rhodium sulfate to Rhodium

[lazersteve]

When a rhodium compound is heated in hydrogen the metal is obtained ; this is insoluble in aqua regia , but can be obtained in solution when it is fused with acid potassium sulphate . The fused mass on treatment with water yields a red solution , from which the metal is precipitated as a black powder on addition of caustic potash and alcohol .

Other routes include removing the sulfate as barium or calcium sulfate with the corresponding nitrate, then reducing the Rh nitrate after filtering out the insoluble sulfate.

And of course there is always zinc reduction if the sulfate is pure enough.

Steve

 

[NanoCat]

Found 2 videos series on Rhodium refining in Arabic. Good procedure. I always wondered about the white Rh salts and how to get em back. I lost a bunch last procedure because I couldn't get em to metal directly with Mg.
next

 

[lazersteve]

I have some completely neutral observations concerning these videos.
1) why contaminate relatively to nearly pure Rh flakes by running thru the processing shown and finishing up with Fe cementation? If all is taken at face value it's easy to see his starting material is purer than his "product"?
2) why perform all this chemistry when direct fusion with salt and sodium/potassium pyrosulfate will produce a more desired end product (ie higher purity). This "process" at the very least creates undue waste if ones goal is to refine Rh flakes.
3) why was there no testing of the presumed pregnant solutions to prove and follow Rh thru the process?
4) assuming all is "as advertised" the black powder will undoubtedly be impure owing to iron and other metals below iron in the activity series that are present in the steel alloy alone.
5) a complete disregard for all safety equipment, chemicals, and lab processes considered minimally acceptable even in basic chemistry classes.

I could go on, but I should caution anyone following these videos to at least consider the above 5 points as a bare minimum before jumping in and trying what is shown. There are plenty of great books, articles, and patents on processing Rh that I feel would be better sources on properly refining Rh.

Steve

 

[lazersteve]

TiCl3 is another method to precipitate Rh from solutions. Gilchrist covers this. It's not selective unless reaction conditions are carefully controlled. Additionally, there may be scaling issues depending on the solution concentration.

Steve

 

[lazersteve]

I will add these images concerning TiCl3 and its reactions with Rhodium solutions. Credit for my knowledge of this all goes to Gilchrist.

TiCl3 added to Solution positive for Rh at proper mixture as described by Gilchrist.

Settled solution after adding TiCl3. Rh is fine gray powder in test tube.

Various chloride solutions of Ti at different valences.

Freshly prepared TiCl3 solution used to directly precipitate Rh in first photo above.

Enjoy!

Steve

 

[lazersteve]

These are but a taste of the experiments that I have been working on while others are remaking outdated information and posting it on YouTube. In time I may be inclined to post more of the fruits of my adventures while experimenting and processing PGMs in my absence on the forum. While others were racking up YouTube subscribers and views I was educating myself in the centuries old knowledge of the founders of PGM chemistry. Suffice it to say that all that you see on YouTube is nothing short of regurgitation of another's knowledge, the true masters of PGMs lived centuries ago and credited all of their peers and sources around the globe. They did this all without internet.

Nothing short of amazing in my book and well deserving of a single line of accolades.

Yet I digress.

Steve

 

[Lou]

TiCl3 is another method to precipitate Rh from solutions. Gilchrist covers this. It's not selective unless reaction conditions are carefully controlled. Additionally, there may be scaling issues depending on the solution concentration.

Steve

We keep that around here and boy is that not stable in dilute solution!

It’s really on selective in Ir/Rh separations after the hydrolytic sep from Pt, extraction of Pd and of course, after Au/Ag removal.

 

[diego Henrique vilela]

good night steve how are you? about the founders of Pmgs techniques you refer to are: Hoke books ?? what other patents would they be? can you indicate links? books and websites ... would be very grateful .

 

[Lou]

These are but a taste of the experiments that I have been working on while others are remaking outdated information and posting it on YouTube. In time I may be inclined to post more of the fruits of my adventures while experimenting and processing PGMs in my absence on the forum. While others were racking up YouTube subscribers and views I was educating myself in the centuries old knowledge of the founders of PGM chemistry. Suffice it to say that all that you see on YouTube is nothing short of regurgitation of another's knowledge, the true masters of PGMs lived centuries ago and credited all of their peers and sources around the globe. They did this all without internet.

Nothing short of amazing in my book and well desering of a single line of accolades.

Yet I digress.

Steve

Steve, I’m glad that you have undertook this—this is exactly how I learned. Having met you I was immediately astonished by your scientific chops and willingness to learn the science. I for one look forward to hearing about your researches into this topic and would gladly share some of my own!

Thanks for coming back to us, you were definitely missed.

 

[Lou]

good night steve how are you? about the founders of Pmgs techniques you refer to are: Hoke books ?? what other patents would they be? can you indicate links? books and websites ... would be very grateful .

He’s talking about the likes of Berzelius, Smithson Tennant, Peyrone, George Matthey, Wollaston, Bishop, Deville and Debray, Moissan and the other giants upon whose the shoulders we stand.

 

[diego Henrique vilela]

He’s talking about the likes of Berzelius, Smithson Tennant, Peyrone, George Matthey, Wollaston, Bishop, Deville and Debray, Moissan and the other giants upon whose the shoulders we stand.

thank you for the quick response, is there any easy literature from these gods to help us?

 

[lazersteve]

Mostly anything prior to 1900...I believe 1886 was a monumental year if memory serves me correctly (I could be off a few years or so). So much information that was either ignored or brushed under the rug by modern science. German and French languages as well as some English so dust off your translators if you are serious about devoting the next 3-5 years of your life to learning the craft. Of course, there are some truly golden nuggets that occur in the early 1900 and later if you are willing to go down the rabbit hole of researching.
I refuse to spoon feed the creme de la creme of my learnings on an open forum as I know they will be monetized overnight which does no justice to the the men or the processes they pioneered. Scientific respect on YouTube channels is nearly non-existent in this day and age of the "look at me" and "make me rich" crowds. If it's not obvious by my tone, it nauseating to me.
Again, I digress.
Freechemist was the last of a rare breed in my honest opinion. Rest in peace my respected friend.

Steve

 

[billgold]

I also was wondering just what that person in the videos was attempting to accomplish.

Just from his lab "technique" alone, I would be inclined to ignore them.

 

[NanoCat]

Steve et al,
That Arabic video for me it was seeing the Rh come down as a white ppt. I had seen that many times before but could never get it to metallic Rh. And then how to work it back into a reducible solution with Sulfuric.
I got some Sodium Pyrosulfate but haven't done the fusion yet. Can I ask what your ratios for this one are? "direct fusion with salt and sodium/potassium pyrosulfate"
Thanks

 

[diego Henrique vilela]

you can always use 10:1 every gram of RH, 10 grams of sodium bisulfate.

 

[diego Henrique vilela]

Please friends, does anyone have a palladium bath formulation? Or could you point me to someone who has?

 

[Yggdrasil]

He’s talking about the likes of Berzelius, Smithson Tennant, Peyrone, George Matthey, Wollaston, Bishop, Deville and Debray, Moissan and the other giants upon whose the shoulders we stand.

As a curiosity, are there any one of these that are the best starting point on reading or is it a parallel study?

 

[lazersteve]

As a curiosity, are there any one of these that are the best starting point on reading or is it a parallel study?

Read anything you can find by Gilchrist and work your way backwards thru his references. Be sure you become familiar with all the reagents, protocols, and indicators he mentions. He is very specific in his work and details matter.

Steve

 

[lazersteve]

As a very specific side note related to PGM chemistry and reagents. Learn not only what "valence" means by definition, but also how to recognize and identify that you are working with the specific valence of solution or reagent that you "believe" you have. Simply using color references is not enough, you must be able to prove you are working with the proper valence with small scale tests before proceeding. Failure to do so will produce incorrect or incomplete results.
Also learn how to modify the valence of your PGM solutions and reagents if required.

Steve

 

[NanoCat]

Diego,
Please clarify this "you can always use 10:1 every gram of RH, 10 grams of sodium bisulfate." Raw Sodium bisulfate will work with sufficient heat or does it need to convert to the Pyrosulfate first?
thanks