Separation efficiency in supercritical fluid chromatography

Patent metadata

Field	Value
Publication number	US-9933399-B2
Application number	US-201314423949-A
Country	US
Kind code	B2
Filing date	Aug 30, 2013
Priority date	Aug 31, 2012
Publication date	Apr 3, 2018
Grant date	Apr 3, 2018

Abstract

The present technology uses one or more separating segments, i.e. chromatography columns, aligned in series along a flow path. The separating segments are divided by a plurality of heating elements or are heated directly. The heating elements heat the supercritical mobile phase and sample to replace heat lost due to axial expansion of the mobile phase along the mobile phase flow path.

First claim

What is claimed is:

1. A method for separating a sample in a compressible fluid chromatography device defining a flow path, the device comprises a plurality of segments for separating the sample and/or heating at least a portion of the flow path, the method comprising:
introducing the sample into the compressible fluid chromatography device;
separating the sample along at least two non-contiguous segments of the compressible fluid chromatography device along the flow path, wherein the said non-contiguous segments are separated by a heating segment; and
heating one or more of the plurality of segments of the compressible fluid chromatography device to reduce heat lost due to expansion of the compressible fluid along the flow path.

2. The method of claim 1 , further comprising collecting fractions of the sample after separation.

3. The method of claim 1 , wherein multiple different types of separating segments are used.

4. The method of claim 1 , wherein the separating segments used are of the same type.

5. The method of claim 1 , further comprising pre-heating the sample before separation with a pre-heater.

6. The method of claim 1 , wherein the heating segment has the characteristics of a pre-heater.

7. The method of claim 1 , wherein the compressible fluid is carbon dioxide.

8. The method of claim 7 , wherein the carbon dioxide is at supercritical conditions within at least a portion of the at least two non-contiguous segments during separation of the sample.

9. The method of claim 1 , wherein the compressible fluid is a chlorofluorocarbon.

10. The method of claim 9 wherein the compressible fluid is Freon.

11. The method of claim 1 wherein the compressible fluid is N 2 O.

12. The method of claim 1 wherein the compressible fluid is SF 6 .

13. A method for separating a sample in a carbon dioxide-based chromatography device defining a flow path, the method comprising:
providing a carbon dioxide-based chromatography device including a plurality of segments for separating the sample and/or heating at least a portion of the flow path;
introducing the sample into the chromatography device;
separating the sample along at least two non-contiguous segments of the flow path of the mobile phase through the device; and
heating at least one of the plurality of segments disposed between the two non-contiguous segments of the flow path of the chromatography device to reduce the heat lost due to expansion of the carbon dioxide along the fluid path.

14. The method of claim 13 , further comprising collecting fractions of the sample after separation.

15. The method of claim 13 , wherein multiple different types of separating segments are used.

16. The method of claim 13 , wherein the separating segments used are of the same type.

17. The method of claim 13 , further comprising pre-heating the sample before separation with a pre-heater.

18. The method of claim 13 , wherein the heating segment has the characteristics of a pre-heater.

19. The method of claim 13 , wherein the carbon dioxide mobile phase is at or near supercritical conditions within at least a portion of the at least two non-contiguous segments during separation of the sample.

Assignees

• Waters Technologies Corp

Inventors

• Fairchild Jacob Nathan
• Wyndham Kevin Daniel

Classifications

• G01N2030/025

  Gas chromatography · CPC title

• G01N1/2202

  involving separation of sample components during sampling · CPC title

• G01N30/6039

  in series · CPC title

• G01N30/80 Primary

  Fraction collectors · CPC title

• B01D15/40 Primary

  using supercritical fluid as mobile phase or eluent · CPC title