WO2020250314A1 - 超臨界流体装置および超臨界流体装置における圧力制御方法 - Google Patents

超臨界流体装置および超臨界流体装置における圧力制御方法 Download PDF

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WO2020250314A1
WO2020250314A1 PCT/JP2019/023153 JP2019023153W WO2020250314A1 WO 2020250314 A1 WO2020250314 A1 WO 2020250314A1 JP 2019023153 W JP2019023153 W JP 2019023153W WO 2020250314 A1 WO2020250314 A1 WO 2020250314A1
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Prior art keywords
pressure
flow path
supercritical fluid
target value
intermediate target
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PCT/JP2019/023153
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English (en)
French (fr)
Japanese (ja)
Inventor
道晃 尾和
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Shimadzu Corp
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Shimadzu Corp
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Priority to CN201980096903.5A priority Critical patent/CN113906363B/zh
Priority to PCT/JP2019/023153 priority patent/WO2020250314A1/ja
Priority to JP2021525450A priority patent/JPWO2020250314A1/ja
Priority to US17/616,657 priority patent/US12332221B2/en
Publication of WO2020250314A1 publication Critical patent/WO2020250314A1/ja
Anticipated expiration legal-status Critical
Priority to JP2023131039A priority patent/JP7582402B2/ja
Ceased legal-status Critical Current

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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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
    • B01D15/40—Selective adsorption, e.g. chromatography characterised by the separation mechanism using supercritical fluid as mobile phase or eluent
    • G—PHYSICS
    • G05—CONTROLLING; REGULATING
    • G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
    • G05D16/00—Control of fluid pressure
    • G05D16/20—Control of fluid pressure characterised by the use of electric means
    • 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
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/027—Liquid chromatography
    • 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
    • G01N2030/285—Control of physical parameters of the fluid carrier electrically driven carrier

Definitions

  • the present invention relates to a supercritical fluid device and a pressure control method executed in the supercritical fluid device.
  • supercritical fluid chromatography SFC: Supercritical Fluid Chromatography
  • a supercritical fluid is used as the mobile phase.
  • Supercritical fluids have both liquid and gas properties, and are characterized by higher diffusivity and lower viscosity than liquids.
  • SFE Supercritical Fluid Extraction
  • a supercritical fluid is used as an extraction medium.
  • the flow rate of the solvent is set to a minute flow rate of 3 ml / min or less, and the pressure in the flow path is set to 10 Mpa or more. Therefore, in a supercritical fluid device that performs supercritical fluid chromatography or supercritical fluid extraction, a pressure control device is provided to adjust the pressure in the flow path of the solvent.
  • Patent Document 1 relates to a configuration of a pressure control valve provided in a supercritical fluid chromatograph.
  • a stepping motor and a piezo element are used as an actuator for driving the valve body.
  • the pressure release step of the flow path is executed by controlling the pressure control device. Then, the pressure in the separation column provided in the supercritical fluid chromatograph also decreases from a high pressure of 10 MPa or more to about atmospheric pressure. At this time, due to a sudden drop in pressure, the stationary phase in the separation column may be biased, or a path due to the mobile phase may occur in the stationary phase. If the uniformity of the stationary phase in the separation column is lowered in this way, it causes deterioration of the separation performance in the next analysis process. Further, when the uniformity of the stationary phase of the separation column is lowered, the life of the separation column is shortened.
  • unnecessary components may be extracted from the extraction container and the residue in the extraction container may be collected as the target sample.
  • the sample in the extraction container is disturbed by the sudden fluctuation of the pressure in the flow path.
  • An object of the present invention is to suppress sudden fluctuations in pressure in the flow path in a supercritical fluid device.
  • a supercritical fluid device includes a solvent supply unit that supplies a solvent, a pressure control device provided in a flow path of the solvent supplied by the solvent supply unit, and a control unit that controls the pressure control device. Be prepared.
  • the control unit terminates the first control unit that raises the pressure in the flow path by controlling the pressure control device to maintain the execution environment of the predetermined process in the state of the solvent as a supercritical fluid, and the execution environment of the predetermined process.
  • it includes a second control unit that sets an intermediate target value of the pressure of the flow path and controls the pressure of the flow path toward the intermediate target value.
  • FIG. 1 is an overall view of a supercritical fluid chromatograph according to the present embodiment.
  • FIG. 2 is a flowchart showing a pressure control method according to the present embodiment.
  • FIG. 3 is a diagram showing experimental results using the pressure control method according to the present embodiment.
  • FIG. 1 is an overall configuration diagram of the supercritical fluid chromatograph 10 according to the present embodiment.
  • the supercritical fluid chromatograph 10 includes a carbon dioxide cylinder 1, a modifier tank 2, a first pump 3, a second pump 4, a mixer 5, an autosampler 6, a separation column 7, a detector 8, and a back pressure control valve (BPR:).
  • BPR back pressure control valve
  • a Back Pressure Regulator 9 is provided.
  • Liquefaction carbon dioxide is stored in the carbon dioxide cylinder 1.
  • the liquefied carbon dioxide in the carbon dioxide cylinder 1 is sent to the carbon dioxide flow path R1.
  • An organic solvent as a modifier is stored in the modifier tank 2.
  • the modifier in the modifier tank 2 is sent to the modifier flow path R2.
  • methanol is used as the modifier.
  • the liquefied carbon dioxide fed in the carbon dioxide flow path R1 and the methanol fed in the modifier flow path R2 are mixed in the mixer 5.
  • liquefied carbon dioxide and methanol are used as mobile phases.
  • Carbon dioxide is supercritical at relatively low temperatures and pressures.
  • Modifiers are used to increase the solubility of the sample to be measured.
  • As the modifier another organic solvent such as ethanol may be used.
  • the liquefied carbon dioxide and methanol mixed by the mixer 5 are supplied to the analysis channel AR as a mobile phase.
  • the internal pressure of the analysis flow path AR is adjusted to 10 MPa or more by the back pressure control valve 9 provided downstream of the detector 8.
  • the temperature of the analysis channel AR is adjusted to an appropriate temperature (31.1 degrees or higher) in order to bring carbon dioxide into a supercritical fluid state.
  • the mobile phase supplied to the analysis flow path AR is in the state of a supercritical fluid.
  • the mobile phase supplied to the analysis flow path AR is sent to the autosampler 6.
  • the injector 61 drops the sample onto the mobile phase in the analysis channel AR.
  • the mobile phase, which is the supercritical fluid into which the sample is dropped in the autosampler 6, is sent to the separation column 7.
  • the mobile phase into which the sample is injected is supplied to the separation column 7.
  • the sample is separated while the mobile phase passes through the stationary phase in the separation column 7.
  • the mobile phase in which the sample flowing out from the separation column 7 is dissolved is sent to the detector 8.
  • the detector 8 is supplied with the mobile phase from which the sample was separated in the separation column 7.
  • the detector 8 detects the sample.
  • an ultraviolet detector, a visible light detector, a fluorescence detector, or the like is used as the detector 8.
  • the supercritical fluid chromatograph 10 includes a pressure sensor 11 and a control unit 12.
  • the pressure sensor 11 is provided in the analysis flow path AR through which the mobile phase, which is a supercritical fluid, flows.
  • the pressure sensor 11 is provided in the analysis flow path AR leading from the detector 8 to the back pressure control valve 9.
  • the control unit 12 detects the pressure of the mobile phase, which is a supercritical fluid detected by the pressure sensor 11.
  • the control unit 12 inputs the detected value of the pressure sensor 11.
  • the control unit 12 controls the back pressure control valve 9 based on the detected value of the pressure sensor 11 and the like.
  • the control unit 12 includes a first control unit 121 and a second control unit 122.
  • the first control unit 121 controls the pressure of the mobile phase in the analysis flow path AR while the supercritical fluid chromatograph 10 is executing the analysis process.
  • the first control unit 121 increases the pressure of the analysis flow path AR by controlling the back pressure control valve 9, and keeps the mobile phase in the state of the supercritical fluid to maintain the execution environment of the analysis process.
  • the first control unit 121 maintains the pressure in the analysis flow path AR at 10 MPa or more by controlling the back pressure control valve 9.
  • the first control unit 121 controls the back pressure control valve 9 based on the detected value of the pressure sensor 11.
  • the second control unit 122 controls the pressure release of the analysis flow path AR after the supercritical fluid chromatograph 10 finishes the analysis process.
  • the second control unit 122 controls the back pressure control valve 9 to reduce the pressure in the analysis flow path AR to about atmospheric pressure.
  • the second control unit 122 controls the back pressure control valve 9 based on the detected value of the pressure sensor 11.
  • FIG. 2 is a flowchart showing a pressure control method executed by the second control unit 122.
  • the second control unit 122 executes the pressure control method shown in FIG. 2 after completing the analysis process by the supercritical fluid chromatograph 10.
  • the pressure control method shown in FIG. 2 is a pressure release processing method for the analysis flow path AR.
  • the second control unit 122 executes the pressure control method shown in FIG. 2 in response to an instruction from the operator to end the analysis process or an instruction from the operator to release the pressure.
  • the second control unit 122 acquires the pressure in the current analysis flow path AR from the pressure sensor 11 when the pressure control method shown in FIG. 2 is started. That is, the second control unit 122 acquires the pressure in the analysis flow path AR in the execution environment of the analysis process. For example, the second control unit 122 acquires a detected value of 10 MPa from the pressure sensor 11 as the pressure in the current analysis flow path AR.
  • the second control unit 122 When the pressure control method shown in FIG. 2 is started, the second control unit 122 resets the timer 123 to 0 and starts measuring the elapsed time (T1) during execution of the pressure control method. In step S1, the second control unit 122 acquires the current elapsed time (T1) from the timer 123. In step S1, the second control unit 122 determines whether or not the current elapsed time (T1) exceeds the depressurization set time (T2).
  • the depressurization set time (T2) is the time required for the pressure in the analysis flow path AR to be reduced from the pressure in the execution environment of the analysis process to about atmospheric pressure. That is, the depressurization set time (T2) is the time required to reduce the pressure in the analysis flow path AR for bringing the solvent into a supercritical fluid state to about atmospheric pressure. For example, it is the time required to reduce the pressure in the analysis flow path AR from 10 MPa, which is the pressure during the analysis process, to 0.1 MPa, which is about atmospheric pressure.
  • the pressure in the analysis flow path AR in the execution environment of the analysis process is 10 MPa
  • the depressurization setting time (T2) is set to 200 seconds.
  • step S2 the second control unit 122 calculates the intermediate target value.
  • the intermediate target value is the target value of the pressure in the analysis flow path AR.
  • the second control unit 122 does not set the final target value of atmospheric pressure as the target value of the pressure in the analysis flow path AR, but sets an intermediate target value higher than the final target value.
  • the second control unit 122 first calculates the depressurization speed (V) in order to calculate the intermediate target value.
  • the depressurization speed (V) is obtained by the following equation 1.
  • Depressurization speed (V) set pressure (P) / depressurization set time (T2)
  • the set pressure (P) is a pressure set in the execution environment of the analysis process.
  • the second control unit 122 calculates the intermediate target value by the following equation 2.
  • the second control unit 122 After the intermediate target value is calculated, the second control unit 122 then performs pressure control based on the intermediate target value in step S3.
  • the second control unit 122 acquires the pressure in the current analysis flow path AR from the pressure sensor 11, and performs feedback control based on the difference between the intermediate target value and the acquired pressure.
  • a stepping motor and a piezo element are used as actuators for driving the valve body of the back pressure control valve 9.
  • the stepping motor or the piezo element included in the back pressure control valve 9 is controlled. For example, when the control amount is large, the valve body is driven by the stepping motor, and when the control amount is small, the valve body is driven by the piezo element.
  • the second control unit 122 returns to step S1 after performing pressure control based on the intermediate target value in step S3. Then, the second control unit 122 acquires the elapsed time (T1) from the timer 123. If the elapsed time (T1) does not exceed the depressurization set time (T2), the second control unit 122 executes step S2 again and calculates a new intermediate target value. Then, in step S3, the second control unit 122 performs pressure control based on the new intermediate target value. In this way, the second control unit 122 calculates a new intermediate target value according to the elapsed time (T1), and performs pressure control based on the new intermediate target value. Since the intermediate target value is calculated by the above equation 2, the intermediate target value becomes smaller with the elapsed time (T1).
  • the second control unit 122 repeatedly executes the processes of steps S1 to S3 to gradually reduce the pressure in the analysis flow path AR. Then, in step S1, when the elapsed time (T1) exceeds the depressurization set time (T2), the second control unit 122 ends the pressure control method shown in FIG.
  • the intermediate target value of the pressure in the analysis flow path AR is set, and the analysis flow is directed toward the intermediate target value.
  • a second control unit 122 for controlling the pressure in the road AR is provided.
  • the second control unit 122 controls the pressure in the analysis flow path AR toward the intermediate target value, and then sets a new intermediate target value lower than the intermediate target value. Set and control the pressure in the analysis channel AR towards a new intermediate target value. As a result, the pressure in the analysis flow path AR can be gradually reduced.
  • the intermediate target value of pressure was calculated using Equations 1 and 2.
  • the pressure reduction rate can be adjusted according to the pressure release set time (T2).
  • T2 By adjusting the depressurization set time (T2), it is possible to suppress pressure fluctuations in the analysis flow path AR and prevent deterioration of the separation column 7.
  • the depressurization setting time (T2) is set to 200 seconds after the analysis process of the supercritical fluid chromatograph 10 is completed, which is an example.
  • the optimum depressurization setting time (T2) may be appropriately determined according to the configuration of the supercritical fluid chromatograph 10 or the configuration of the separation column 7. For example, it is preferable to set the depressurization set time (T2) so that the time until the set pressure (P) is halved is at least 10 seconds or more. By setting the depressurization set time (T2) so that the time until the set pressure (P) is halved is 10 seconds or more, sudden fluctuations in the pressure in the analysis flow path AR can be suppressed.
  • the time until the set pressure (P) is halved is 1 minute or more.
  • the depressurization set time (T2) so that the time until the set pressure (P) is halved is 1 minute or more, sudden fluctuations in the pressure in the analysis flow path AR can be more effectively suppressed. Can be done.
  • 200 seconds is set as the depressurization set time (T2), so that the time until the set pressure (P) is halved is about 100 seconds.
  • FIG. 3 is a graph showing the experimental results when the pressure control method of the present embodiment is implemented.
  • the horizontal axis of FIG. 3 is the elapsed time T1 (minutes), and the vertical axis is the pressure (MPa) on the upstream side of the back pressure control valve 9.
  • the graph G1 shown by the solid line is a graph showing the detected value of the pressure sensor 11 when the pressure control method of the present embodiment is executed. That is, the graph G1 is a graph showing the pressure change on the upstream side of the back pressure control valve 9 when the pressure control method according to the present embodiment is executed.
  • the graph G2 shown by the dotted line is a graph showing the detected value of the pressure sensor 11 when the pressure control method of the present embodiment is not executed. That is, the graph G2 is a graph showing the pressure change when the valve body of the back pressure control valve 9 is fully opened at the end of the analysis process and the pressure in the analysis flow path AR is reduced at once.
  • the second control unit 122 controls the pressure toward the intermediate target value, so that the pressure fluctuation becomes gentle. There is.
  • the pressure control method of the present embodiment is not executed, it can be seen that the pressure on the upstream side of the back pressure control valve 9 drops sharply.
  • the reduction rate of the pressure reduced toward the intermediate target value is larger than the reduction rate of the pressure when the pressure is reduced without setting the intermediate target value. It is gradual. As a result, the pressure fluctuation in the flow path can be suppressed as compared with the case where the back pressure control valve 9 is fully opened at once.
  • the supercritical fluid chromatograph 10 is an example of a supercritical fluid device.
  • the carbon dioxide cylinder 1, the modifier tank 2, the first pump 3, the second pump 4, the carbon dioxide flow path R1 and the modifier flow path R2 are examples of the solvent supply unit.
  • the back pressure control valve 9 is an example of the pressure control device
  • the analysis flow path AR is an example of the flow path
  • the analysis process by the supercritical fluid chromatograph 10 is an example of the predetermined process. Is.
  • a supercritical fluid chromatograph 10 has been described as an example of an apparatus using a supercritical fluid.
  • the present invention is also applicable to a device that executes a method (SFE) of extracting a sample with a supercritical fluid as a supercritical fluid device.
  • SFE a method of extracting a sample with a supercritical fluid as a supercritical fluid device.
  • SFE a method of extracting a sample with a supercritical fluid as a supercritical fluid device.
  • the supercritical fluid device includes a solvent supply unit for supplying a solvent and a solvent supply unit.
  • a pressure control device provided in the flow path of the solvent supplied by the solvent supply unit, and A control unit that controls the pressure control device and With
  • the control unit A first control unit that raises the pressure in the flow path by controlling the pressure control device to keep the solvent in a supercritical fluid state and maintains an execution environment for a predetermined process.
  • the execution environment of the predetermined process may include a second control unit that sets an intermediate target value of the pressure of the flow path and controls the pressure of the flow path toward the intermediate target value.
  • the second control unit controls the pressure of the flow path toward the intermediate target value, and then is newer than the intermediate target value.
  • An intermediate target value may be set and the pressure in the flow path may be controlled toward the new intermediate target value.
  • the pressure in the flow path can be gradually reduced.
  • the pressure of the flow path in the execution environment of the predetermined process is set to the set pressure (P), and the time from the start of depressurization to the flow path is set.
  • Intermediate target value set pressure (P)-(depressurization speed (V) x elapsed time (T1)) It may be calculated by.
  • the pressure reduction rate can be adjusted according to the depressurization set time. By adjusting the depressurization setting time, it is possible to suppress the pressure fluctuation in the flow path.
  • the reduction rate of the pressure reduced toward the intermediate target value is the pressure reduction rate when the pressure is reduced without setting the intermediate target value. May be looser than.
  • the intermediate target value is set so that at least 10 seconds or more elapse as a time until the pressure of the flow path in the execution environment of the predetermined process is halved. It may be set.
  • the intermediate target value is set so that at least 1 minute or more elapses as the time until the pressure of the flow path in the execution environment of the predetermined treatment is halved. It may be set.
  • the supercritical fluid device may include a supercritical fluid chromatograph.
  • the supercritical fluid device may include a device that performs supercritical fluid extraction.
  • the pressure fluctuation of the flow path can be suppressed. This prevents the sample in the extraction container from being disturbed.
  • the pressure control method in the supercritical fluid device is A process of increasing the pressure of the flow path by controlling a pressure control device provided in the flow path of the solvent supplied by the solvent supply unit to keep the solvent in a supercritical fluid state and maintaining an execution environment of a predetermined process.
  • a pressure control device provided in the flow path of the solvent supplied by the solvent supply unit to keep the solvent in a supercritical fluid state and maintaining an execution environment of a predetermined process.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
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  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Extraction Or Liquid Replacement (AREA)
PCT/JP2019/023153 2019-06-11 2019-06-11 超臨界流体装置および超臨界流体装置における圧力制御方法 Ceased WO2020250314A1 (ja)

Priority Applications (5)

Application Number Priority Date Filing Date Title
CN201980096903.5A CN113906363B (zh) 2019-06-11 2019-06-11 超临界流体装置及超临界流体装置的压力控制方法
PCT/JP2019/023153 WO2020250314A1 (ja) 2019-06-11 2019-06-11 超臨界流体装置および超臨界流体装置における圧力制御方法
JP2021525450A JPWO2020250314A1 (https=) 2019-06-11 2019-06-11
US17/616,657 US12332221B2 (en) 2019-06-11 2019-06-11 Supercritical fluid apparatus and pressure control method used in supercritical fluid apparatus
JP2023131039A JP7582402B2 (ja) 2019-06-11 2023-08-10 超臨界流体装置および超臨界流体装置における圧力制御方法

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WO2015029253A1 (ja) * 2013-09-02 2015-03-05 株式会社島津製作所 圧力制御バルブ及び超臨界流体クロマトグラフ

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US20220229023A1 (en) 2022-07-21
CN113906363A (zh) 2022-01-07
CN113906363B (zh) 2025-01-14
JP7582402B2 (ja) 2024-11-13
US12332221B2 (en) 2025-06-17
JP2023155278A (ja) 2023-10-20

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