 007 (Dec 24, 2010)

pgm said:


> Barren Realms 007 said:
> 
> 
> > You might want to try a charmin plug thru a funnel. And when you filter your solution if you still get material passing thru refilter with the same plug. As the plug gathers your PM's it will fill the voids that some of your material might be passing thru and recover more of your material. The filtering will get considerably slower but you will recover more of your material.
> ...



Steve or one of the other members could answer this better than I could. If you were working with just gold powder I would say yes. But with the material you are working with I am not 100% sure and don't want to lead you in the wrong direction.


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## pgm (Dec 24, 2010)

Barren Realms 007 said:


> pgm said:
> 
> 
> > Barren Realms 007 said:
> ...



i am waitng for steve to guide me..................i went wrong...i ended up added too much nitric.....i have done the process before but with aluminum but guessing was a major part of it............................so i decided to do a more controlled test......at the moment i have clean black powder this...i will only impove on this....but in the gold refine i have gotten pretty good...well i have improved 90% of my process....thanks for the reply


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## skippy (Dec 27, 2010)

Steve, does this very dilute approach require extended leaching times? In any case Neutralization would be a snap . 
I'll have to give it a try - do you think a nalgene (polypropylene) bottle would be suitable?



lazersteve said:


> You are using way too much HCl and nitric. Try covering the comb in tap water then add enough AR (5:1 HCl:HNO3 muriatic:nitric) to dissolve about five grams of PGMs (25mL HCl : 5 mL HNO3). Double the amounts if you are processing cats from high end foreign model vehicles. I usually use more HCl than 5 times the nitric so the solution is a little more acidic. You can double or even triple the amount of HCl, *but not the nitric* and still get good results.
> 
> Add the nitric in 1-2 mL additions at 60-90C and stop adding if you don't see any tiny bubbles coming from the material with each added dose. The crushed material has to be stirred also to expose the fine grains to the acid. You should notice the color of the solution darkening as the PGMs are extracted. Test periodically with stannous chloride and DMG to monitor the reaction progress.
> 
> Steve


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## lazersteve (Dec 27, 2010)

The leach times will be slightly longer due to the lower population of the nitrate ions in the solution.

Steve


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## pgm (Dec 27, 2010)

hi Steve..

well an update where i have got to.....i have filtered via a sharman plug but still the black powder was getting through so...i used a fine filter paper and then kept on filtering now the black liquid has changed to brown as i have kept on re-filtering and filtering time has gotten longer....i have 3 filters runing these are ashless filters...have pics


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## pgm (Dec 27, 2010)

ok here are some more pics....always had something at the bottom....and the powder well here it is


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## rusty (Dec 27, 2010)

From page 173 Hokes Refining Precious Metals Wastes.

While washing the powder into the filter paper, drop in
one or two crystals of sodium nitrate. (If washed with plain water,
this very fine powder will run through the paper; we add the sodium
nitrate and in some way it coagulates the fine powder and keeps it from
running through.


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## lazersteve (Dec 27, 2010)

First off I would not try to filter out that much sediment. I would advise you allow the sediment all to settle overnight before even considering any filtration. Once the sediment has completely settled, siphon off the top layer of transparent liquid. This liquid should be sediment free and can be processed directly as usual.

Once you are down to the last of the liquid with the bulk of the powder in it, filter the large particles out using Whatman filter disc or several coffee filters. These will not get the fine stuff, but will get the larger particles out.

Now pack the neck of a plastic or glass funnel with enough sheets of Charmin tissue to allow 1-3 drops per second of flow through. Test with water first to get the flow rate to 1-3 drops per second, once the flow is right pour in the liquid that has been through a course filtration first to remove the bulk of the sediment. After a few hours the 100% sediment free liquid will be in the collection flask and can be treated as usual.

Steve


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## rusty (Dec 27, 2010)

lazersteve said:


> First off I would not try to filter out that much sediment. I would advise you allow the sediment all to settle overnight before even considering any filtration. Once the sediment has completely settled, siphon off the top layer of transparent liquid. This liquid should be sediment free and can be processed directly as usual..
> 
> Once you are down to the last of the liquid with the bulk of the powder in it, filter the large particles out using Whatman filter disc or several coffee filters. These will not get the fine stuff, but will get the larger particles out.
> 
> ...



So adding sodium nitrate to enhance clumping as quoted from Hoke's book not a good idea, thanks for setting me straight on this Steve a fellow just never knows how far the art of refining has progressed since she wrote the book. I'm pleased to be advised of the new procedure.


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## lazersteve (Dec 28, 2010)

rusty said:


> ...
> So adding sodium nitrate to enhance clumping as quoted from Hoke's book not a good idea, thanks for setting me straight on this Steve a fellow just never knows how far the art of refining has progressed since she wrote the book. I'm pleased to be advised of the new procedure.



Gill,

You mistook my post, I'm offering an alternative to your suggestion, not a replacement.

I have never tried the procedure you recommend, so I can not personally attest as to whether or not it works. I have utilized the method I posted many times and it works fine for me. I would suggest that the reader try both methods on a small scale and use the one that work best for them.

Steve


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## pgm (Dec 28, 2010)

lazersteve said:


> rusty said:
> 
> 
> > ...
> ...



thanks just doing what you have said and it is working thankyou.....steve once i have the powder....what about any excess zinc....or should i not worry about this right now?.....or maybe i wash again with hcl only on the boil to clean the black powder...then filter again....


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## pgm (Dec 28, 2010)

rusty said:


> From page 173 Hokes Refining Precious Metals Wastes.
> 
> While washing the powder into the filter paper, drop in
> one or two crystals of sodium nitrate. (If washed with plain water,
> ...



How are you rusty....or shall i call you safty inspector...just joking....lol....thanks rusty....your a star

i will try adding sodium nitrate and do a test rusty......i will post what happens....i am doing a few leaches but learning and having plenty of fun at the same time


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## Oz (Dec 28, 2010)

Just thinking out loud, if you add a little sodium nitrate to HCl you will be making a weak AR. So the addition of sodium nitrate may just give the allusion of speeding the settling process, when it is in fact just re-digesting your fine particulates instead.

When I do converters I typically cement with zinc, and yes you can get a very fine particulate. I do not beat myself up trying to filter it though. I let the solution settle overnight after cementation is complete and then decant it to get the bulk of PGMs, Then I let the decanted solution set for 3 days to a week before I carefully siphon the solution away from the small amount of very fine values that settled.


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## rusty (Dec 28, 2010)

Oz said:


> Just thinking out loud, if you add a little sodium nitrate to HCl you will be making a weak AR. So the addition of sodium nitrate may just give the allusion of speeding the settling process, when it is in fact just re-digesting your fine particulates instead..



We've been taught to test all solutions with Stannous Chloride to assure they're barren before discarding. The idea of adding a couple of sodium nitrate crystals is not mine but came directly from within the pages of Hokes Refining Precious Metals.

Ms. Hoke claims that this method worked, given her expertise I would think that she would have tested here solutions before tossing.

How about it Harold do you have a comment on this procedure, your self taught in the art of refining using only Hokes Book as a guide along with some experimentation as your knowledge and confidence built to level to permit this.


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## Harold_V (Dec 29, 2010)

rusty said:


> How about it Harold do you have a comment on this procedure, your self taught in the art of refining using only Hokes Book as a guide along with some experimentation as your knowledge and confidence built to level to permit this.


The only comment I have is more of a question. Why in hell would ANYONE want to wash the precipitated gold to a filter? There is no good reason to do so----and it just complicates the finishing process of washing the gold. Even if it's already washed, there's no better place to dry the gold than in the container in which it was washed. A gentle heat applied will dry the gold perfectly well, causing it to clump to the point where there are no fine particles about which to worry. If it doesn't, the gold isn't very clean. 

When it comes to filtering, you have to know when to hold 'em, and know when to fold 'em. Anywhere in the process of washing, once gold is precipitated, is definitely not the time to do any filtering. The question is pointless. 

Harold


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## rusty (Dec 29, 2010)

Harold_V said:


> rusty said:
> 
> 
> > How about it Harold do you have a comment on this procedure, your self taught in the art of refining using only Hokes Book as a guide along with some experimentation as your knowledge and confidence built to level to permit this.
> ...



Ouch! Harold this discussion is about platinum - not gold. Ms Hoke says adding a couple of crystals of sodium nitrate helps in clumping the pt powders during the filtering precess. It all there on page 173 in black and white.

The only time I would consider using sodium nitrate with gold is during the smelting process.


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## Oz (Dec 29, 2010)

Rusty,

Well you caused me to check Hoke to see a bit more of the context of her comments, never a bad thing.

Did you notice that on that same page where Hoke is addressing “stock pot concentrates” and you took your note from, she starts off by clearly stating “First wash the black powder with unusual care to get rid of every trace of hydrochloric acid. Wash until the washings have no effect upon blue litmus paper”. If I am not mistaken we are still discussing the removal of cemented values from AR that has had the nitric consumed by the addition of zinc. In essence a hydrochloric acid solution.

She clearly understood what I was pointing out, and yes, always test waste solutions. Pay attention as well that she is talking about filtering a nitric acid wash by adding sodium nitrate crystals.

While Harold may have misspoke saying gold, his advice is accurate. For me, settling and then decanting/siphoning is the way to go. With gold it takes little time to settle, but I have had PGM zinc precipitations take 5 days. That kind of fine precipitate is not something I wish to filter or have to separate from the filter later. The more you manipulate values from one container to the next, the more opportunity you have for losses.

The fact remains that if you add a soluble nitrate to HCl you are making a form of AR. 

I am however sorry that it seems you felt I was criticizing you personally when it was obvious you were quoting someone else. I thought I was being rather casual in sharing my thoughts by saying “just thinking out loud”.


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## Harold_V (Dec 29, 2010)

Sorry about my less than appropriate response. I was in a hurry and back tracked only enough to get a hint of a clue (obviously I wasn't successful!) I definitely should have gone beyond, so I would have had a better understanding of the question. 

My apologies!  

However, I tend to stand by my comments. Once you have values in a vessel, there is generally little need to filter unless you are shooting for precipitation. My policy was to leave values in the container and siphon or pour solutions, with the exception of solutions that were filtered in preparation for precipitation. 

Any time you get a filter involved, you have the problem of material being trapped in the filter, plus the time it can take for filtration, which can be prolonged if the material being processed hasn't been treated well. It can be avoided by not filtering unless it's necessary. It often is not. 

If the discussion is revolving around platinum group values recovered from solution with zinc, nothing changes. I good wash with HCl, then several rinses, followed by a drying, much the same as with gold, is all that is required. Filtration is a waste of time and serves no real purpose. 

Harold


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## Harold_V (Dec 29, 2010)

Oz said:


> but I have had PGM zinc precipitations take 5 days.


Next time you have that experience, try boiling the solution with some added HCl. You may be pleasantly surprised that the solution clarifies and settle instantly. Excess zinc in solution tends to yield similar problems to aluminum in solution. 

Harold


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## Oz (Dec 29, 2010)

Harold_V said:


> Oz said:
> 
> 
> > but I have had PGM zinc precipitations take 5 days.
> ...


I have not processed converters for a while (I have a pile of them that need to be done though). I am a bit doubtful your solution will have much effect however as I do this hot and with excess HCl. Next time I do some I will try your suggestion just in case though. 

When running converter material I usually use HCl and Cl2. Using chlorine I do not have the problem of nitric removal. Beyond the Pd, Pt, and Rh, there are other elements present that also go into solution. I use a stir plate when cementing with zinc as it is critical all solution comes into contact with the metallic zinc. Right near the endpoint of cementation you get a queer greenish hue to the solution. Then all at once, no matter how fine or how little the zinc additions are the solution goes black. It is the very end reaction that makes the finest particulate. 

One of these days I should take my decanted solutions result of fine precipitate (not the main values, but only the finely divided and suspended values) and determine what percentage is PGM verses base metal cemented by the zinc. Purely speculating here, but I would think this last bit is Rh and base metal that gives the fine precipitate. 

Have you done zinc cementation of just Rh perchance where you could describe the reaction? I am thinking that perhaps the difference is that any PGMs you would typically have been cementing with zinc may well have had the base metals removed prior. It may be also that there are base metals in converters that are not typically found in karat or dental scrap. 

I would imagine Steve has seen what I am discussing. Perhaps he has tested the fine particulates from converter cementation further than I have.


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## pgm (Dec 29, 2010)

Harold_V said:


> Sorry about my less than appropriate response. I was in a hurry and back tracked only enough to get a hint of a clue (obviously I wasn't successful!) I definitely should have gone beyond, so I would have had a better understanding of the question.
> 
> My apologies!
> 
> ...



hi harold

the bit you say about the link between gold is what i was thinking.....thanks the more times i do this the simpler it gets...


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## jimdoc (Dec 29, 2010)

I have heard of some rare earth metals being used in converters,I will try to find the info to ad a link.

Jim

Cerium;

http://www.suite101.com/content/applications-of-the-rare-earth-elements-a186755

http://autocatalyst-recycling.umicore.com/catalyticConverter/


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## pgm (Dec 29, 2010)

jimdoc said:


> I have heard of some rare earth metals being used in converters,I will try to find the info to ad a link.
> 
> Jim
> 
> ...



i would be carful of umicore.....i rang them a few times,....never can get a straight answer from them......waste of time...i think based on my experience


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## kjavanb123 (Feb 9, 2011)

lazersteve said:


> You are using way too much HCl and nitric. Try covering the comb in tap water then add enough AR (5:1 HCl:HNO3 muriatic:nitric) to dissolve about five grams of PGMs (25mL HCl : 5 mL HNO3). Double the amounts if you are processing cats from high end foreign model vehicles. I usually use more HCl than 5 times the nitric so the solution is a little more acidic. You can double or even triple the amount of HCl, *but not the nitric* and still get good results.
> 
> Add the nitric in 1-2 mL additions at 60-90C and stop adding if you don't see any tiny bubbles coming from the material with each added dose. The crushed material has to be stirred also to expose the fine grains to the acid. You should notice the color of the solution darkening as the PGMs are extracted. Test periodically with stannous chloride and DMG to monitor the reaction progress.
> 
> Steve



Steve,

Is this ratio of acid good for honeycomb or just bead? I thought to extract Pt and Rh one needs more concentrated AR?

Thanks
Kev


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## lazersteve (Feb 9, 2011)

The ratio of HCl to HNO3 and the solution concentration are two different aspects of the reaction.

The ratio is the amount of each reagent that is in the solution with respect to one another, the concentration is the ratio of these reagents to the overall solution volume which is made up of water in aqueous reactions like AR.

The amount of water is what determines the concentration of the solution, the amounts of HCl and HNO3 determine the ratio of the reactants. With dilute solutions the ratio of HCl to HNO3 is the same as with concentrated solutions, the only difference between concentrated and dilute is the amount of water present.

Steve


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## kjavanb123 (Feb 9, 2011)

Opps,

Then I added way tooo much muratic to my honeycomb, almost 2liters of HCL and 400cc HNO3 added whilte HCL was heating. Let me get this straight, if I wanted to do this I would have used 2 liters of tap water, 50ml of HCL and 10mlHNO3?

Thanks
Kev


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## lazersteve (Feb 9, 2011)

I would split the water and HCl, using more HCl, less water, but the same nitric acid.

You can also use the same AR solution over and over again for several passes through several combs until the solution becomes saturated enough to warrant the clean up process.

So for your two liter scenario:

1000 mL of HCl, 100 mL of HNO3, 900 mL of water will do 10 cats processed one after the next in the same AR. Gentle heating is required. 

You'll find that HCl-Cl is more economical and can be just as effective if the reaction is driven properly (plenty of agitation/stirring). For the same scenario (2 Liter reaction) above you would have:
1000 mL HCl, 1000 mL H2O, NaClO added as needed in 25-50 mL increments with stirring to produce chlorine. 

Add more bleach only after the solution no longer fizzes when stirred, or until the color of the stannous test swab no longer get any darker after sitting for several hours. This reaction works fine in the cold as well as at warmer temperatures below 60C. I prefer to use it in the cold.

Steve


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## kjavanb123 (Feb 9, 2011)

Steve,
well noted, and very well explained. Once i finished processing 10 cats, I would like to donate 10 grams of PGMs to your site for your helpfull tips.
Thanks
Kev


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