IP Library Granted Patent US 12,420,262
Granted Patent B2
US 12,420,262 · App. 17/779,247 · Granted Sep 23, 2025

Chromatographic column having stationary phase thickness gradient

Inventors: Xudong Fan (Saline, MI); Hongbo Zhu (Johnson City, TN); Jinyan She (Ann Arbor, MI); Maxwell Wei-Hao Li (Troy, MI); Katsuo Kurabayashi (Ann Arbor, MI)
Assignee: The Regents of The University of Michigan
B01J20/287B01J20/285B01J20/3282G01N30/6065G01N30/6078G01N2030/025
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Quick Facts
Patent No.
US 12,420,262
App. No.
17/779,247
Granted
Sep 23, 2025
Kind
B2
Abstract

A gas chromatography device for peak focusing of one or more target analytes is provided that include a chromatographic column with an inlet and an outlet. A stationary phase is deposited inside the chromatographic column and has a positive thickness gradient. The stationary phase extends from the inlet to the outlet and has a first thickness at the inlet of the chromatographic column and a second thickness at the outlet of the chromatographic column. The second thickness is at least about 10% greater than the first thickness. Methods of peak focusing in a gas chromatography device, method of verifying peak focusing in a gas chromatography device and creating a gas chromatography device having a chromatographic column with a positive thickness gradient are also provided.

Claims (30)

1. A gas chromatography device for peak focusing of one or more target analytes, comprising:

a chromatographic column with an inlet and an outlet, wherein the inlet receives a sample comprising one or more target analytes that exits the chromatographic column at the outlet; and

a stationary phase deposited inside the chromatographic column and having a positive thickness gradient, wherein the stationary phase extends from the inlet to the outlet and has a first thickness at the inlet of the chromatographic column and a second thickness at the outlet of the chromatographic column, wherein the second thickness is at least about 10% greater than the first thickness.

2. The gas chromatography device of claim 1 , wherein the first thickness is greater than or equal to about 10 nm to less than or equal to about 10 micrometers and the second thickness is greater than or equal to about 30 nm to less than or equal to about 30 micrometers.

3. The gas chromatography device of claim 1 , wherein the second thickness is at least about 100% greater than or equal to the first thickness.

4. The gas chromatography device of claim 1 , wherein the second thickness is at least about 300% greater than or equal to the first thickness.

5. The gas chromatography device of claim 1 , wherein the chromatographic column is a microgas chromatographic column.

6. The gas chromatography device of claim 1 , wherein the stationary phase comprises a siloxane polymer.

7. The gas chromatography device of claim 6 , wherein the siloxane polymer comprises at least one alkyl group or aryl group comprising 1 to 30 carbon atoms.

8. The gas chromatography device of claim 1 , wherein a cross-sectional shape of the chromatographic column is selected from the group consisting of: circular, oval, rectangular, and triangular.

9. A method of peak focusing in a gas chromatography device, comprising:

introducing two or more target analytes into an inlet of a chromatographic column comprising a stationary phase deposited inside the chromatographic column and having a positive thickness gradient, wherein the stationary phase extends from the inlet to an outlet and has a first thickness at the inlet of the chromatographic column and a second thickness at the outlet of the chromatographic column, wherein the second thickness is at least about 10% greater than the first thickness;

separating two or more target analytes in the chromatographic column; and

eluting the two or more target analytes from the outlet of the chromatographic column.

10. The method of claim 9 , wherein the two or more target analytes are volatile organic compounds (VOCs).

11. The method of claim 9 , wherein at least one of the two or more target analytes comprises an aromatic compound and an overall peak focusing rate for the aromatic compound is greater than or equal to about 25%.

12. The method of claim 9 , wherein at least one of the two or more target analytes comprises an alkane compound and an overall peak focusing rate for the alkane compound is greater than or equal to about 10%.

13. The method of claim 9 , wherein the first thickness is greater than or equal to about 10 nm to less than or equal to about 10 micrometers and the second thickness is greater than or equal to about 30 nm to less than or equal to about 30 micrometers.

14. The method of claim 9 , wherein the second thickness is at least about 300% greater than or equal to the first thickness.

15. The method of claim 9 , wherein the chromatographic column is a microgas chromatographic column.

16. The method of claim 9 , wherein the stationary phase comprises a siloxane polymer comprising at least one alkyl group or aryl group comprising 1 to 30 carbon atoms.

17. The method of claim 9 , wherein a cross-sectional shape of the chromatographic column is selected from the group consisting of: circular, oval, rectangular, and triangular.

18. A method of verifying peak focusing in a gas chromatography device, comprising:

conducting a forward operation by introducing two or more target analytes into an inlet of a chromatographic column comprising a stationary phase deposited inside the chromatographic column and having a positive thickness gradient, wherein the stationary phase extends from the inlet to an outlet of the chromatographic column and has a first thickness at the inlet of the chromatographic column and a second thickness at the outlet, wherein the second thickness is at least about 10% greater than the first thickness;

separating the two or more target analytes in the chromatographic column;

eluting the two or more target analytes from the outlet of the chromatographic column;

conducting a reverse operation by introducing the two or more target analytes into the outlet of the chromatographic column comprising the stationary phase;

separating the two or more target analytes in the chromatographic column;

eluting the two or more target analytes from the inlet of the chromatographic column; and

comparing chromatographic resolutions from the forward operation and the reverse operation, wherein a peak focusing rate for at least one corresponding pair of two peaks from two target analytes is greater than 5%.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 24, 2022
From: FAN, XUDONG; ZHU, HONGBO; SHE, JINYAN; LI, MAXWELL WEI-HAO; KURABAYASHI, KATSUO
To: THE REGENTS OF THE UNIVERSITY OF MICHIGAN
Reel/Frame 059999/0380 →
Continuity (2)
Provisional Application 62940038 · Nov 25, 2019
Related Publication 20220410122A1 · Dec 29, 2022
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