Retention-time locked comprehensive multidimensional gas chromatography

• US 6,494,078 B1
• Filed: 06/25/2001
• Issued: 12/17/2002
• Est. Priority Date: 06/25/2001
• Status: Active Grant

• Current Assignee: Agilent Technologies, Inc.
• Original Assignee: Agilent Technologies, Inc.
• Inventors: Klee, Matthew S.
• Primary Examiner(s): Williams, Hezron
• Assistant Examiner(s): WIGGINS, JOHN DAVID
• Application Number:
  US09/888,927
• Publication Number:
  US 20020194898A1
• Time in Patent Office: 540 Days
• Field of Search: 73/233.5, 73/232.2, 73/233.6, 73/232.7, 73/233.9, 73/232.4, 73/232.3, 55/67, 210/198.2, 210/656, 422/70, 422/89
• US Class Current: 73/23.35
• CPC Class Codes: G01N 2030/025 Gas chromatography
• CPC Class Codes: G01N 2030/324 speed, flow rate
• CPC Class Codes: G01N 30/32 of pressure or speed G01N30/36 takes precedence
• CPC Class Codes: G01N 30/462 with different eluents or with eluents in different states G01N30/463 takes precedence
• CPC Class Codes: G01N 30/463 for multidimensional chromatography
• CPC Class Codes: G01N 30/465 with specially adapted interfaces between the columns
• CPC Class Codes: G01N 30/8672 not depending on an individual instrument, e.g. retention time indexes or calibration transfer

Abstract

A method applies retention-time locking to the retention times and/or the column(s) void times of a target analyte(s) being eluted thru a multidimensional gas chromatography system. Retention time locking is applied to both standard and comprehensive multidimensional gas chromatography via the steps of adjusting column(s) head pressure in a locking multidimensional gas chromatograph system such that the measured retention times and/or void times match the known accepted. Retention time locking may be applied to either or both of the columns in a multidimensional gas chromatography system. Additionally, if the multidimensional system contains more than two columns in series, retention time locking can be applied to any or all of the columns as required.

Claims

1. A method of retention time locking a multidimensional GC system, comprising:

(i) configuring operating parameters of a reference multidimensional GC system in accordance with a known chromatographic method, wherein the reference multidimensional GC system includes more than one column connected in series, each of the columns having a known stationary phase, nominal diameter and length, and phase ratio;

(ii) introducing one or more target analytes into the reference multidimensional GC system yielding defined analyte retention times and/or defined void times for one or more columns of the reference multidimensional GC system;

(iii) configuring operating parameters of a locking multidimensional GC system in accordance with the known chromatographic method, wherein the locking multidimensional GC system includes a same number of columns connected in series as the reference multidimensional GC system, each of the same number of columns having a same known stationary phase, nominal diameter and length and phase ratio as the reference multidimensional GC system and wherein each column of the locking multidimensional GC system has a head pressure;

(iv) locking the retention times of the target analytes or void times on one or more columns of the locking multidimensional GC system, beginning with a last column in series to be locked and proceeding sequentially to a first column to be locked, by adjusting the head pressure of the column to be locked such that the retention times of the target analytes or column void times measured on the locking multidimensional GC system are matched to the corresponding defined analyte retention times and/or defined column void times.

2. The method of claim 1, further comprising locking all of the columns of the locking multidimensional GC system.

3. The method of claim 1, further comprising converting the retention times of the analytes to retention factors and locking the columns on the locking multidimensional GC system based on retention factors.

4. The method of claim 1, wherein the reference multidimensional GC system and the locking multidimensional GC system are comprehensive multidimensional GC systems.

5. The method of claim 1, further comprising scaling the conditions of one or more of the columns of the locking multidimensional GC system.

6. The method of claim 5, wherein the scaling is accomplished by method translation.

7. The method of claim 1 wherein the reference multidimensional GC system includes a multidimensional detector.

8. The method of claim 7, further comprising tuning the multidimensional detector to respond to specific attributes of the analytes.

9. The method of claim 1 further comprising generating a retention time database of the defined analyte retention times in multidimensional chromatographic space.

10. The method of claim 9 further comprising plotting the defined analyte retention time to create an isoplot.

11. The method of claim 10 further comprising generating a set of homolog vectors in the multidimensional chromatographic space.

20. The method of claim 10 further comprising using the retention time database, isoplot and/or homolog vectors to identify unknown analytes on the locking multidimensional GC system.

12. A method of locking the overall retention time of a multidimensional GC system comprising:

(i) configuring operating parameters of a reference multidimensional GC system in accordance with a known chromatographic method, wherein the reference multidimensional GC system includes two or more columns connected in series, each of the columns having known stationary phase, nominal diameter and length, and phase ratio;

(ii) introducing one or more known analytes into the reference multidimensional GC system yielding defined analyte retention times and/or defined void time for each column;

(iii) configuring operating parameters of a locking multidimensional GC system in accordance with the known chromatographic method wherein the locking multidimensional GC system includes a same number of columns connected in series, each of the same number of columns having a same known stationary phase, nominal diameter and length, and phase ratio as the reference multidimensional GC system and wherein each column of the locking multidimensional GC system has a head pressure;

(iv) locking the retention times of the known analytes or void times on the locking multidimensional GC system by adjusting the head pressures of each column on the locking multidimensional GC system, beginning with a last column in series and proceeding sequentially to a first column in series, such that the retention times of the known analytes or column void times measured on the locking multidimensional GC system are matched to the corresponding defined analyte retention times and/or defined column void time.

13. The method of claim 12, wherein the reference multidimensional GC systems and the locking multidimensional GC systems are comprehensive multidimensional GC systems.

14. The method of claim 12, further comprising converting the retention times of the analytes to retention factors and locking the columns on the locking multidimensional GC system based on retention factors.

15. The method of claim 12, further comprising scaling the conditions of one or more of the columns of the locking multidimensional GC system.

16. The method of claim 15, wherein the scaling is accomplished by method translation.

17. A method of retention time locking a multidimensional GC system comprising:

(i) configuring operating parameters of a reference multidimensional GC system in accordance with a known chromatographic method, wherein the reference multidimensional GC system includes a first column and a second column connected in series, each of the columns having a known stationary phase, nominal diameter and length, and phase ratio;

(ii) injecting one or more known analytes into the reference multidimensional GC system yielding defined analyte retention times and/or defined void times for each column;

(iii) configuring operating parameters of a locking mulitidmensional GC system in accordance with the known chromatographic method, wherein the locking multidimensional GC includes a first column and a second column, each of the columns having a same known stationary phase, nominal diameter and length and phase ratio as the reference multidimensional GC system and wherein the first column and second column have a head pressure;

(iv) adjusting the head pressure of the second column such that the retention times of the known analytes and/or void time measured for the second column are matched to the corresponding defined analyte retention times and/or defined void time;

(v) adjusting the head pressure of the first column such that the retention times of the known analytes and/or void time for the second column are matched to the corresponding defined analyte retention times and/or defined void time.

18. The method of claim 17, wherein the reference multidimensional GC system and the locking multidimensional GC system are comprehensive multidimensional GC systems.

19. The method of claim 17 further comprising converting the retention times of the analytes to retention factors and locking the columns on the locking multidimensional GC system based on retention factors.