Method and system for self-regulating a suppressor

Patent metadata

Field	Value
Publication number	US-2023194484-A1
Application number	US-202117558464-A
Country	US
Kind code	A1
Filing date	Dec 21, 2021
Priority date	Dec 21, 2021
Publication date	Jun 22, 2023
Grant date	—

Abstract

A system for self-regulating a suppressor includes an ion chromatography suppressor, a power supply for applying an electric potential to the suppressor, and a control unit configured to provide an offset voltage Vos and an applied voltage VA to the suppressor, measure a current of the suppressor responsive to the offset and applied voltages VOS and VA, determine a suppressor state of the suppressor based upon the measured current, and adjust the offset voltage Vos based upon the suppressor state. A method for self-regulating a suppressor is also disclosed.

First claim

What is claimed is:

1 . A method for self-regulating a suppressor of an ion chromatography system, the method comprising:
setting a power supply to provide an offset voltage VOS to the suppressor; activating the power supply to provide an applied voltage waveform VA to the suppressor in addition to the offset voltage VOS; commencing an ion chromatography run on the ion chromatography system in which an eluent flows through the suppressor; measuring a current of the suppressor responsive to the offset and applied voltages VOS and VA during the ion chromatography run; determining a suppressor state of the suppressor based upon the measured current in response to the offset voltage; and adjusting the offset voltage VOS based upon the suppressor state, wherein (a) offset voltage VOS is increased for an unsuppressed state, and (b) offset voltage VOS is maintained for a suppressed state.

2 . The method according to claim 1 , wherein a concentration of the eluent is varied with time as the eluent flows through the suppressor, and wherein the adjusting step varies the offset voltage VOS over time in response to the varied concentration of the eluent with time.

3 . The method according to claim 1 , wherein (a) diminishing upper current indicates electrical capacitance and resistance within the suppressor, and (b) substantially constant current indicates substantially constant electrical resistance within the suppressor.

4 . The method according to claim 1 , wherein:
the determining step is also based upon the measured current in response to the offset voltage, wherein (c) increasing upper current indicates an over-suppressed state; and the adjusting step is also based on the suppressor state wherein (c) offset voltage VOS is decreased for an over-suppressed state.

5 . The method according to claim 4 , wherein the oscillating voltage has a voltage amplitude A and a voltage frequency F, and wherein the applied voltage VA is a square-waveform voltage having a positive pulse width and a negative pulse width, and wherein (a) a current slope (SP) of the positive pulse width less than a first predetermined threshold indicates an unsuppressed state, (b) a substantially neutral current slope (SP) of the positive pulse width greater than the first predetermined threshold and less than a second predetermined threshold indicates a suppressed state, and (c) a current slope (SP) of the positive pulse width greater than the second predetermined threshold indicates an over-suppressed state.

6 . The method according to claim 5 , wherein the applied voltage VA is a square waveform voltage having a positive pulse width and a negative pulse width, and the positive pulse width has a slope SP, wherein (a) a slope SP of less than 0.1 mA/s indicates an unsuppressed state, (b) a slope SP of 0.1 mA/s to 0.3 mA/s indicates a suppressed state, and (c) a slope SP greater than 0.3 mA/s indicates an over-suppressed state.

7 . The method according to claim 5 , wherein the applied voltage VA is a square waveform voltage having a positive pulse width and a negative pulse width, and the negative pulse width has a slope SN, wherein (a) a slope SN greater than -0.05 mA/s indicates an unsuppressed state, and (b) a slope SN less than -0.05 indicates a suppressed or over-suppressed state.

8 . The method according to claim 1 , wherein the applied voltage VA is the oscillating voltage having period T, wherein the measuring, determining, and adjusting steps are performed for each period T.

9 . The method according to claim 8 , wherein the adjusting step adjusts the offset voltage VOS by an adjusted voltage ΔV each period T.

10 . The method according to claim 9 , wherein the adjusted voltage ΔV is less than the applied voltage VA.

11 . The method according to claim 10 , wherein the adjusted voltage ΔV is less than 10% of the applied voltage VA.

12 . The method according to claim 11 , wherein the adjusted voltage ΔV is 5 mV.

13 . The method according to claim 4 , wherein increasing upper current indicates increased electrical resistance and thermal effects within the suppressor.

14 . The method according to claim 1 , wherein (a) a diminishing upper current indicates an unsuppressed state of the eluent flowing through the suppressor, and (b) a substantially constant upper current indicates a suppressed state.

15 . A system for self-regulating the separation of ionic species in a liquid sample comprising:
an ion chromatography suppressor including a liquid-sample channel, an ion-receiving channel, and an ion-exchange membrane configured to substantially block bulk liquid flow between the liquid-sample and ion-receiving channels while allowing passage of ions of one charge, positive or negative, between the channels; first and second electrodes in electrical communication with the liquid-sample and ion-receiving channels, respectively; a power supply for applying an electric potential to the suppressor via the first and second electrodes; and a control unit including one or more processors and memory, wherein the one or more processors run software configured to perform the following steps:
setting the power supply to provide an offset voltage VOS to the suppressor;
activating the power supply to provide an applied voltage VA to the suppressor in addition to the offset voltage VOS;
commencing an ion chromatography run in which an eluent flows through the suppressor;
measuring a current of the suppressor responsive to the offset and applied voltages VOS and VA during the ion chromatography run;
determining a suppressor state of the suppressor based upon the measured current in response to the offset voltage; and
adjusting the offset voltage VOS based upon the suppressor state, wherein (a) offset voltage VOS is increased for an unsuppressed state, and (b) offset voltage VOS is maintained for a suppressed state.

16 . The system according to claim 15 , the system further comprising a chromatography column upstream from the suppressor and a conductivity detector downstream from the suppressor.

17 . The system according to claim 15 , wherein the power supply is a dedicated power supply providing the electric potential to the suppressor.

18 . The system according to claim 15 , the system further comprising a power-supply module that includes the power supply and the control unit.

19 . A device for self-regulating the separation of ionic species in a liquid sample comprising:
a power supply configured to apply an electric potential to an ion chromatography suppressor, the suppressor including a liquid-sample channel, an ion-receiving channel, and an ion-exchange membrane configured to substantially block bulk liquid flow between the liquid-sample and ion-receiving channels while allowing passage of ions of one charge, positive or negative, between the channels; and a control unit including one or more processors and memory, wherein the one or more processors run software configured to perform the following steps:
setting the power supply to provide an offset voltage VOS to the suppressor;
activating the power supply to provide an applied voltage waveform VA to the suppressor in addition to the offset voltage VOS;
commencing an ion chromatography run in which an eluent flows through the suppressor;
measuring a current of the suppressor responsive to the offset and applied voltages VOS and VA during the ion chromatography run;
determining a suppressor state of the suppressor based upon the measured current in response to the offset voltage; an

Assignees

• Dionex Corp

Inventors

• Kadjo Akinde F

Classifications

• G01N2030/027

  Liquid chromatography · CPC title

• G01N30/8658 Primary

  Optimising operation parameters · CPC title

• G01N30/64

  Electrical detectors · CPC title

• G01N2030/965

  suppressor columns · CPC title

• G01N30/02

  Column chromatography · CPC title