Method for separation of chemically pure Os from metal mixtures

Patent metadata

Field	Value
Publication number	US-9528169-B2
Application number	US-201414336767-A
Country	US
Kind code	B2
Filing date	Jul 21, 2014
Priority date	Aug 3, 2011
Publication date	Dec 27, 2016
Grant date	Dec 27, 2016

Abstract

A method for separating an amount of osmium from a mixture containing the osmium and at least one other additional metal is provided. In particular, method for forming and trapping OsO 4 to separate the osmium from a mixture containing the osmium and at least one other additional metal is provided.

First claim

What is claimed is:

1. A method of separating an amount of osmium from a mixture comprising the amount of osmium and at least one additional metal, the method comprising:
contacting the mixture with an oxidizing solution to form a volatile OsO 4 vapor;
bubbling the OsO 4 vapor through a KOH trapping solution to form an amount of K 2 [OsO 4 (OH) 2 ] dissolved in the KOH trapping solution;
contacting the dissolved K 2 [OsO 4 (OH) 2 ] with a reducing agent to form an Os precipitate; and
separating the Os precipitate from the KOH trapping solution, wherein the mixture is an irradiated osmium metal target comprising at least one osmium isotope selected from the group consisting of Os-184, Os-186, Os-187, Os-188, Os-189, Os-190, and Os-192.

2. The method of claim 1 , wherein:
the mixture is an irradiated osmium metal target comprising at least one of Os-189, or Os-192; and
the at least one additional metal comprises at least one of Re-186, Ir-186, Ir-187, Ir-188, or Ir-190.

3. A method of separating an amount of osmium from a mixture comprising the amount of osmium and at least one additional metal, comprising:
contacting the mixture with an aqueous solution of NaClO at a concentration of about 12% w/v available chlorine to form a volatile OsO 4 vapor;
bubbling the OsO 4 vapor through a trapping solution comprising an aqueous solution of KOH at a concentration of about 25% w/v to form an amount of dissolved K 2 [OsO 4 (OH) 2 ];
contacting the dissolved K 2 [OsO 4 (OH) 2 ] with an aqueous solution of NaHS at a concentration of about 10% w/v to form an OsS 2 precipitate;
washing the OsS 2 precipitate by agitating with water;
separating the OsS 2 precipitate from the KOH trapping solution by centrifuging;
rinsing the OsS 2 precipitate with acetone; and
drying the OsS 2 precipitate;
wherein the mixture is an irradiated osmium metal target comprising at least one osmium isotope selected from the group consisting of Os-184, Os-186, Os-187, Os-188, Os-189, Os-190, and Os-192.

4. The method of claim 3 , wherein:
the mixture is an irradiated osmium metal target comprising at least one of Os-189, or Os-192; and
the at least one additional metal comprises at least one of Re-186, Ir-186, Ir-187, Ir-188, or Ir-190.

5. A method of separating an amount of osmium from a mixture comprising the amount of osmium and at least one additional metal, the method comprising:
a. contacting the mixture with an oxidizing solution to form a volatile OsO 4 vapor;
b. bubbling the OsO 4 vapor through a KOH trapping solution to form an amount of K 2 [OsO 4 (OH) 2 ] dissolved in the KOH trapping solution;
c. contacting the dissolved K 2 [OsO 4 (OH) 2 ] with a reducing agent to form an Os precipitate; and
d. separating the Os precipitate from the KOH trapping solution,
wherein the oxidizing solution comprises an aqueous solution of an oxidizing agent chosen from NaClO, LiClO, KClO, NalO 4 , Na 2 S 4 O 8 , XeO 3 , NaClO 2 , NaClO 3 , NaClO 4 , NaOH in contact with Cl 2 gas, alkali salts of ClO, ClO 2 , ClO 3 and ClO 4 , or combinations thereof.

6. The method of claim 5 , wherein the mixture is an irradiated Os-190 metal target, the amount of osmium comprises an amount of Os-191, and the at least one additional metal is chosen from Ir-192, Ir-193, Ir-194, Pt-192, Pt-194, or combinations thereof.

7. The method of claim 5 , wherein the oxidizing solution is an aqueous solution of NaClO at a concentration of about 12% w/v available chlorine.

8. The method of claim 7 , wherein the mixture is contacted with the oxidizing solution in an impinger device.

9. The method of claim 7 , wherein the mixture is contacted with the oxidizing solution at a temperature of about 40° C. until the mixture is dissolved, and the dissolved mixture is contacted with the oxidizing solution at a temperature of about 90° C.

10. The method of claim 5 , wherein the KOH trapping solution comprises an aqueous solution of KOH at a concentration of about 25% w/v.

11. The method of claim 10 , wherein the KOH trapping solution is maintained at a temperature of less than about 5° C.

12. The method of claim 5 , wherein the reducing agent is chosen from absolute ethanol, Zn shavings, Al shavings, Mg shavings, NaBH 4 , NaHS, H 2 S gas, Na 2 S 2 O 3 , UV light, phosphine ligands, hydrazine, hydroquinone, hydrophosphorous acid, formaldehyde, hydroxylamine, or citrate.

13. The method of claim 12 , wherein the reducing agent is absolute ethanol at a concentration of 5% v/v and the Os precipitate is K 2 [OsO 2 (OH) 4 ].

14. The method of claim 12 , wherein the reducing agent is a mixture of Zn shavings and Al shavings, and the Os precipitate is Os metal.

15. The method of claim 12 , wherein the reducing agent is chosen from Zn shavings, Mg shavings, or Al shavings, the reducing agent is contacted with the dissolved K 2 [OsO 4 (OH) 2 ] in combination with HCl, and the Os precipitate is Os metal.

16. The method of claim 12 , wherein the reducing agent is NaBH 4 and the Os precipitate is Os metal.

17. The method of claim 12 , wherein the reducing agent is chosen from NaHS, H 2 S gas, or Na 2 S 2 O 3 and the Os precipitate is OsS 2 .

18. The method of claim 5 , wherein a remaining mixture in the oxidizing solution is contacted with a reducing agent to form an osmium-free mixture comprising the at least one additional metal.

19. A method of separating an amount of osmium from a mixture comprising the amount of osmium and at least one additional metal, comprising:
a. contacting the mixture with an aqueous solution of NaClO at a concentration of about 12% w/v available chlorine to form a volatile OsO 4 vapor;
b. bubbling the OsO 4 vapor through a trapping solution comprising an aqueous solution of KOH at a concentration of about 25% w/v to form an amount of dissolved K 2 [OsO 4 (OH) 2 ];
c. contacting the dissolved K 2 [OsO 4 (OH) 2 ] with an aqueous solution of NaHS at a concentration of about 10% w/v to form an OsS 2 precipitate;
d. washing the OsS 2 precipitate by agitating with water;
e. separating the OsS 2 precipitate from the KOH trapping solution by centrifuging;
f. rinsing the OsS 2 precipitate with acetone; and
g. drying the OsS 2 precipitate.

20. The method of claim 19 , wherein the mixture is an irradiated Os-190 metal target, the amount of osmium comprises an amount of Os-191, and the at least one metal is chosen from Ir-192, Ir-193, Ir-194, Pt-192, Pt-194, or combinations thereof.

21. The method of claim 19 , wherein the mixture is contacted with the aqueous solution of NaClO at a temperature of about 40° C. until completely dissolved, and the dissolved mixture is contacted with the aqueous solution of NaClO at a temperature of about 90° C.

22. The method of claim 21 , wherein the dissolved mixture is contacted with the aqueous solution of NaClO until the aqueous solution of NaClO is colorless.

23. The method of claim 19 , wherein the trapping solution is situated within an ice bath while the dissolved K 2 [OsO 4 (OH) 2 ] is forming.

Assignees

• Univ Missouri

Inventors

• Engelbrecht Hendrik P
• Cutler Cathy S
• Manson Leonard
• Wilder Stacy Lynn

Classifications

• C22B11/042 Primary

  Recovery of noble metals from waste materials · CPC title

• C01G55/004

  Oxides; Hydroxides · CPC title

• C01G47/00

  Compounds of rhenium · CPC title

• C01G55/00

  Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum · CPC title

• C22B11/04

  by wet processes (extraction of metal compounds by leaching in organic solutions C22B3/16; treatment or purification of solutions by liquid-liquid extraction C22B3/26) · CPC title