WO2022239652A1 - 圧力センサの調整方法および液体クロマトグラフ分析装置 - Google Patents
圧力センサの調整方法および液体クロマトグラフ分析装置 Download PDFInfo
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- 239000007788 liquid Substances 0.000 title claims abstract description 63
- 238000000034 method Methods 0.000 title claims description 16
- 238000009434 installation Methods 0.000 claims abstract description 34
- 239000000945 filler Substances 0.000 claims abstract description 3
- 238000012937 correction Methods 0.000 claims description 21
- 238000012546 transfer Methods 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- 238000012856 packing Methods 0.000 claims description 7
- 230000005856 abnormality Effects 0.000 claims description 4
- 238000007689 inspection Methods 0.000 abstract description 8
- 238000000926 separation method Methods 0.000 description 8
- 238000010586 diagram Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000011144 upstream manufacturing Methods 0.000 description 2
- 230000005526 G1 to G0 transition Effects 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
Definitions
- the present invention relates to a pressure sensor adjustment method and a liquid chromatograph analyzer.
- a liquid chromatograph is a chromatograph that uses a liquid as the mobile phase sent to a column that separates samples.
- a liquid sample containing an object to be measured introduced from the injection part into the analysis channel is sent to the column by the mobile phase.
- a liquid sample is separated into a plurality of components using the difference in affinity between the stationary phase (filler) packed in the column and the mobile phase.
- Each separated component is detected using a detector such as an ultraviolet/visible absorption photometer, a fluorometer, or a mass spectrometer.
- Liquid chromatographs also known as HPLC (High Performance Liquid Chromatograph) aim to shorten analysis time and improve separation performance. Analysis is performed using compressed liquids.
- HPLC High Performance Liquid Chromatograph
- UHPLC ultra high performance liquid chromatograph
- the devices and channels that make up the liquid chromatograph have high pressure resistance performance. It has been demanded. This is because, as the apparatus becomes more pressurized, pressure leaks from the liquid transfer apparatus and the analysis flow path under a high-pressure environment have a greater influence on the analysis performance. Therefore, the reliability of the pressure sensor that detects the pressure of the liquid transfer device and the analysis channel is required.
- the liquid transfer device may not meet the desired performance, so it is desirable to perform regular inspections and adjustments.
- what the user of the device does as maintenance of the pressure sensor is mainly offset adjustment (Patent Document 1).
- the gain adjustment of the pressure sensor is performed by an engineer with specialized knowledge using dedicated equipment such as an external pressure gauge, which is not easy to implement.
- a column installation part a liquid delivery device that delivers a mobile phase to the column installed in the column installation part, and a pressure sensor that detects the pressure in the flow path from the liquid delivery device to the column installed in the column installation part.
- a method for adjusting a pressure sensor in a liquid chromatograph analyzer comprising A first step of acquiring a first output value P1 of the pressure sensor measured by setting the channel to the atmosphere or by installing a first column not filled with packing material in the column installation part; A second step of obtaining a second output value P2 of the pressure sensor measured by installing a second column having a known pressure resistance Ps in the installation part, and using the first output value P1 and the second output value P2 and a gain update step of updating the gain of the pressure sensor.
- a liquid chromatograph analysis apparatus and a pressure sensor adjustment method that make it possible to easily inspect and adjust a pressure sensor without adding a complicated mechanism.
- FIG. 4 is a flow chart of a pressure sensor inspection/adjustment procedure;
- FIG. 5 is a diagram for explaining pressure correction type gain update processing;
- 1 is a schematic configuration diagram of a liquid chromatograph analyzer according to Example 2.
- FIG. 4 is a flow chart of a pressure sensor inspection/adjustment procedure;
- FIG. 5 is a diagram for explaining pressure correction type gain update processing;
- 1 is a schematic configuration diagram of a liquid chromatograph analyzer according to Example 2.
- the liquid chromatograph analyzer 100 is roughly composed of a mobile phase tank 101, a liquid feed section 102, a sample introduction section 103, a column installation section 104, a detector 105, a control section 112, an operation section 113, and a display section 114. .
- the liquid sending unit 102 includes, for example, a liquid sending device 106, a pressure sensor 107, a channel switching valve 108, a liquid sending channel C0, an analysis channel C1, and a liquid draining channel C2.
- the liquid delivery device 106 sucks the mobile phase used for transporting and separating the sample from the mobile phase tank 101, compresses it under high pressure, and discharges it.
- a configuration example is shown in which one liquid transfer device 106 is used to transfer one type of mobile phase or a mixture of multiple types of mobile phases.
- the pressure sensor 107 detects the pressure in the pipe from the liquid feeding channel C0 for feeding the mobile phase of the liquid feeding section 102 to the column installed in the column installation section.
- the channel switching valve 108 is connected to the downstream side of the liquid delivery device 106, and selectively connects the liquid delivery channel C0 to the analysis channel C1 connected to the sample introduction section 103 or the drainage channel C2. do.
- the column installation part 104 can be replaced with a separation column 109 during analysis and with an empty column 110 or a column 111 with a known pressure resistance during inspection/adjustment of the pressure sensor 107 .
- the separation column 109, the empty column 110, and the column 111 having a known pressure resistance are all connected to the sample introduction section 103 via the analysis channel C3.
- the pressure resistance value of column 111 is Ps.
- the separation column 109 installed in the column installation section 104 separates the sample introduced by the mobile phase from the sample introduction section 103 into each component.
- the detector 105 is connected downstream of the column installation section 104 and detects each component of the sample separated in the separation column 109 .
- the control unit 112 controls the liquid feeding unit 102, the sample introduction unit 103, the column installation unit 104, and the detector 105 to acquire liquid chromatograph data and perform data processing for pressure sensor inspection/adjustment.
- the operation unit 113 includes an input device such as a keyboard, numeric keypad, mouse, etc., and the user inputs various instructions regarding the device to the control unit 112 .
- the display unit 114 is a device for displaying analysis conditions and analysis results, and is composed of, for example, a liquid crystal display or an organic EL display.
- the flow path switching valve 108 is switched to the drainage flow path C2 side, and the flow path provided with the pressure sensor 107 is opened to the atmosphere, and the output value of the pressure sensor 107 is Get P1.
- the output value P1 of the pressure sensor 107 when an empty column 110 filled with no packing material is installed in the column installation section 104 and the pressure resistance is infinitely close to zero, and the liquid is fed under the specified liquid feeding conditions.
- the prescribed liquid feeding conditions are the liquid feeding conditions when the analysis is performed by the liquid chromatograph analyzer 100 .
- the true value of the output value P1 is 0.
- the column 111 having a known pressure resistance (Ps) is installed in the column installation unit 104, and the output value P2 of the pressure sensor 107 when the liquid is fed under the specified liquid feeding conditions is to get
- step S203 and S207 it is determined whether the pressure sensor output value is within the allowable range ( ⁇ Pd) according to (Equation 1).
- -Pd ⁇ (P2-P1)-Ps ⁇ +Pd (Equation 1) is such that the difference (P2-P1) between the output value P2 of the pressure sensor 107 obtained in the second step and the output value P1 of the pressure sensor 107 obtained in the first step becomes the true value (Ps-0).
- step S203 if the output value of the pressure sensor is within the allowable range, the process ends normally, and if it is determined that the output value of the pressure sensor is outside the allowable range, the gain of the pressure correction formula is updated.
- the pressure sensor 107 corrects the detected pressure value by a pressure correction formula and outputs it.
- the pressure correction formula for the pressure sensor 107 is as follows, where P r is the output value (detected value) of the pressure sensor 107 before correction, P m is the output value of the pressure sensor 107 after correction, K G is the gain, and K O is the offset. (Equation 2).
- P m K G (P r -K O ) (equation 2)
- the gain KG is updated so that the output value Pr of the pressure sensor 107 before correction and the output value Pm corrected by the pressure correction formula represented by (Equation 2) indicates a true value.
- the pre-correction output value P r in the second step is set to P0.
- the post-update gain K2 can be updated using (Equation 5).
- step S204 After updating the pressure correction type gain (step S204), the first step (step S205), the second step (step S206), and the pressure sensor output value determination (step S207) are performed again to determine the pressure sensor output value (step S207). is within the allowable range, it terminates normally. If it is out of the allowable range, a pressure sensor abnormality is notified. In this case, there is a possibility that the pressure sensor 107 has an abnormality and a possibility that an abnormality such as a leak has occurred in the liquid transfer device 106 .
- the column 110 was open to the atmosphere or the empty column 110 was used. , and if there is a pressure value that serves as a reference for each, correction is possible. Therefore, instead of the empty column 110, even if a column with a known pressure resistance that is lower in pressure resistance than the column 111 with a known pressure resistance used in the second step (steps S202 and S206) is used, pressure correction can be performed. is possible.
- the pressure sensor 107 can be installed without special knowledge and without adding a complicated mechanism simply by replacing the separation column attached to the column installation section with an empty column or a column with a known pressure resistance. Gain adjustments can be easily performed.
- the liquid chromatograph analyzer 100A is roughly composed of a mobile phase tank 101, a liquid feed section 102, a sample introduction section 103, a column unit 116, a detector 105, a control section 112, an operation section 113, and a display section 114.
- the column unit 116 includes column switching valves 115A and 115B for selectively connecting the separation column 109, the empty column 110, and the column 111 having a known pressure resistance to the analysis flow path, on the upstream side of the column setting sections 104A to 104C. It is equipped on the downstream side.
- the inspection and adjustment of the pressure sensor 107 are performed in the same procedure as in the first embodiment. However, when performing the first step (steps S201 and S205), the empty column 110 is connected to the analysis channel in the column unit 116, and when performing the second step (steps S202 and S206), the column A column 111 with a known pressure resistance is connected to the analysis flow path in unit 116 .
- the columns can be switched by selecting the flow path using the column switching valves 115A and 115B, so that the manual column switching work is unnecessary, and the pressure sensor 107 inspection and adjustment can be automatically performed by the control unit 112. becomes possible.
- SYMBOLS 100 100A... Liquid chromatograph analyzer, 101... Mobile-phase tank, 102... Liquid sending part, 103... Sample introduction part, 104, 104A, 104B, 104C... Column setting part, 105... Detector, 106... Liquid sending apparatus , 107... pressure sensor, 108... channel switching valve, 109... separation column, 110... empty column, 111... column with known pressure resistance, 112... control unit, 113... operation unit, 114... display unit, 115A, 115B... Column switching valve, 116... Column unit.
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Abstract
Description
流路を大気開放状態にして、または、カラム設置部に充填剤が充填されていない第1のカラムを設置して測定した圧力センサの第1出力値P1を取得する第1の工程と、カラム設置部に既知の圧力抵抗Psを有する第2のカラムを設置して測定した圧力センサの第2出力値P2を取得する第2の工程と、第1出力値P1及び第2出力値P2を用いて、圧力センサのゲインを更新するゲイン更新工程とを有する。
-Pd<(P2-P1)-Ps<+Pd (式1)
(式1)は、第2工程で取得した圧力センサ107の出力値P2と第1工程で取得した圧力センサ107の出力値P1の差分(P2-P1)が真の値(Ps-0)に対して、許容範囲(±Pd)内であるか判定するものである。
Pm=KG(Pr-KO) (式2)
補正前の圧力センサ107の出力値Prが(式2)で表される圧力補正式により補正された出力値Pmが真値を示すように、ゲインKGを更新する。なお、オフセットKOについては、第1工程において0=Pm=Pr-KOを満たすよう算出され、更新されている。
(P2-P1)=Pm=K1(P0-KO) (式3)
となっている。
(Ps-0)=Pm=K2(P0-KO) (式4)
となるように、ゲインKGを定めればよい。
K2=K1×Ps/(P2-P1) (式5)
(式5)は(式3)と(式4)より、導くことができる。
Claims (12)
- カラム設置部と、前記カラム設置部に設置されたカラムに移動相を送液する送液装置と、前記送液装置から前記カラム設置部に設置されたカラムに至る流路の圧力を検出する圧力センサとを備える液体クロマトグラフ分析装置における圧力センサの調整方法において、
前記流路を大気開放状態にして、または、前記カラム設置部に充填剤が充填されていない第1のカラムを設置して測定した前記圧力センサの第1出力値P1を取得する第1の工程と、
前記カラム設置部に既知の圧力抵抗Psを有する第2のカラムを設置して測定した前記圧力センサの第2出力値P2を取得する第2の工程と、
前記第1出力値P1及び前記第2出力値P2を用いて、前記圧力センサのゲインを更新するゲイン更新工程とを有する圧力センサの調整方法。 - 請求項1において、
前記ゲイン更新工程は、前記第2出力値P2と前記第1出力値P1の差分と前記圧力抵抗Psとの差が許容範囲を超える場合に実行される圧力センサの調整方法。 - 請求項1において、
前記圧力センサは検知した圧力値Prを圧力補正式により補正して、補正後出力値Pmとして出力する圧力センサであり、
前記圧力センサのゲインKG、オフセットKOとして、前記圧力補正式はPm=KG(Pr-KO)と表される圧力センサの調整方法。 - 請求項3において、
前記第1の工程において、前記圧力センサのオフセットKOを更新する圧力センサの調整方法。 - 請求項4において、
前記ゲイン更新工程において、更新前の前記圧力センサのゲインKGをK1、更新後の前記圧力センサのゲインKGをK2とするとき、
K2=K1×Ps/(P2-P1)
とする圧力センサの調整方法。 - 請求項5において、
前記ゲイン更新工程の実行後に、再度前記第1の工程と前記第2の工程を実行し、再度の前記第1の工程及び前記第2の工程により得られた前記第2出力値P2と前記第1出力値P1の差分と前記圧力抵抗Psとの差が許容範囲を超える場合には異常を報知する圧力センサの調整方法。 - 請求項1において、
前記液体クロマトグラフ分析装置は、複数の前記カラム設置部と、複数の前記カラム設置部に設置されたカラムのいずれか一つを前記流路に接続するカラム切替バルブとを備えるカラムユニットを備え、
前記カラムユニットのある前記カラム設置部には充填剤が充填された第3のカラムが、他の前記カラム設置部には前記第2のカラムが少なくとも設置されている圧力センサの調整方法。 - カラム設置部と、
前記カラム設置部に設置されたカラムに移動相を送液する送液装置と、
前記送液装置から前記カラム設置部に設置されたカラムに至る流路の圧力を検出する圧力センサと、
前記圧力センサの調整を行う制御部とを有し、
前記制御部は、
前記流路を大気開放状態にして、または、前記カラム設置部に充填剤が充填されていない第1のカラムを設置して測定された前記圧力センサの第1出力値P1を取得し、
前記カラム設置部に既知の圧力抵抗Psを有する第2のカラムを設置して測定された前記圧力センサの第2出力値P2を取得し、
前記第1出力値P1及び前記第2出力値P2を用いて、前記圧力センサのゲインを更新する液体クロマトグラフ分析装置。 - 請求項8において、
前記圧力センサは検知した圧力値Prを圧力補正式により補正して、補正後出力値Pmとして出力する圧力センサであり、
前記圧力センサのゲインKG、オフセットKOとして、前記圧力補正式はPm=KG(Pr-KO)と表される液体クロマトグラフ分析装置。 - 請求項9において、
前記制御部は、更新前の前記圧力センサのゲインKGをK1、更新後の前記圧力センサのゲインKGをK2とするとき、
K2=K1×Ps/(P2-P1)
とする液体クロマトグラフ分析装置。 - 請求項8において、
複数の前記カラム設置部と、複数の前記カラム設置部に設置されたカラムのいずれか一つを前記流路に接続するカラム切替バルブとを備えるカラムユニットを有する液体クロマトグラフ分析装置。 - 請求項11において、
前記カラムユニットのある前記カラム設置部には充填剤が充填された第3のカラムが、他の前記カラム設置部には前記第2のカラムが少なくとも設置され、
前記制御部は、前記第2出力値P2を取得するために、前記カラム切替バルブを、前記流路が前記第2のカラムに接続されるよう切り替える液体クロマトグラフ分析装置。
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EP22807354.0A EP4339608A1 (en) | 2021-05-13 | 2022-04-27 | Method for adjusting pressure sensor, and liquid chromatograph analysis device |
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JPH08240578A (ja) * | 1995-01-23 | 1996-09-17 | Hewlett Packard Co <Hp> | ガスクロマトグラフにおける流量センサの補正方法および圧力センサの補正方法 |
JPH10148631A (ja) * | 1996-11-01 | 1998-06-02 | Varian Assoc Inc | クロマトグラフィーカラム用のキャリブレーション方法 |
JP2001174445A (ja) * | 1999-12-17 | 2001-06-29 | Shimadzu Corp | ガスクロマトグラフ装置及びその調整方法 |
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WO2015033664A1 (ja) | 2013-09-03 | 2015-03-12 | 株式会社島津製作所 | 流量調整装置及びこれを備えた分析装置 |
US20150168956A1 (en) * | 2012-02-22 | 2015-06-18 | Agilent Technologies, Inc. | Mass flow controllers and methods for auto-zeroing flow sensor without shutting off a mass flow controller |
JP2018031630A (ja) * | 2016-08-23 | 2018-03-01 | 株式会社島津製作所 | 液体クロマトグラフ用ポンプ |
JP2020094817A (ja) * | 2018-12-10 | 2020-06-18 | 株式会社日立ハイテク | 液体クロマトグラフ質量分析装置 |
WO2020171240A1 (ja) * | 2019-02-22 | 2020-08-27 | 株式会社日立ハイテク | 分析装置 |
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- 2022-04-27 JP JP2023520966A patent/JPWO2022239652A1/ja active Pending
- 2022-04-27 EP EP22807354.0A patent/EP4339608A1/en active Pending
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JPH08240578A (ja) * | 1995-01-23 | 1996-09-17 | Hewlett Packard Co <Hp> | ガスクロマトグラフにおける流量センサの補正方法および圧力センサの補正方法 |
JPH10148631A (ja) * | 1996-11-01 | 1998-06-02 | Varian Assoc Inc | クロマトグラフィーカラム用のキャリブレーション方法 |
JP2001174445A (ja) * | 1999-12-17 | 2001-06-29 | Shimadzu Corp | ガスクロマトグラフ装置及びその調整方法 |
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US20150168956A1 (en) * | 2012-02-22 | 2015-06-18 | Agilent Technologies, Inc. | Mass flow controllers and methods for auto-zeroing flow sensor without shutting off a mass flow controller |
WO2015033664A1 (ja) | 2013-09-03 | 2015-03-12 | 株式会社島津製作所 | 流量調整装置及びこれを備えた分析装置 |
JP2018031630A (ja) * | 2016-08-23 | 2018-03-01 | 株式会社島津製作所 | 液体クロマトグラフ用ポンプ |
JP2020094817A (ja) * | 2018-12-10 | 2020-06-18 | 株式会社日立ハイテク | 液体クロマトグラフ質量分析装置 |
WO2020171240A1 (ja) * | 2019-02-22 | 2020-08-27 | 株式会社日立ハイテク | 分析装置 |
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