Device and method of a supercritical fluid system for detecting analytes using a low pressure detector

Patent metadata

Field	Value
Publication number	US-10695692-B2
Application number	US-201514750437-A
Country	US
Kind code	B2
Filing date	Jun 25, 2015
Priority date	Jun 25, 2015
Publication date	Jun 30, 2020
Grant date	Jun 30, 2020

Abstract

A device is provided in a supercritical fluid system, which uses a mobile phase output by a separation device, the mobile phase volumetrically expanding as it decompresses. The device includes a passive splitter and a shuttle valve. The passive splitter is configured to receive the mobile phase and to split the mobile phase into a primary flow stream and a split flow stream, where the primary flow stream is directed to a pressure maintenance device. The passive splitter is further configured to reduce pressure of the split flow stream, causing volumetric expansion of the split flow stream. The shuttle valve is configured to insert volumetric aliquots of the volumetrically expanded split flow stream into a dilution flow stream to provide a diluted split flow stream, and to direct the diluted split flow stream to a low pressure detector.

First claim

What is claimed:

1. A flow splitter device in a supercritical fluid system, using a mobile phase output by a separation device, the mobile phase volumetrically expanding as it decompresses, the device comprising:
a passive splitter comprising a splitter tee and a splitter tee restrictor, the splitter tee configured to receive the mobile phase and to split the mobile phase into a primary flow stream and a split flow stream and, the splitter tee restrictor configured to reduce pressure of the split flow stream, causing volumetric expansion of the split flow stream containing an expanded gaseous CO 2 portion, wherein the primary flow stream is directed to a pressure maintenance device; and
a shuttle valve configured to insert volumetric aliquots of the volumetrically expanded split flow stream into a dilution flow stream to provide a diluted split flow stream, and to direct the diluted split flow stream to a low pressure detector, and direct the remaining portions of the volumetrically expanded split flow stream away from the low pressure detector.

2. The device of claim 1 , wherein the shuttle valve is further configured to direct remaining portions of the volumetrically expanded split flow stream, not inserted as volumetric aliquots into the dilution flow stream, to waste via a waste flow stream regulator, the waste flow stream regulator setting a pressure density experienced by the shuttle valve.

3. The device of claim 2 , wherein the waste flow stream regulator is dynamically adjustable, enabling adjustments in the pressure density experienced by the shuttle valve.

4. The device of claim 2 , wherein the waste flow regulator comprises at least one of a waste restrictor or a back pressure regulator.

5. The device of claim 1 , wherein the primary flow stream is directed to one or more high pressure detectors and a fraction collector for collecting a portion of the primary flow stream, as identified by at least one of the one or more high pressure detectors or the low pressure detector.

6. The device of claim 1 , wherein the passive splitter is configured to operate at a pressure of at least 90 bar.

7. The device of claim 1 , wherein the splitter restrictor comprises at least one of a narrow restrictor tube or a frit restrictor.

8. The device of claim 1 , further comprising:
a makeup pump is configured to provide solvent to the mobile phase prior to the passive splitter, wherein the dilution flow stream comprises a portion of the solvent provided by the makeup pump via a passive restrictor.

9. The device of claim 1 , wherein the dilution flow stream is provided by a dilution pump.

10. The device of claim 1 , wherein the pressure maintenance device comprises a back pressure regulator (BPR).

11. The device of claim 1 , wherein the low pressure detector comprises a mass spectrometer.

12. The device of claim 1 , wherein the shuttle valve comprises a mass rate attenuator.

13. A method of supplying a sample from a mobile phase output by a separation device of a supercritical fluid system to a low pressure detector, the method comprising:
splitting the mobile phase output by the separation device into a split flow stream and a primary flow stream, by directing the mobile phase output through a splitter tee;
reducing pressure of the split flow stream by directing the split flow stream through a splitter restrictor, causing volumetric expansion of the split flow stream containing an expanded gaseous CO 2 portion;
inserting volumetric aliquots of the volumetrically expanded split flow stream into a dilution flow stream to provide a diluted split flow stream;
directing the diluted split flow stream to the low pressure detector; and
directing remaining portions of the volumetrically expanded split flow stream away from the low pressure detector.

14. The method of claim 13 , further comprising:
directing the primary flow stream to a pressure maintenance device, a high pressure detector and a fraction collector for collecting a portion of the primary flow stream having an analyte of interest, as identified by at least one of the high pressure detector and the low pressure detector.

15. The method of claim 13 , further comprising:
directing remaining portions of the volumetrically expanded split flow stream, not inserted as volumetric aliquots into the dilution flow stream, to waste via a waste flow stream regulator; and
adjusting a pressure set by the waste flow stream regulator in order to adjust a pressure density experienced by the shuttle valve.

16. A chromatographic system, comprising:
a chromatographic column having a stationary phase for separating analytes in a high pressure mobile phase; and
the flow splitter device of claim 1 for reducing pressure of the high pressure mobile phase, wherein the passive splitter comprises:
a splitter tee configured to receive the mobile phase with separated analytes from the chromatographic column and to split the mobile phase into the primary flow stream and the split flow stream; and
a splitter restrictor configured to reduce pressure of the split flow stream, causing volumetric expansion of the split flow stream.

17. The chromatographic system of claim 16 , wherein the flow splitter further comprises:
a waste flow stream regulator in a split waste flow path positioned between the shuttle valve and waste, the waste flow stream regulator being configured to set a pressure density experienced by the shuttle valve,
wherein the shuttle valve directs remaining portions of the volumetrically expanded split flow stream to the waste via the split waste flow path.

18. The device of claim 1 , comprising a configuration selected from the group consisting of:
the passive splitter is configured to split the mobile phase and reduce the pressure of the split flow stream without diluting the split flow stream, and to direct the undiluted, volumetrically expanded split flow stream to the shuttle valve;
the splitter tee is the only splitter tee between the separation device and the low pressure detector; and
both of the foregoing.

19. The method of claim 13 , comprising a feature selected from the group consisting of:
the splitting the mobile phase output and the reducing pressure of the split flow stream are done without diluting the split flow stream, wherein the undiluted, volumetrically expanded split flow stream is directed to the shuttle valve;
the splitter tee is the only splitter tee between the separation device and the low pressure detector; and
both of the foregoing.

20. The method of claim 13 , comprising operating a shuttle valve to perform the inserting volumetric aliquots of the volumetrically expanded split flow stream into the dilution flow stream, and the directing the diluted split flow stream to the low pressure detector.

Assignees

• Agilent Technologies Inc

Inventors

• Wikfors Edwin E

Classifications

• G01N30/10

  using a splitter · CPC title

• G01N30/32

  of pressure or speed (G01N30/36 takes precedence) · CPC title

• G01N30/84

  Preparation of the fraction to be distributed · CPC title

• B01D15/40

  using supercritical fluid as mobile phase or eluent · CPC title

• B01D15/163 Primary

  Pressure or speed conditioning · CPC title