# Stumped by Stannous...



## CatGrl00 (Oct 3, 2022)

Trying to get the hang of reading my PGM stannous tests. Looking for any insight or opinions on these results to see if they match what I think. I know it's best to test on a swab or filter paper but I couldn't get a great pic that way. Any help is appreciated!


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## orvi (Oct 4, 2022)

Looks like PdPt in solution. What is the source of the liquid ? Is it acidic ? Does it contain base metals ? What is the original colur ?


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## 4metals (Oct 4, 2022)

What are the chunks in the test dish. Looks like you dropped your pop corn snack in! We need a few more details for a better answer.


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## orvi (Oct 5, 2022)

4metals said:


> What are the chunks in the test dish. Looks like you dropped your pop corn snack in! We need a few more details for a better answer.


I bet either silver chloride or solid stannous "crystals". But more probably AgCl. We will see what is what. 

As I do not know original colour, hard to say, but that colour combination I have seen numerous times - PtPd. As SnCl2 in solution is way more sensitive than XRF - we perform drop tests on regular basis.


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## CatGrl00 (Oct 6, 2022)

Thanks for the replies! haha, the "popcorn" is the salt not fully dissolved in the test dish, that I have been accumulating from boiling down my stock pot after multiple attempts at precipitating platinum palladium and hopefully rhodium from scrap catalytic converters. The liquid surrounding the salt is HCl. Trying to sort through the stock pot and separate the salts into Pt and Pd separately and trying to make sure I am reading my stannous tests accurately. I am hoping that I have boiled out majority of the base metals as removing them is the problem I seem to be running into the most. I appreciate the help and any suggestions for removing base metals is appreciated!


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## 4metals (Oct 6, 2022)

So you evaporated the values in a stock pot down to a crust and solvated that crust with some acid and tested with stannous? Did you cement out the values in the stock pot with copper first?


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## CatGrl00 (Oct 6, 2022)

yes, I boiled the stock pot down to a crust, added HCl to the dried crusts and tested with stannous. I have not cemented with copper, I have read mixed posts about whether or not to cement with copper vs zinc. I have tried zinc in the past but found I still ended up with base metals present in the PGM solution and was unable to successfully separate them. When I tested the crust with stannous after boiling down and adding HCl I did not see much indication of base metals, as far as I am aware, from what I have read, watched and tried.


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## Yggdrasil (Oct 7, 2022)

CatGrl00 said:


> yes, I boiled the stock pot down to a crust, added HCl to the dried crusts and tested with stannous. I have not cemented with copper, I have read mixed posts about whether or not to cement with copper vs zinc. I have tried zinc in the past but found I still ended up with base metals present in the PGM solution and was unable to successfully separate them. When I tested the crust with stannous after boiling down and adding HCl I did not see much indication of base metals, as far as I am aware, from what I have read, watched and tried.


Zinc will drop all metals.
You really need to use copper with strong agitation and heat.


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## CatGrl00 (Oct 7, 2022)

Thanks for the advice, I really appreciate it!! Once I drop the PGM metals with copper, then I should redissolve in AR (or just HCl maybe?)
and precipitate Pt with ammonium chloride and Pd with sodium chlorate as normal, correct? I've tried multiple times without successfully ending up with a high purity result and really want to get it right this time! I've read Hoke, many posts on this forum and other websites and I know I'm close but haven't quite gotten it just yet! Thank you for the help!


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## Yggdrasil (Oct 7, 2022)

I'm no master of the PGMs. 
But they are notoriously hard to separate completely.
One of the old ways is Bromate Hydrolysis which can separate quite good, but is quite laboriously and need meticulous control of pH and such.
DMG can be used to separate most of the Pd from the mix, but will need several rounds.
There are also solvent extraction routes that are quite effective.

There are more skilled members than me, to answer these questions, so lets hope they chime in.


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## CatGrl00 (Oct 7, 2022)

Thank you! If anyone else is willing to chime in, any tips or advice is greatly appreciated!


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## CatGrl00 (Oct 7, 2022)

Just found the "When in Doubt, Cement It Out" post, very helpful information! Yggdrasil thanks for mentioning the use of copper which led me to find that post! Definetly sounds like that may be the best method for what I am trying to do!


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## 4metals (Oct 7, 2022)

Please be aware that refining the PGM salts by dropping with Dimethylglyoxime and ammonium chloride will not yield metallic Platinum or Palladium. You have to (in addition to some purification steps) reduce the salts to metals at the end. Read up on platinosis. It is a serious and can be deadly bodily reaction from exposure to these salts. Be careful. 

If you are doing this purely as a hobbyist small scale chemistry project I understand wanting to get to the highest purity possible. But if this is a business venture, consider separating the metals as best as possible without exposing yourself to the salts and sell the relatively high purity metals to a refiner equipped to handle this.


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## CatGrl00 (Oct 7, 2022)

I am aware of all those things, safety is definitely a top priority for me, and I understand how to reduce the salts to metals, but I appreciate the thought! Not necessarily looking to make this a business venture, mainly want to prove I can do it!


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## orvi (Oct 7, 2022)

CatGrl00 said:


> Thanks for the advice, I really appreciate it!! Once I drop the PGM metals with copper, then I should redissolve in AR (or just HCl maybe?)
> and precipitate Pt with ammonium chloride and Pd with sodium chlorate as normal, correct? I've tried multiple times without successfully ending up with a high purity result and really want to get it right this time! I've read Hoke, many posts on this forum and other websites and I know I'm close but haven't quite gotten it just yet! Thank you for the help!


You would be best served with copper cementation. If you do the cementation rig as described in the post "When in doubt, cement it out", it will work well, but it really needs that bubbling. Agitation is helpful only to some extent.
If you do not have the capability to build one (which is I think very cheap setup with great performance), you can used powdered copper instead of the copper plate or bar. This time you will need good agitation to swirl the copper powder in the beaker well to let it react with PGMs in solution. This time, thick coating of PGM forms on the grains of copper dust particles, but as they have big surface area and aggresive mixing (best on magnetic stirrer) wil break that coating down and liberate fresh metal underneath. With copper dust cementation is usually done after half-hour or so. You can clearly see the copper catching black colouration. And with this procedure (Cu powder, not bar), you want to exclude air as much as possible. Otherwise your copper will quickly react with HCL and air, without doing it´s purpose.

Then you filter the Cu-PGM dust out. Be prepared for very fine particles, so filtration can be a bit tricky with ordinary coffee filters etc. But you can add some flocculent to coalesce the miniscule particles to agglomerates. Or Celite/Bentonite to contain them better, allowing easier - altough more lenghty - filtration. 

Also, be aware of a fact, that CuCl2 in solution can and will redissolve finely divided Pd and Pt back to the solution, if not enough fresh surface of copper is available. It is equilibrium reaction.


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## orvi (Oct 7, 2022)

CatGrl00 said:


> Thanks for the advice, I really appreciate it!! Once I drop the PGM metals with copper, then I should redissolve in AR (or just HCl maybe?)
> and precipitate Pt with ammonium chloride and Pd with sodium chlorate as normal, correct? I've tried multiple times without successfully ending up with a high purity result and really want to get it right this time! I've read Hoke, many posts on this forum and other websites and I know I'm close but haven't quite gotten it just yet! Thank you for the help!


Maybe I will slightly crush your expectations now, but refining PGM mixtures is hard. Literally hard, in amateur setup. Without fancy liquid extractants, expensive chemicals and most importantly lacking know-how.
From the conventional and well known separation techniques for PGMs, you usually don´t end up with 99+% pure metal/metal salt. Also, these precipitations/selective droppings aren´t complete. With NH4Cl, you will precipitate MOST of the platinum, but if you aim for higher purity, you need to use less NH4Cl - and thus impairing the yield. And from Pd containing solutions, you will always get contamined Pt salt.









 Pd Pt Rh mix industrial cat refining tips ?


Hi for a longer time, we have a quite complex problem sitting in our refining shop. Solution containing approx.: 34% Pd 9% Pt 2% Rh rest is base metals mainly Fe, Co, Ni, some trace Pb, no Ag nor Au. Metals are in form of chlorides in used up AR soln. Some nitric is certainly present. We aim to...




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read this whole thread. I tried many many experiments and conditions-altering things to separate PtPdRh mixture with aim of concentrating the Rh. You may find this useful 
Only precipitant which is quite selective from all "low-budget easy to use" alternatives is DMG. Altough working with higher quantities of it is hard -precipitate is voluminous and in bulk it practically need to be incinerated to get the metallic Pd - and this procedure leads to losses due to evaporation of complex. But for small scale it is sufficient and excellent Pd scavenger - in chloride enviroment you get quantitative recovery of Pd from solution. You can easily get 99% Pd from one DMG drop with thorough washing of the ppt.

Slightly more elaborate procedure for platinum is bromate hydrolysis. Also look it up here on the forum, post from 4metals. And study, understand the chemistry, and be well prepared that these compounds are very harmful to your health - and effects are scarry and irreversible, no cure to this day 

Minimize your contact with PGM to necessary minimum. Be safe.


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## CatGrl00 (Oct 7, 2022)

orvi said:


> You would be best served with copper cementation. If you do the cementation rig as described in the post "When in doubt, cement it out", it will work well, but it really needs that bubbling. Agitation is helpful only to some extent.
> If you do not have the capability to build one (which is I think very cheap setup with great performance), you can used powdered copper instead of the copper plate or bar. This time you will need good agitation to swirl the copper powder in the beaker well to let it react with PGMs in solution. This time, thick coating of PGM forms on the grains of copper dust particles, but as they have big surface area and aggresive mixing (best on magnetic stirrer) wil break that coating down and liberate fresh metal underneath. With copper dust cementation is usually done after half-hour or so. You can clearly see the copper catching black colouration. And with this procedure (Cu powder, not bar), you want to exclude air as much as possible. Otherwise your copper will quickly react with HCL and air, without doing it´s purpose.
> 
> Then you filter the Cu-PGM dust out. Be prepared for very fine particles, so filtration can be a bit tricky with ordinary coffee filters etc. But you can add some flocculent to coalesce the miniscule particles to agglomerates. Or Celite/Bentonite to contain them better, allowing easier - altough more lenghty - filtration.
> ...


Orvi- Thank you very much for taking the time to send this information to me, in both of your replies. I am grateful for the information you, as well as the other posters, have been willing to share. I also appreciate the concern for safety that is expressed here, I have read much about the dangers of doing this and am very careful!  
From the replies and information I have received I think I will give the copper cementation a try. Thanks everyone!


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## CatGrl00 (Oct 9, 2022)

orvi said:


> Maybe I will slightly crush your expectations now, but refining PGM mixtures is hard. Literally hard, in amateur setup. Without fancy liquid extractants, expensive chemicals and most importantly lacking know-how.
> From the conventional and well known separation techniques for PGMs, you usually don´t end up with 99+% pure metal/metal salt. Also, these precipitations/selective droppings aren´t complete. With NH4Cl, you will precipitate MOST of the platinum, but if you aim for higher purity, you need to use less NH4Cl - and thus impairing the yield. And from Pd containing solutions, you will always get contamined Pt salt.
> 
> 
> ...


Starting my copper cementation setup and attempt today. No expectations crushed here; I've learned this is much harder than it looks, but I've came quite far, learned a lot, and am not one who's willing to give up easily! Thanks again!


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## CatGrl00 (Oct 10, 2022)

First attempt cementing with copper...seemed like it worked, but also seemed like it happened a lot quicker than I thought it would. Test with stannous does read pt and pd, remaining solution is clear/very light green and not testing positive for any pgm's. Thoughts on how this looks and the best way to now easily and efficiently separate the pt and pd as much as possible? Redissolve in AR and precipitate with ammonium chloride and chlorine gas as I have in the past? Feel like I've learned a lot the last few days and don't want to mess it up now!


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## FrugalRefiner (Oct 10, 2022)

CatGrl00 said:


> Test with stannous does read pt and pd, remaining solution is clear/very light green and not testing positive for any pgm's.


I don't understand this. You say "stannous does read pt and pd,", but then that the solution is "not testing positive for any pgm's"

Please clarify this for us.

Dave


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## CatGrl00 (Oct 11, 2022)

The precipitate that came from the solution tests positive, the remaining solution does not.


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## Yggdrasil (Oct 11, 2022)

CatGrl00 said:


> The precipitate that came from the solution tests positive, the remaining solution does not.


Now I'm a bit confused, a precipitate do not test anything in Stannous.
When it is precipitated or cemented it is metallic powder and Stannous only reacts to ionic compounds aka salts.
So please can you elaborate a bit, I really do not understand how.


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## CatGrl00 (Oct 11, 2022)

I am honestly not sure...I have apparently done something quite wrong then because if I take what I thought I had cemented from the copper (as shown in the pic above), put it in the test plate with HCl and then stannous test it I get readings that look exactly like the colors for Pt and Pd. I will try again.


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## CatGrl00 (Oct 11, 2022)

I do have what looks likes metallic powder but there is also a yellowish powder attached with it that I was unsure of...maybe that is what the stannous is reading, although I tried to keep them separate.


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## Yggdrasil (Oct 11, 2022)

CatGrl00 said:


> I do have what looks likes metallic powder but there is also a yellowish powder attached with it that I was unsure of...maybe that is what the stannous is reading, although I tried to keep them separate.


Can you describe in detail how you did it?
I'm expecting that you used air bubbling or strong stirring in the solution before adding the Copper.
It should also preferably be hot, not boiling, but hot.


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## CatGrl00 (Oct 11, 2022)

I placed the salts I had previously obtained by boiling the stock pot down to a crust and put them into HCl, got it to boiling to dissolve them, lowered the heat a bit to stop the boiling but still kept the temperature hot. Then I added an aerator/bubbler (just a basic fish tank style) that sat above the bottom of the beaker but below the copper and let the solution stir for a few minutes before I added the copper. For the copper I used thick gauge wire in a bundle and placed it inside of a pvc pipe with holes drilled into it (similar to what I saw in the article "when in doubt, cement it out"). When I placed that into the HCl solution it immediately started bubbling and spinning around in the beaker. I let it go for about 45 minutes until I noticed the copper starting to dissolve and turn black. I then removed the copper, turned off the heat and let everything in the solution settle for about 4 hours until the solution looked clear/very pale green. Filtered the solution off and then dried the cement at the bottom of the beaker on low heat.


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## Yggdrasil (Oct 11, 2022)

CatGrl00 said:


> I placed the salts I had previously obtained by boiling the stock pot down to a crust and put them into HCl, got it to boiling to dissolve them, lowered the heat a bit to stop the boiling but still kept the temperature hot. Then I added an aerator/bubbler (just a basic fish tank style) that sat above the bottom of the beaker but below the copper and let the solution stir for a few minutes before I added the copper. For the copper I used thick gauge wire in a bundle and placed it inside of a pvc pipe with holes drilled into it (similar to what I saw in the article "when in doubt, cement it out"). When I placed that into the HCl solution it immediately started bubbling and spinning around in the beaker. I let it go for about 45 minutes until I noticed the copper starting to dissolve and turn black. I then removed the copper, turned off the heat and let everything in the solution settle for about 4 hours until the solution looked clear/very pale green. Filtered the solution off and then dried the cement at the bottom of the beaker on low heat.


You dissolved the metals in AR i guess?
There is no need to evaporate unless there is Nitric at play.
And it should not be evaporated to a crust, just syrup.
Actually evaporating to a crust may have negative effects, I can't remember why just now.
Add a bit of salt to avoid this.

The cementing part seem OK though, but again no need to evaporate all, then you will get all other dissolved salts too.
Just let it settle and pour off the surplus liquid.

Edit to add:
It is wise to siphon off with pipette or other method of suction to avoid loosing the cement which may be very fine.


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## CatGrl00 (Oct 11, 2022)

Evaporating to a crust was only when I boiled down the stock pot. When I did the cementing with copper, I did not evaporate any of it. Just filtered out the liquid. I am going to try another round with the copper and see what I end up with, but my question is once I have the PGM's cemented, would the best method be to dissolve the cemented value in nitric to remove any possible copper which should leave only the Pt and Pd (from what I've read neither of these should dissolve in the nitric) and then dissolve this into AR and to individually precipitate the Pt and Pd salts?

edited thought:
or maybe doing nitric alone first is a bit overkill as the copper would dissolve anyways if I put all of it straight into AR... just trying to remove everything unwanted as much as possible before attempting to precipitate individually again.

I appreciate you taking the time to help me out. I loved chemistry when I was in school, and it amazes me how much I seem to have forgotten since then.


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## Yggdrasil (Oct 11, 2022)

CatGrl00 said:


> Evaporating to a crust was only when I boiled down the stock pot. When I did the cementing with copper, I did not evaporate any of it. Just filtered out the liquid. I am going to try another round with the copper and see what I end up with, but my question is once I have the PGM's cemented, would the best method be to dissolve the cemented value in nitric to remove any possible copper which should leave only the Pt and Pd (from what I've read neither of these should dissolve in the nitric) and then dissolve this into AR and to individually precipitate the Pt and Pd salts?
> 
> edited thought:
> or maybe doing nitric alone first is a bit overkill as the copper would dissolve anyways if I put all of it straight into AR... just trying to remove everything unwanted as much as possible before attempting to precipitate individually again.
> ...


 A couple of things.
Pd dissolves in Nitric alone, and when Pd and Pt is intermingled, a significant amount of Pt will follow.
Dissolving Cu can be done with Ammonia or Copper Chloride etch.
The issue with the Copper Chloride aka AP etch is that some Pd may be dissolved in that too.
Why are you going to redissolve them in AR again when you already have them as Cement?
Separating them is at best tricky and lengthy if you need complete separation.

What is your plan with them?


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## CatGrl00 (Oct 11, 2022)

Thank you for the info...separating the platinum from palladium, as much as I can anyways, is my plan. Basically, long story short, my husband and I are mechanics and have accumulated around 15 catalytic converters. I've always had an interest in chemistry and have read a lot about people breaking them down into their separate PGM's and wanted to try it; my husband thinks there is no way it'll work. I'm trying to prove him wrong. If I am successful and can send them to a refinery for a few extra bucks, great, if I can't do it then my husband gets to say, "I told you so" and I'm trying to not let that happen ha-ha. I've come this far after many tries and would like to try my best to separate the Pt from Pd as much as I can which is where my plan for redissolving the cement into AR (now that the base metals are out, which was the problem I kept running into prior to all the help I've received on this forum) and reprecipitating the Pt and Pd individually, came from. If I can get them precipitated separately, or as much as I can, I have a pretty good understanding of calcining the salts into sponge. If I can get to that point, I will consider this experiment a great accomplishment.


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## Yggdrasil (Oct 11, 2022)

CatGrl00 said:


> Thank you for the info...separating the platinum from palladium, as much as I can anyways, is my plan. Basically, long story short, my husband and I are mechanics and have accumulated around 15 catalytic converters. I've always had an interest in chemistry and have read a lot about people breaking them down into their separate PGM's and wanted to try it; my husband thinks there is no way it'll work. I'm trying to prove him wrong. If I am successful and can send them to a refinery for a few extra bucks, great, if I can't do it then my husband gets to say, "I told you so" and I'm trying to not let that happen ha-ha. I've come this far after many tries and would like to try my best to separate the Pt from Pd as much as I can which is where my plan for redissolving the cement into AR (now that the base metals are out, which was the problem I kept running into prior to all the help I've received on this forum) and reprecipitating the Pt and Pd individually, came from. If I can get them precipitated separately, or as much as I can, I have a pretty good understanding of calcining the salts into sponge. If I can get to that point, I will consider this experiment a great accomplishment.


PS! Take care for your health working with PGM salts.

Catalytic converters should not have base metals, unless they are of the metal honeycomb version.
The powders from cementing might go easily into solution using HCl Peroxide, which will remove the need for evaporating.
If you can get your hands on some DMG(Dimethylglyoxime), it is quite selective for Pd.
There will be drag down of Pt but not too bad, and it can be repeated so the situation improves.
How about Rhodium in the Cats?


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## CatGrl00 (Oct 11, 2022)

They are all the honeycomb type. I had not thought of using HCl Peroxide, that might be a good way for me to go about it. I have tried DMG when I first started this project, but I think I had messed up several other steps leading me to believe I wasn't having luck with the DMG. I have read much more about it since then and I can't see the DMG having been the problem. I think I will try the HCl Peroxide solution and then try again using the DMG to precipitate the Pd. The rhodium is still a work in progress but is definitely on my list of things to figure out. I can't seem to find nearly as much definite information for the rhodium and so far, the times I've attempted to do anything with it, I've felt like I'm running in circles with no real progress made. 

Safety/health has been a priority for me when doing this experimenting. I've built a fume hood and scrubber in addition to always wearing a respirator, gloves, safety googles and keeping everything clean and organized! I know working with these materials isn't something to take lightly!


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## CatGrl00 (Oct 11, 2022)

What ratio would you recommend for the HCl & Peroxide?


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## Yggdrasil (Oct 11, 2022)

CatGrl00 said:


> They are all the honeycomb type. I had not thought of using HCl Peroxide, that might be a good way for me to go about it. I have tried DMG when I first started this project, but I think I had messed up several other steps leading me to believe I wasn't having luck with the DMG. I have read much more about it since then and I can't see the DMG having been the problem. I think I will try the HCl Peroxide solution and then try again using the DMG to precipitate the Pd. The rhodium is still a work in progress but is definitely on my list of things to figure out. I can't seem to find nearly as much definite information for the rhodium and so far, the times I've attempted to do anything with it, I've felt like I'm running in circles with no real progress made.
> 
> Safety/health has been a priority for me when doing this experimenting. I've built a fume hood and scrubber in addition to always wearing a respirator, gloves, safety googles and keeping everything clean and organized! I know working with these materials isn't something to take lightly!


Pt and Pd is like another continent comparing to Gold and Silver. Rhodium is then the other planet.
A lot less information and a lot harder to do. 
It is there though.

When doing ceramic honeycombs, just cement on Zinc. There should be no base metals to worry about.
But to get the most Rhodium one might need concentrated Sulphuric acid.
Orvi has a good thread where he discusses separation of Pd and Rh and his struggle to get it done to a sufficient purity so he could get paid for it.


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## Yggdrasil (Oct 11, 2022)

CatGrl00 said:


> What ratio would you recommend for the HCl & Peroxide?


I just use full strength HCl and add Peroxide as needed. My Peroxide was old 30%, so I guess it was around 15-20 for real. 
So I use Peroxide as I use Nitric.


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## CatGrl00 (Oct 11, 2022)

ok, thank you very much!! I believe Orvi sent me the post you are referring to in one of his responses to me earlier in this post! I greatly appreciate all of your advice today and throughout this posting! It has helped me a lot!


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## CatGrl00 (Oct 13, 2022)

Platinum precipitation seems to have been a success! Palladium is proving to be much more difficult...I don't currently have access to DMG so I am attempting to precipitate using sodium chlorate and chlorine granules (not at the same time, I've tried with each individually) but I continue to only precipitate a yellow crystal looking salt (last image, other images are the platinum) that isn't stannous testing positive for Pd, or anything else.


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## Yggdrasil (Oct 14, 2022)

CatGrl00 said:


> Platinum precipitation seems to have been a success! Palladium is proving to be much more difficult...I don't currently have access to DMG so I am attempting to precipitate using sodium chlorate and chlorine granules (not at the same time, I've tried with each individually) but I continue to only precipitate a yellow crystal looking salt (last image, other images are the platinum) that isn't stannous testing positive for Pd, or anything else.


I believe something is off somehow.
These images are a bit puzzling, can you describe each one a little bit.
The spot plate has a brown precipitate, can you try it on paper or cotton bud in stead?
The gray one, what is that?


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## CatGrl00 (Oct 14, 2022)

I'll try posting a pic with it on cotton or a paper filter, but usually I have a problem with it running everywhere and it's hard to see. the bit of precipitate is the piece of salt not fully dissolved in hcl when I added stannous. the gray is what the orange precipitated salt in the pics turned into upon heating. upon further heating this was my end result...


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## CatGrl00 (Oct 14, 2022)

the yellow salt was my attempt at precipitating the pd but didn't work, that salt is what I keep ending up with but it doesn't test positive for pd or anything else and i can't get the red palladium salt to precipitate. the solution to my best understanding is testing positive for pd. I'll post pics of that with the retake of my pt test on a filter paper in a bit.


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## Yggdrasil (Oct 14, 2022)

CatGrl00 said:


> I'll try posting a pic with it on cotton or a paper filter, but usually I have a problem with it running everywhere and it's hard to see. the bit of precipitate is the piece of salt not fully dissolved in hcl when I added stannous. the gray is what the orange precipitated salt in the pics turned into upon heating. upon further heating this was my end result...


It looks like nothing I have seen before.
The yellow salt should be fluffy and light.
Upon heating it should be completely dry and starts by giving up white smoke until it is a grey powder.
If the smoke gets dark you are loosing values.
Can you describe point by point what you have done to the yellowish salt is in the filter?


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## CatGrl00 (Oct 14, 2022)

I haven't done anything with the yellow crystals, as they didn't seem correct I still have them the way they are. That is this picture. 

after I precipitated the platinum using ammonium chloride, I reheated the remaining solution which tested positive for pd, brought it to a boil, let it cool, added more ammonium chloride and then added chlorine granules turned off the heat and let it sit overnight and this is what I ended up with.


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## CatGrl00 (Oct 14, 2022)

the platinum I precipitated is what I heated up. the pictures attached here show the stannous test (left is the salt dissolved in hcl and right is the same salt dissolved in hcl and then tested), the orange platinum salts I precipitated and dried. the Grey salt when I continued heating for hours on a low temp and the last pictures where it looks like grey/red rocks is when I put it under higher temperature and then stopped.


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## Yggdrasil (Oct 15, 2022)

CatGrl00 said:


> the platinum I precipitated is what I heated up. the pictures attached here show the stannous test (left is the salt dissolved in hcl and right is the same salt dissolved in hcl and then tested), the orange platinum salts I precipitated and dried. the Grey salt when I continued heating for hours on a low temp and the last pictures where it looks like grey/red rocks is when I put it under higher temperature and then stopped.


You have not told us much in details here, but many of your pictures do not look right.
Your stannous looks almost gelatinous. A picture on paper before and after would be nice.
The crystalline look of the orange salt looks strange (I don't have much experience with Pt salts) 
but it should have more homogeneous color and consistency I think.
How did you rinse them?
At what temperature did you heat it?


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