SYSTEM AND METHOD OF PRESSURE-CONTROLLED SPLITTING OF A CHEMICAL SAMPLE

• US 20200132641A1
• Filed: 10/24/2019
• Published: 04/30/2020
• Est. Priority Date: 10/25/2018
• Status: Active Grant

• Current Assignee: Entech Instruments Inc.
• Original Assignee: Entech Instruments Inc.
• Inventors: CARDIN, Daniel B.
• Granted Patent: US 11,536,703 B2
• Time in Patent Office: Days
• CPC Class Codes: G01N 2030/025 Gas chromatography
• CPC Class Codes: G01N 2030/324 speed, flow rate
• CPC Class Codes: G01N 30/10 using a splitter
• CPC Class Codes: G01N 30/16 Injection G01N30/24 takes precedence
• CPC Class Codes: G01N 30/20 using a sampling valve
• CPC Class Codes: G01N 30/32 of pressure or speed G01N30/36 takes precedence
• CPC Class Codes: G01N 30/7206 interfaced to gas chromatograph interfaces in general for introducing or extracting samples to be analysed with specially adapted mass spectrometer, see H01J49/04
• CPC Class Codes: G01N 30/8658 Optimising operation parameters

Abstract

Pressure-controlled splitting can be used to inject a chemical sample from an injection source to a detector (e.g., a mass spectrometer) for chemical analysis (e.g., gas chromatography or gas chromatography-mass spectrometry) with reduced peak widths. For example, the sample is first transferred to a first compression volume; then pressure in the system is increased to compress the sample to split it between a second compression volume and a column. The fraction of the sample split to the column can have reduced peak widths compared to the peak widths prior to compression and splitting yet can maintain the same peak height to preserve high sensitivity for trace level analysis. This portion of the sample can traverse the column and elute to the detector for analysis with reduced chemical noise. Faster injection rates can allow faster analysis times, as less separation of chemicals is needed before the sample reaches the detector.

Claims

1. A method, comprising:

transferring a sample from an injector source of a system to a first compression volume;

increasing pressure in the system at a steady rate while splitting the sample into a first portion that is transferred to a column of the system and a second portion that is transferred to a second compression volume of the system, wherein the first compression volume, the second compression volume, and the column are coupled by a tee;

separating chemical compounds of the sample from one another as a first portion of the sample moves through the column; and

conducting chemical analysis of the first portion of the sample with a detector.

2. The method of claim 1, wherein a width of a peak of the sample decreases as the peak moves past the tee, and a height of the peak remains substantially constant as the peak moves past the tee.

3. The method of claim 1, further comprising:

opening a vent solenoid valve that is fluidly coupled to the second compression volume to remove the second portion of the sample from the system.

4. The method of claim 3, wherein the vent solenoid valve is opened after the entire sample is split between the column and the second compression volume.

5. The method of claim 1, wherein a restricting outlet is coupled fluidly coupled to the second compression volume, and the restricting outlet is configured to allow gas to exit the system at a flow rate that is lower than a flow rate of gas through the column.

6. The method of claim 1, wherein the entire sample traverses a tee that connects the first compression volume, the second compression volume, and the column while the pressure is increasing.

7. The method of claim 1, wherein conducting chemical analysis of the first portion of the sample includes performing gas chromatography-mass spectrometry (GC-MS).

8. The method of claim 1 further comprising:

selecting the second compression volume from a plurality of compression volumes, each of the plurality of compression volumes having a unique volume and being switchably couplable to the first compression volume and the column.

9. The method of claim 1, wherein increasing the pressure in the system is performed such that an injection rate of the sample into the detector increases, wherein the detector comprises one of a gas chromatography analyzer and a gas chromatography-mass spectrometry analyzer.

10. A system, comprising:

an injector source;

a first compression volume fluidly coupled to the injector source at a first end of the first compression volume;

a second compression volume;

a column;

a tee fluidly connecting a second end of the first compression volume, the second compression volume, and the column;

a detector; and

an electronic pressure controller configured to;

transfer a sample from an injector source of a system to a first compression volume; and

increase pressure in the system at a steady rate while splitting the sample between a second compression volume and a column, wherein;

the column is configured to separate chemical compounds of the sample from one another as a first portion of the sample moves through the column, and

the detector is configured to conduct chemical analysis of the first portion of the sample.

11. The system of claim 10, wherein a width of a peak of the sample decreases as the peak moves past the tee, and a height of the peak remains substantially constant as the peak moves past the tee.

12. The system of claim 10, further comprising:

a vent solenoid valve that is fluidly coupled to the second compression volume, wherein opening the vent solenoid valve allows the second portion of the sample to be removed from the system.

13. The system of claim 12, wherein the vent solenoid valve is configured to be opened after the entire sample is split between the column and the second compression volume.

14. The system of claim 10, further comprising:

a restricting outlet that is fluidly coupled to the second compression volume, wherein the restricting outlet is configured to allow gas to exit the system at a flow rate that is lower than a flow rate of gas through the column.

15. The system of claim 10, wherein the entire sample traverses a tee that connects the first compression volume, the second compression volume, and the column while the pressure is increasing.

16. The system of claim 10, wherein conducting chemical analysis of the first portion of the sample includes performing gas chromatography-mass spectrometry (GC-MS).

17. The system of claim 10, further comprising:

a plurality of compression volumes including the second compression volume, each of the plurality of compression volumes having a unique volume and being switchably couplable to the first compression volume and the column.

18. The system of claim 10, wherein the electronic pressure controller is configured to increase the pressure in the system is performed such that an injection rate of the sample into the detector increases, wherein the detector comprises one of a gas chromatography analyzer and a gas chromatography-mass spectrometry analyzer.