IP Library Granted Patent US 10,357,758
Granted Patent B2
US 10,357,758 · App. 13/707,824 · Granted Jul 23, 2019

Method of pre-treating an adsorbent for a chromatographic separation

Inventor: Steve Oelsner (Ottawa, CA)
Assignee: BWXT ITG CANADA, INC.
B01J20/3021B01D15/20B01D15/203B01J20/06B01J20/08B01J20/103B01J20/282B01J20/283B01J20/284B02C23/08G21G1/001G21G2001/0021G21G2001/0031G21G2001/0042G21G2001/0057G21G2001/0073G21G2001/0084
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Quick Facts
Patent No.
US 10,357,758
App. No.
13/707,824
Granted
Jul 23, 2019
Kind
B2
Abstract

A method of treating an adsorbent for a chromatographic separation. The method involves sonicating particles of an inorganic metal oxide having fragile edges in the absence of any alkylating or acylating agent to form smoothened particles of the inorganic metal oxide and washing the smoothened particles of the inorganic metal oxide to remove fine particulate matter to produce a treated adsorbent. The treated adsorbent can be used in a method of isolating a daughter radioisotope from a daughter radioisotope that is produced from the parent radioisotope by radioactive decay.

Claims (46)

1. A method of producing a treated chromatographic separation adsorbent, comprising:

crystallizing titanium oxide or tin oxide in the presence of a base to form a crystalline metal oxide;

drying the crystalline metal oxide to form a chromatographic separation adsorbent;

sonicating the chromatographic separation adsorbent, in the absence of any alkylating or acylating agent to form sonicated particles of the crystalline metal oxide and fine particulate matter of the crystalline metal oxide;

washing the sonicated particles of the crystalline metal oxide to remove the fine particulate matter of the crystalline metal oxide to produce a washed, treated chromatographic separation adsorbent; and

drying the washed, treated chromatographic separation adsorbent, thereby producing the treated chromatographic separation adsorbent.

2. The method according to claim 1 , wherein the chromatographic separation adsorbent is sonicated for a period of about 1 to about 4 hours.

3. The method according to claim 1 , wherein the chromatographic separation adsorbent is sonicated for a period of about 1 to about 2 hours.

4. The method according to claim 1 , wherein the sonicated particles of the crystalline metal oxide have a particle size of from about 10 μm to about 300 μm.

5. The method according to claim 1 , wherein the crystalline metal oxide is titanium oxide, and wherein after the step of drying the treated chromatographic separation adsorbent is baked at a temperature of from about 400° C. to about 600° C. for about 1 to about 2 hours to produce a baked chromatographic separation adsorbent, the baked chromatographic separation adsorbent configured to reduce plugging of a filtration membrane in a chromatographic column.

6. The method according to claim 1 , wherein the crystalline metal oxide is titanium oxide, and wherein after the step of drying the treated chromatographic separation adsorbent is baked at a temperature of from about 500° C. to about 600° C. for about 1 to about 2 hours to produce anatase titanium oxide.

7. The method as claimed in claim 1 further comprising a step of packing a chromatographic column with the treated chromatographic separation adsorbent.

8. A method of isolating a daughter radioisotope from a parent radioisotope, the daughter radioisotope produced from the parent radioisotope by radioactive decay, the method comprising:

adsorbing the parent radioisotope onto the treated chromatographic separation adsorbent produced by the method according to claim 1 to produce a treated chromatographic separation adsorbent comprising an adsorbed parent radioisotope;

allowing a portion of the parent radioisotope adsorbed on the treated chromatographic separation adsorbent comprising an adsorbed parent radioisotope to decay to the daughter radioisotope; and

eluting a solution of the daughter radioisotope from the treated chromatographic separation adsorbent comprising an adsorbed parent radioisotope, thereby isolating the daughter radioisotope from the parent radioisotope.

9. The method according to claim 8 , wherein the sonicated particles of the crystalline metal oxide have a particle size of about 10 μm to about 300 μm.

10. The method according to claim 8 , wherein the chromatographic separation adsorbent is sonicated for a period of about 1 to about 4 hours.

11. The method according to claim 8 , wherein the chromatographic separation adsorbent is sonicated for a period of about 1 to about 2 hours.

12. The method according to claim 8 , wherein the crystalline metal oxide is titanium oxide, and wherein after the step of drying the treated chromatographic separation adsorbent is baked at a temperature of from about 400° C. to about 600° C. for about 1 to about 2 hours.

13. The method according to claim 8 , wherein the crystalline metal oxide is titanium oxide, and wherein after the step of drying the chromatographic separation adsorbent is baked at a temperature of from about 500° C. to about 600° C. for about 1 to about 2 hours to produce anatase titanium oxide.

14. The method according to claim 8 , wherein:

i) the parent radioisotope is 68 Ge and the daughter radioisotope is 68 Ga;

ii) the parent radioisotope is 82 Sr and the daughter radioisotope is 82 Rb;

iii) the parent radioisotope is 99 Mo and the daughter radioisotope is 99m Tc;

iv) the parent radioisotope is 188 W and the daughter radioisotope is 188 Re;

v) the parent radioisotope is 62 Zn and the daughter radioisotope is 62 Cu;

vi) the parent radioisotope is 113 Sn and the daughter radioisotope is 113m In;

vii) the parent radioisotope is 228 Th and the daughter radioisotope is 212 Bi; or

viii) the parent radioisotope is 225 Ac and the daughter radioisotope is 221 Fr.

15. The method according to claim 8 , further comprising a step of grinding and sieving the crystalline metal oxide to a particle size of from about 10 μm to about 300 μm.

16. A method of isolating a compound of interest from a crude sample, comprising:

crystallizing titanium oxide or tin oxide in the presence of a base to form a crystalline metal oxide;

drying the crystalline metal oxide to form a chromatographic separation adsorbent;

sonicating the chromatographic separation adsorbent in the absence of any alkylating or acylating agent to form sonicated particles of the crystalline metal oxide and fine particulate matter of the crystalline metal oxide;

washing the sonicated particles of the crystalline metal oxide to remove the fine particulate matter of the crystalline metal oxide, to produce a washed, treated chromatographic separation adsorbent;

drying the washed, treated chromatographic separation adsorbent, thereby producing a treated chromatographic separation adsorbent that reduces plugging of a filtration membrane in a chromatographic column; and

using the treated chromatographic separation adsorbent in the chromatographic column to isolate the compound of interest.

17. The method according to claim 16 , wherein the step of using comprises:

adsorbing the compound of interest from the crude sample onto the treated chromatographic separation adsorbent to produce the treated chromatographic separation adsorbent comprising an adsorbed compound of interest; and

a solution of the compound of interest from the treated chromatographic separation adsorbent comprising the adsorbed compound of interest, thereby isolating the compound of interest from the crude sample.

18. The method according to claim 16 , wherein the crystalline metal oxide is titanium oxide, and after the step of drying the treated chromatographic separation adsorbent is baked at a temperature of from about 400° C. to about 600° C. for about 1 to about 2 hours, the treated chromatographic separation adsorbent configured to reduce plugging of the filtration membrane in the chromatographic column.

19. The method according to claim 16 , wherein the crystalline metal oxide is titanium oxide, and wherein after the step of drying the treated chromatographic separation adsorbent is baked at a temperature of from about 500° C. to about 600° C. for about 1 to about 2 hours to produce anatase titanium oxide.

20. The method according to claim 16 , wherein the chromatographic separation adsorbent is sonicated for a period of about 1 to about 4 hours.

21. The method according to claim 16 , wherein the chromatographic separation adsorbent is sonicated for a period of about 1 to about 2 hours.

22. The method according to claim 16 , further comprising a step of grinding and sieving the crystalline metal oxide to a particle size of from about 10 μm to about 300 μm.

Assignments (4)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 31, 2026
From: NORDION (CANADA) INC.
To: BWXT ITG CANADA, INC.
Reel/Frame 075491/0345 →
CHANGE OF NAME Recorded Jul 31, 2026
From: BWXT ITG CANADA, INC.
To: BWXT MEDICAL LTD
Reel/Frame 075491/0353 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 20, 2018
From: NORDION (CANADA) INC.
To: BWXT ITG CANADA, INC.
Reel/Frame 047830/0091 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 26, 2013
From: OELSNER, STEVE
To: NORDION (CANADA) INC.
Reel/Frame 029879/0307 →
Continuity (2)
Provisional Application 61568524 · Dec 8, 2011
Related Publication 20130220928A1 · Aug 29, 2013