Ruthenium Impurity Removal (TBP or tetroxide)

[goldandsilver123]

I have a solution of Cr, Fe, Zn, Ni, Pt, Pd, Rh mixed with 0,2% of Ru (relative to total metal content), I want to extract the Ruthenium so it will not contaminate the other PGMs

It's concentrated HCl solution and there's no nitric present, it was dissolved in HCl / chlorate

Right now, I can say that I can safely distill RuO4, but I saw that in acidic chloride solutions there's no complete removal of Ru (with difficult formation of RuO4)

Anyone know if this solution neutralized will distill RuO4 with Chlorate addition to completion?

I've only seen sources of extraction o Ru in Nitric acid with TBP, will TBP extract Ru in chloride solutions (no nitric)?

 

[Yggdrasil]

I have a solution of Cr, Fe, Zn, Ni, Pt, Pd, Rh mixed with 0,2% of Ru (relative to total metal content), I want to extract the Ruthenium so it will not contaminate the other PGMs

It's concentrated HCl solution and there's no nitric present, it was dissolved in HCl / chlorate

Right now, I can say that I can safely distill RuO4, but I saw that in acidic chloride solutions there's no complete removal of Ru (with difficult formation of RuO4)

Anyone know if this solution neutralized will distill RuO4 with Chlorate addition to completion?

I've only seen sources of extraction o Ru in Nitric acid with TBP, will TBP extract Ru in chloride solutions (no nitric)?

Are you sure about this?
Here is from Gilchrist and Wichers:

Separation of Ruthenium by Distillation as Ruthenium
Tetroxide.-Place 150 ml. of diluted hydrochloric
acid (1 + 1 j, freshly saturated with sulfur dioxide, in the
first receiving flask and 50 ml. of the same reagent in each
of the other two flasks. Add 100 ml. of a filtered 10%
solution of sodium bromate through the thistle tube to the
distilling flask. This tube should be flushed with water
occasionally in order to remove any ruthenium tetroxide
which dissol.ves in the column of liquid held in the tube.
In order to maintain an excess of sulfur dioxide in the absorbing
solution, a saturated solution of sulfur dioxide in
water should be added from time to time through the
thistle tube situated between the first and second receiving
flasks. Pass a gentle current of air through the apparatus,
and heat the solution in the distilling flask to boiling.
Distil9 in this fashion for one and one-half hours. Add
25 ml. of the bromate solution, and continue to distil for an
additional hour.

 

[goldandsilver123]

I've read differently:

 

[Alondro]

RUTHENIUM!?! AHHHHHHHHHHHHHHHH!!!! (It does not play nice with anyone...)

 

[Darkthirty]

RUTHENIUM!?! AHHHHHHHHHHHHHHHH!!!! (It does not play nice with anyone...)

Ruthless is it?

 

[Yggdrasil]

I've read differently:

Which book is this by the way?
I need to read some more

Edit to remove uninformed comment.

 

[Yggdrasil]

I have a solution of Cr, Fe, Zn, Ni, Pt, Pd, Rh mixed with 0,2% of Ru (relative to total metal content), I want to extract the Ruthenium so it will not contaminate the other PGMs

It's concentrated HCl solution and there's no nitric present, it was dissolved in HCl / chlorate

Right now, I can say that I can safely distill RuO4, but I saw that in acidic chloride solutions there's no complete removal of Ru (with difficult formation of RuO4)

Anyone know if this solution neutralized will distill RuO4 with Chlorate addition to completion?

I've only seen sources of extraction o Ru in Nitric acid with TBP, will TBP extract Ru in chloride solutions (no nitric)?

If you reread the procedure you will see that the solution is of Sulfuric acid.
The HCl is used to drive off any Nitrogen Oxides left, in this case evaporate to syrup I guess, dissolve in water and add Sulfuric.
Again from the same Gilchrist and Wichers:

Preparation of the Solution.
Evaporate to dryness on the steam-bath the solution which remains in the distilling
flask after the elimination of osmium.
Add 5 to 10 ml. of hydrochloric acid and again evaporate.
Repeat the evaporation with hydrochloric acid until oxides of
nitrogen are no longer evolved.
Dissolve the residue from the last evaporation in about 20 to 30 ml. of water.
Add 10 ml. of sulfuric acid and evaporate the resulting solution
carefully until vapors of sulfuric acid are evolved.
Transfer the solution, and any residue of platinum which may
have separated, to the distilling flask that was used for the
distillation of osmium tetroxide.
Dilute the solution in the distilling flask to 100 ml. with water.

 

[Lou]

You can eventually get rid of it in an acid chloride solution. The base metals’ hydroxides don’t help things.

 

[goldandsilver123]

Which book is this by the way?
I need to read some more

Edit to remove uninformed comment.

A method for the separation of ruthenium from platinum , palladium, rhodium and iridium

by Raleigh Gilchrist

You can eventually get rid of it in an acid chloride solution. The base metals’ hydroxides don’t help things.

I did try TBP this time, slowly learning how to work with it. It did extract. Will try distilling the extracted aqueous phase.



For those not familiar with X-ray Spectrum. There's no Cd and Ag.

 

[Lou]

The sulfuric bromate works well but careful attention needs to be paid to removing all the chlorospecies. This means fuming it hard. Many times you get metallic Pt. The Pd can be separated as its iodide.