Automatic leak detection

Patent metadata

Field	Value
Publication number	US-2025052728-A1
Application number	US-202118719491-A
Country	US
Kind code	A1
Filing date	Dec 16, 2021
Priority date	Dec 16, 2021
Publication date	Feb 13, 2025
Grant date	—

Abstract

Gas is flowed through a gas chromatography column at a first flow rate to cause a first change in pressure defining a first pressure differential. The first pressure differential and/or a first time duration for the first change in pressure is measured. At least one closed exhaust path is opened and a second flow rate through each of the at least one open exhaust paths is set. Gas is flowed through the column at a third flow rate and each of the at least one open exhaust paths at the second flow rate, causing a second change in pressure defining a second pressure differential. The second pressure differential and/or a second time duration for the second change in pressure is measured. A leak is determined based on one or more of measured first pressure differential and/or first time duration and measured second pressure differential and/or second time duration.

First claim

What is claimed is:

1 . A method comprising steps of:
in a gas chromatography system having at least one closed exhaust path, flowing gas through a column of the gas chromatography system at a first flow rate to cause a first change in pressure from a first pressure, the first change defining a first pressure differential, and measuring the first pressure differential and/or a first time duration for the first change in pressure; opening at least one closed exhaust path and setting a respective second flow rate through each of the at least one open exhaust paths; flowing the gas through the column at a third flow rate and each of the at least one open exhaust paths at the respective second flow rate, thereby causing a second change in pressure in the gas chromatography system from a second pressure, the second change defining a second pressure differential, and measuring the second pressure differential and/or a second time duration for the second change in pressure; determining whether there is a leak in the gas chromatography system based on the measured first pressure differential and/or first time duration and measured second pressure differential and/or second time duration.

2 . The method of claim 1 , wherein the step of determining comprises determining there is a leak in the gas chromatography system if the first pressure differential and/or first time duration differ from an expected value established based on the respective second pressure differential and/or the second time duration by more than a threshold amount.

3 . The method of claim 1 , wherein the step of determining comprises determining there is a leak in the gas chromatography system if an amount of gas indicated by the second time duration differs from an expected value established from an amount of gas indicated by the first time duration and/or if an amount of gas indicated by the first time duration differs from an expected value established from an amount of gas indicated by the second time duration by more than a threshold amount.

4 . The method of claim 1 , wherein the step of determining comprises determining there is a leak based on a difference between an expected flow rate and a sum of the first flow rate and the at least one second flow rate that is greater than a threshold amount, wherein the expected flow rate is established based on the first time duration and the second time duration.

5 . The method of claim 1 , wherein flowing gas through the column comprises flowing gas through the column and at least one open exhaust path.

6 . The method of claim 1 , wherein the step of opening at least one exhaust path comprises opening multiple exhaust paths.

7 . The method of claim 1 , wherein one or more of the respective second flow rates are a multiple of the first flow rate and/or wherein the third flow rate is a multiple of the first flow rate.

8 . The method of claim 1 , wherein the at least one exhaust path is one or more of: a septum purge path, a split path and a depressurization path.

9 . The method of claim 1 , wherein the first pressure is equal to the second pressure, the first pressure differential is equal to the second pressure differential and/or the first time duration is equal to the second time duration.

10 . The method of claim 1 , further comprising a step of:
pressurizing the gas chromatography system at the first pressure and the second pressure by opening a gas inlet.

11 . The method of claim 1 , further comprising a step of:
closing the gas inlet prior to the steps of measuring the first time duration and measuring the second time duration.

12 . The method of claim 1 , further comprising a step of:
prior to measuring the first pressure differential and/or first time duration, calibrating the column by determining parameters of the column, wherein the parameters comprise a length and an inner diameter of the column.

13 . The method of claim 1 , wherein the gas chromatography system includes a mass spectrometer.

14 . The method of claim 1 , further comprising a step of:
following a determination that there is a leak, logging, via the gas chromatography system, a record of the determination and providing an indication to a user that a leak has been detected.

15 . The method of claim 1 , further comprising steps of:
following a determination that there is not a leak:
determining a first parameter relating the first pressure differential and the first time duration and/or the second pressure differential and the second time duration;
flowing gas through the column at a further flow rate to cause a further change in pressure from a further pressure, the further change in pressure defining a further pressure differential, and measuring the further pressure differential and/or a further time duration for the further change in pressure; and
determining whether there is a leak based on the first parameter, the further pressure differential and the further time duration.

16 . The method of claim 15 , wherein the step of determining whether there is a leak comprises determining that there is a leak if:
the measured further time duration differs from an expected value established based on the further pressure differential and the first parameter; and/or the measured further pressure differential differs from an expected value based on the further time duration and the first parameter.

17 . The method of claim 15 , wherein the step of determining whether there is a leak comprises:
determining a further parameter relating the further pressure differential and the further time duration; and determining that there is a leak if the further parameter differs from the first parameter by more than a threshold amount.

18 . The method of claim 15 , wherein the first parameter represents a pressure drop per time increment and the step of determining comprises:
determining an additional parameter representing a pressure drop per time increment based on the further pressure differential and the further time duration; and determining that there is a leak if the additional parameter is greater than the first parameter.

19 . A system comprising a gas chromatography arrangement and a controller configured to operate the gas chromatography arrangement in accordance with claim 1 .

20 . A non-transitory storage medium storing machine-executable instructions that, when executed, cause a computing device to perform the steps of claim 1 .

Assignees

• Thermo Fisher Scient S P A
• Thermo Finnigan Llc

Inventors

• Facchetti Riccardo
• Magni Paolo
• Quarmby Scott T
• Srinivasan Kannan

Classifications

• G01N2030/025

  Gas chromatography · CPC title

• G01M3/26

  by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors · CPC title

• G01N30/32 Primary

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