Gas-less eluent generator

Patent metadata

Field	Value
Publication number	US-2024209517-A1
Application number	US-202218146485-A
Country	US
Kind code	A1
Filing date	Dec 27, 2022
Priority date	Dec 27, 2022
Publication date	Jun 27, 2024
Grant date	—

Abstract

An eluent generation module includes an electrolytic gas generator and an electrolytic eluent generator. The electrolytic gas generator includes a generation chamber having an inlet and an outlet; an outlet electrode within the generation chamber; a first ion exchange connector; a bulk solvent chamber separated from the generation chamber by the ion exchange connector; and a bulk solvent chamber electrode within the bulk solvent chamber. The electrolytic eluent generator includes an electrolyte chamber containing an aqueous electrolyte solution; an electrolyte chamber electrode within the electrolyte chamber; a second ion exchange connector; an eluent generation chamber separated from the electrolyte chamber by the second ion exchange connector; and an eluent generation chamber electrode.

First claim

What is claimed is:

1 . An eluent generation module comprising:
an electrolytic gas generator including:
a generation chamber having an inlet and an outlet;
an outlet electrode within the generation chamber;
a first ion exchange connector;
a bulk solvent chamber separated from the generation chamber by the ion exchange connector; and
a bulk solvent chamber electrode within the bulk solvent chamber; and
an electrolytic eluent generator including:
an electrolyte chamber containing an aqueous electrolyte solution;
an electrolyte chamber electrode within the electrolyte chamber;
a second ion exchange connector;
an eluent generation chamber separated from the electrolyte chamber by the second ion exchange connector; and
an eluent generation chamber electrode.

2 . The eluent generation module of claim 1 wherein the electrolytic eluent generator is configured to generate an acid eluent, the second ion exchange connector including an anion exchange barrier, the electrolyte chamber electrode being a cathode, the eluent generation chamber electrode being an anode.

3 . The eluent generation module of claim 2 wherein the electrolytic gas generator is configured to generate H 2 at the outlet to combine with O 2 generated at the eluent generation chamber electrode, the first ion exchange connector including an anion exchange barrier, and the outlet electrode being a cathode, the bulk solvent chamber electrode being an anode.

4 . The eluent generation module of claim 2 wherein the aqueous electrolyte solution includes carbonic acid, sulfuric acid, phosphoric acid, acetic acid, methanesulfonic acid, or any combination thereof.

5 . The eluent generation module of claim 2 wherein the generation chamber includes an anion exchange bed.

6 . The eluent generation module of claim 1 wherein the eluent generation module is configured to generate a base eluent, the second ion exchange connector including a cation exchange barrier, the electrolyte chamber electrode being an anode, the eluent generation chamber electrode being a cathode.

7 . The eluent generation module of claim 5 wherein the electrolytic gas generator is configured to generate O 2 at the outlet to combine with H 2 generated at the eluent generation chamber electrode, the first ion exchange connector including a cation exchange barrier, and the outlet electrode being an anode, the bulk solvent chamber electrode being a cathode.

8 . The eluent generation module of claim 5 wherein the aqueous electrolyte solution includes potassium hydroxide, sodium hydroxide, lithium hydroxide, other alkali hydroxides, or any combination thereof.

9 . The eluent generation module of claim 2 wherein the generation chamber includes an anion exchange bed.

10 . The eluent generation module of claim 1 wherein the outlet electrode is a perforated platinum electrode.

11 . A method of generating a gas-free base eluent, comprising:
supplying a liquid to an inlet of an electrolytic gas generator, the electrolytic gas generator including a generation chamber having the inlet and an outlet; an outlet anode within the generation chamber; a first cation exchange connector; a bulk solvent chamber separated from the generation chamber by the cation exchange connector; and a bulk solvent chamber cathode within the bulk solvent chamber; applying a current across the outlet anode and the bulk solvent chamber cathode to generate O 2 at the outlet anode; providing a liquid stream containing oxygen gas from the outlet to an electrolytic eluent generator, the electrolytic eluent generator including an electrolyte chamber containing an aqueous electrolyte solution, an electrolyte chamber anode within the electrolyte chamber, a second cation exchange connector, an eluent generation chamber separated from the electrolyte chamber by the second cation exchange connector; and an eluent generation chamber cathode; applying a current across the electrolyte chamber anode and the eluent generation chamber cathode to migrate electrolyte ions from the electrolyte chamber across the second cation exchange connector to form the base eluent in the eluent generation chamber; and reacting the O 2 with H 2 formed at the eluent generation chamber cathode to produce the gas-free base eluent.

12 . The method of claim 11 wherein the aqueous electrolyte solution includes potassium hydroxide, sodium hydroxide, lithium hydroxide, other alkali hydroxides, or any combination thereof.

13 . The method of claim 11 wherein the outlet anode is a perforated platinum anode.

14 . The method of claim 11 wherein the gas-free base eluent contains less than about 0.2 ml of gas per ml of eluent.

15 . The method of claim 14 wherein the gas-free base eluent contains less than about 0.1 ml of gas per ml of eluent.

16 . The method of claim 15 wherein the gas-free base eluent contains less than about 0.05 ml of gas per ml of eluent.

17 . The method of claim 11 further comprising:
injecting a sample onto a chromatography column;
varying the current applied across the generation chamber anode and the bulk solvent chamber cathode of the electrolytic gas generator and varying the current applied across the electrolyte chamber anode and the eluent generation chamber cathode to vary the concentration of the gas-free base eluent;
supplying the gas-free base eluent to the chromatography column;
eluting sample analytes from the chromatography column; and
detecting the sample analytes using a detector.

18 . A method of generating a gas-free acid eluent, comprising:
supplying a liquid to an inlet of an electrolytic gas generator, the electrolytic gas generator including a generation chamber having the inlet and an outlet; an outlet cathode within the generation chamber; a first anion exchange connector; a bulk solvent chamber separated from the generation chamber by the anion exchange connector; and a bulk solvent chamber anode within the bulk solvent chamber; applying a current across the outlet cathode and the bulk solvent chamber anode to generate H 2 at the outlet cathode; providing a liquid stream containing hydrogen gas from the outlet to an electrolytic eluent generator, the electrolytic eluent generator including an electrolyte chamber containing an aqueous electrolyte solution, an electrolyte chamber cathode within the electrolyte chamber, a second anion exchange connector, an eluent generation chamber separated from the electrolyte chamber by the second anion exchange connector; and an eluent generation chamber anode; applying a current across the electrolyte chamber cathode and the eluent generation chamber anode the migrate electrolyte ions from the electrolyte chamber across the second anion exchange connector to form the acid eluent in the eluent generation chamber; and reacting the H 2 with O 2 formed at the eluent generation chamber anode to produce the gas-free acid eluent.

19 . The method of claim 18 wherein the aqueous electrolyte solution includes carbonic acid, sulfuric acid, phosphoric acid, acetic acid, methanesulfonic acid, or any combination thereof.

20 . The method of claim 18 wherein the outlet electrode is a perforated platinum electrode.

21 . The method of claim 18 wherein the gas-free acid eluent contains less than about 0.2 ml of gas per ml of eluent.

22 . The method of claim 21 wherein the gas-free acid eluent contains less than about 0.1 ml of gas per ml of eluent.

23 . The me

Assignees

• Dionex Corp

Inventors

• Chen Yongjing
• Liu Yan

Classifications

• G01N30/72

  Mass spectrometers {(mass spectrometers per se H01J49/00)} · CPC title

• G01N2030/965

  suppressor columns · CPC title

• G01N30/96

  using ion-exchange (G01N30/02, G01N30/90 take precedence) · CPC title

• C25B11/042

  Electrodes formed of a single material · CPC title

• C25B1/02 Primary

  Hydrogen or oxygen · CPC title