Catalytic oxidation of polar modifiers in chromatographic mobile phases

Patent metadata

Field	Value
Publication number	US-10151733-B2
Application number	US-201414484350-A
Country	US
Kind code	B2
Filing date	Sep 12, 2014
Priority date	Sep 13, 2013
Publication date	Dec 11, 2018
Grant date	Dec 11, 2018

Abstract

The present disclosure relates to an oxidizer, and related methods, for oxidizing polar modifiers in chromatographic mobile phases. The oxidizer enables the use of flame-based detection in chromatographic separations, such as carbon dioxide based chromatography, which employ polar modifiers, such as methanol. Upon exiting a chromatographic column, the mobile phase containing the polar modifier is flowed through an oxidizer that contains a catalyst to oxidize at least a portion of the polar modifier to a species that does not interfere with the function of the flame-based detector. The oxidizer allows for flame-based detection, such as flame ionization detection, in applications in which a polar modifier with a reduced form of carbon is used.

First claim

What is claimed is:

1. A method of oxidizing a polar modifier in a chromatographic mobile phase containing at least one analyte of interest, comprising:
(i) providing a chromatographic system having a separation column, an oxidizer in fluid communication with and downstream of the column, and a flame-based detector in fluid communication with and downstream of the oxidizer; and
(ii) oxidizing at least a portion of the polar modifier consisting essentially of methanol in the oxidizer to carbon dioxide, wherein the oxidizer has a catalyst that (a) facilitates selective oxidation of at least a portion of the polar modifier to carbon dioxide which does not substantially produce a signal in the flame-based detector and (b) does not permit the complete oxidation of the at least one analyte of interest.

2. The method of claim 1 , wherein the mobile phase comprises carbon dioxide.

3. The method of claim 1 , wherein the flame-based detector is a flame ionization detector or a flame photometric detector.

4. The method of claim 1 , wherein the catalyst comprises one or more constituents selected from the group consisting of: Ag, Au, Rh, Ni, Cd, Pt, Pd, Cu, TiO 2 , ZnO, ZrO 2 , and Al 2 O 3 ; or combinations, alloys, or mixtures thereof.

5. The method for claim 1 , wherein the oxidizer further comprises a reagent gas.

6. The method of claim 1 , wherein the catalyst is deposited on the surface of a ceramic support.

7. The method of claim 1 , wherein the oxidizer further comprises a heater in thermal communication with the oxidizer wherein the heater is capable of maintaining the catalyst at a temperature range.

8. The method of claim 1 , wherein over 50 wt % of the polar modifier in the mobile phase entering the oxidizer is oxidized.

9. The method of claim 1 , wherein the polar modifier in the mobile phase entering the oxidizer is substantially completely oxidized.

10. A chromatographic system comprising
a mobile phase source;
a polar modifier source;
a sample source;
a separation column in fluid communication with each of the mobile phase source, the polar modifier source, and the sample source and which receives therefrom a combined flow of mobile phase, polar modifier consisting essentially of methanol, and sample;

an oxidizer comprising:
(i) an inlet port that receives the combined flow from the separation column;
(ii) a chamber in fluid communication with the inlet port, wherein the chamber has a catalyst configured to (a) facilitate selective oxidation of at least a portion of the polar modifier to carbon dioxide which does not substantially produce a signal in a flame-based detector and (b) does not permit the complete oxidation of at least one analyte of interest within the sample; and
(iii) an outlet port in fluid communication with the chamber for exiting the mobile phase and carbon dioxide from the chamber; and

the flame-based detector in fluid communication with the outlet port.

11. The chromatographic system of claim 10 , wherein the mobile phase comprises carbon dioxide.

12. The chromatographic system of claim 10 , wherein the flame-based detector is a flame ionization detector or a flame photometric detector.

13. The chromatographic system of claim 10 , wherein the catalyst comprises one or more constituents selected from the group consisting of: Ag, Au, Rh, Ni, Cd, Pt, Pd, Cu, TiO 2 , ZnO, ZrO 2 , and Al 2 O 3 ; or combinations, alloys, or mixtures thereof.

14. The chromatographic system of claim 10 , further comprising a reagent gas in the chamber.

15. The chromatographic system of claim 10 , wherein the catalyst is deposited on the surface of a ceramic support.

16. The chromatographic system of claim 10 , further comprising a heater in thermal communication with the chamber wherein the heater is capable of maintaining the catalyst at a temperature range.

17. The chromatographic system of claim 10 , wherein over 50 wt % of the polar modifier in the mobile phase entering the chamber is oxidized.

18. The chromatographic system of claim 10 , wherein the polar modifier in the mobile phase entering the chamber is substantially completely oxidized.

Assignees

• Waters Technologies Corp

Inventors

• Fogwill Michael O
• Michienzi Joseph D
• Murphy James P

Classifications

• G01N27/626

  using heat to ionise a gas · CPC title

• G01N30/84 Primary

  Preparation of the fraction to be distributed · CPC title

• G01N30/68

  Flame ionisation detectors · CPC title

• G01N2030/8435

  for chemical reaction · CPC title