WO2018220664A1 - Valve de commutation de circuit d'écoulement et chromatographe en phase liquide - Google Patents

Valve de commutation de circuit d'écoulement et chromatographe en phase liquide Download PDF

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Publication number
WO2018220664A1
WO2018220664A1 PCT/JP2017/019844 JP2017019844W WO2018220664A1 WO 2018220664 A1 WO2018220664 A1 WO 2018220664A1 JP 2017019844 W JP2017019844 W JP 2017019844W WO 2018220664 A1 WO2018220664 A1 WO 2018220664A1
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WO
WIPO (PCT)
Prior art keywords
flow path
rotor
pressing mechanism
stator
switching valve
Prior art date
Application number
PCT/JP2017/019844
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English (en)
Japanese (ja)
Inventor
統宏 井上
理沙 梶山
研壱 保永
Original Assignee
株式会社島津製作所
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 株式会社島津製作所 filed Critical 株式会社島津製作所
Priority to PCT/JP2017/019844 priority Critical patent/WO2018220664A1/fr
Publication of WO2018220664A1 publication Critical patent/WO2018220664A1/fr

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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16K—VALVES; TAPS; COCKS; ACTUATING-FLOATS; DEVICES FOR VENTING OR AERATING
    • F16K11/00—Multiple-way valves, e.g. mixing valves; Pipe fittings incorporating such valves
    • F16K11/02—Multiple-way valves, e.g. mixing valves; Pipe fittings incorporating such valves with all movable sealing faces moving as one unit
    • F16K11/06—Multiple-way valves, e.g. mixing valves; Pipe fittings incorporating such valves with all movable sealing faces moving as one unit comprising only sliding valves, i.e. sliding closure elements
    • F16K11/072—Multiple-way valves, e.g. mixing valves; Pipe fittings incorporating such valves with all movable sealing faces moving as one unit comprising only sliding valves, i.e. sliding closure elements with pivoted closure members
    • F16K11/074—Multiple-way valves, e.g. mixing valves; Pipe fittings incorporating such valves with all movable sealing faces moving as one unit comprising only sliding valves, i.e. sliding closure elements with pivoted closure members with flat sealing faces
    • 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

Definitions

  • the present invention relates to a rotary flow path switching valve that switches a connection state between flow paths by rotating a rotor, and a liquid chromatograph including the flow path switching valve.
  • a liquid chromatograph is configured to switch whether to introduce a sample loop holding a sample into an analysis flow path by driving a rotary flow path switching valve.
  • Such a rotary flow path switching valve has a disk-shaped stator having a plurality of holes communicating with each of a plurality of connection ports to which a flow path is connected, and a contact surface in contact with the stator. And a rotor provided with a flow path for communicating two or more connection ports on the surface. When the rotor rotates while sliding with the stator, the combination of connection ports communicating with each other through a groove provided on the contact surface of the rotor is switched (see Patent Document 1).
  • the rotor is pressed against the stator by the elastic force of an elastic body such as a spring, and the liquid tightness between the rotor and the stator is maintained. Since the pressure resistance performance of the flow path switching valve is determined by the magnitude of the stress that presses the rotor to the stator side, the high pressure resistance flow path switching valve sets a large pressing force on the rotor, and the low pressure resistance flow path switching valve has a rotor. The pressing force is set small.
  • High friction pressure switching valve has a large frictional force with the stator when the rotor rotates, so the contact surface between the rotor and the stator is easily worn and has a short life compared to low pressure resistance switching valve. For this reason, it is common to select and use a pressure-switching valve having a pressure resistance according to the use environment.
  • analysis may be performed under various conditions, and the liquid feeding pressure varies depending on the analysis conditions.
  • a gradient analysis may be performed in which the composition of the mobile phase is changed over time.
  • the pressure in the analysis channel also changes over time due to a change in the composition of the mobile phase. . Therefore, the pressure resistance of the flow path switching valve is suitable for the maximum pressure during a series of analysis operations.
  • the pressure in the analysis channel reaches the maximum pressure only during some time periods during the series of analysis operations, and the pressure in the analysis channel is lower than that during most of the remaining time periods. . Nevertheless, at all times during the analysis operation, the rotor and stator of the flow switching valve are pressed with a stress corresponding to the maximum pressure during the series of analysis operations, so that the contact surface of the rotor and stator An excessive load will be applied.
  • the present invention has been made in view of the above-described problems, and an object thereof is to reduce an excessive load applied to the contact surface between the rotor and the stator of the flow path switching valve.
  • the flow path switching valve has a plurality of connection ports for connecting flow paths, a stator having a plurality of holes communicating with each of the connection ports, and a contact surface in contact with the stator, A rotor having a flow path for communicating between the connection ports on the contact surface, a drive mechanism for rotationally driving the rotor, and an electric power provided at a position opposite to the stator across the rotor Reads the output signal value from the pressure mechanism that detects the pressure in the flow path connected to the connecting port and the pressing mechanism that presses the rotor to the stator side with the stress according to the signal, and according to the output signal value And a pressing mechanism control unit configured to apply the electrical signal to the pressing mechanism.
  • the “electric signal” applied to the pressing mechanism is a voltage or a current.
  • the electrical signal applied to the pressing mechanism changes according to the pressure in the flow path connected to the connection port of the flow path switching valve, and the magnitude of the stress that presses the rotor to the stator side is increased.
  • Cited Document 2 (WO2012 / 151080) describes using a linear actuator that generates a force according to an applied electric signal to make the force pressing the rotor against the stator variable.
  • the technique disclosed in the cited document 2 reduces the wear of the rotor and the stator when the rotor is rotated by weakening the force applied to the rotor when the rotor is rotating than when the rotor is stationary.
  • the technique disclosed in the cited document 2 changes the force applied to the rotor when the rotor is stationary and when it rotates, and the pressure in the flow path can change during a series of analysis operations. It is not considered at all.
  • the rotor When the rotor is stationary, the rotor is pressed to the stator side with a certain force, and when the rotor rotates, the rotor is only pressed to the stator side with another constant force. Therefore, the present invention is different from the technique disclosed in the cited document 2 in that it corresponds to a necessary change in breakdown voltage during a series of analysis operations.
  • the pressing mechanism may be configured so that a partial area of the contact surface of the rotor can be pressed to the stator side with a stress different from other areas. If it does so, distribution of the stress which presses a rotor to the stator side can be given also in a field. For example, a portion of the rotor contact surface that requires high pressure resistance can be pressed to the stator side with a large stress, and a portion that does not have a problem even if the pressure resistance is low can be pressed to the stator side with a smaller stress. Become. Thereby, the excessive load concerning the contact surface of a rotor and a stator can be reduced.
  • the pressing mechanism includes a plurality of piezo elements that are driven independently of each other, and each piezo element is configured to press different regions on the contact surface of the rotor toward the stator side. Has been.
  • the flow path switching valve includes an applied electrical signal information holding unit that holds applied electrical signal information that defines the applied electrical signal to the pressing mechanism corresponding to the output signal value from the pressure sensor,
  • the pressing mechanism control unit is configured to apply an electric signal derived based on an output signal value from the pressure sensor and the applied electric signal information held in the applied electric signal information holding unit to the pressing mechanism. May be. If comprised in this way, the electric signal applied to a press mechanism can be determined easily.
  • a mobile phase supply channel for supplying a mobile phase by a liquid delivery device, an analysis channel provided with a separation column and a detector, a sample loop for holding a sample, And the above-described channel switching valve configured to selectively switch between the state in which the sample loop is interposed between the mobile phase supply channel and the analysis channel and the state in which the sample loop is not interposed It is.
  • the flow path switching valve according to the present invention is configured such that the magnitude of the stress that presses the rotor toward the stator changes according to the pressure in the flow path connected to the connection port. Excessive load on the contact surface is reduced, and wear of the rotor and the stator is reduced.
  • the liquid chromatograph according to the present invention is configured to selectively switch between a state in which a sample loop is interposed between a mobile phase supply channel and an analysis channel and a state in which no sample loop is interposed between the channel switching valve. Therefore, the maintenance cost can be reduced by extending the life of the flow path switching valve.
  • Fig. 1 shows an example of the configuration of the flow path switching valve.
  • the flow path switching valve 2 of this embodiment is a rotary type switching valve that switches the flow path configuration by rotating the rotor 8 provided inside the valve body 12.
  • the distal end portion 12a of the valve body 12 is provided with a plurality of connection ports 4 for connecting the flow paths.
  • a stator 6 is provided on the side wall surface of the distal end portion 12 a inside the valve body 12. The stator 6 is provided with a hole leading to the connection port 4.
  • a rotor 8, a rotor shaft 10, a bearing 14, a pressing mechanism 16, and the like are provided in the valve body 12.
  • the rotor 8 is a disk-shaped member, and is held by a holding portion 11 provided at the tip of the rotor shaft 10 in a state where the center portion is in contact with the stator 6.
  • the rotor shaft 10 is rotated about the axis by the drive mechanism 20.
  • the rotor 8 is fixed to the holding portion 11 at least in the rotational direction.
  • the drive mechanism 20 that rotationally drives the rotor shaft 10 includes a motor and a gear that transmits the rotation of the motor to the rotor shaft 10.
  • the holding portion 11 provided at the tip of the rotor shaft 10 has an outer diameter larger than that of the rotor shaft 10.
  • a bearing 14 and a pressing mechanism 16 are provided around the rotor shaft 10, and a base end surface 11 a of the holding portion 11 is supported by the bearing 14 and the pressing mechanism 16.
  • the pressing mechanism 16 is composed of a piezoelectric element that expands and contracts in the axial direction of the rotor shaft 10 in accordance with a voltage as an applied electric signal.
  • the base end face (lower end face in the figure) of the pressing mechanism 16 is supported by a support member 19 whose relative position with respect to the valve body 12 is fixed by a screw 18.
  • the front end surface (upper end surface in the drawing) of the pressing mechanism 16 supports the bearing 14. Thereby, the rotor 8 is pressed against the stator 6 side by the stress from the pressing mechanism 16.
  • control unit 22 for controlling the operation of the drive mechanism 20 also has a function of adjusting the magnitude of the voltage applied to the pressing mechanism 16.
  • control unit 22 includes a pressing mechanism control unit 24 and an applied electric signal information holding unit 26.
  • the control unit 22 can be realized by a dedicated computer or a general-purpose personal computer.
  • the pressing mechanism control unit 24 is a function obtained by executing a program in such a computer
  • the applied electric signal information holding unit 26 is a function realized by one area of a storage device provided in such a computer. It is.
  • the control unit 22 receives an output signal from a pressure sensor that detects the pressure in the flow path connected to the connection port 4.
  • the pressing mechanism control unit 24 determines an applied voltage (applied electric signal) to the pressing mechanism 16 based on an output signal from the pressure sensor taken into the control unit 22, and a value that determines the applied voltage to the pressing mechanism 16. It is configured to adjust to.
  • the applied electrical signal information holding unit 26 holds applied electrical signal information that defines the output signal from the pressure sensor taken into the control unit 22 and the applied voltage corresponding thereto.
  • the pressing mechanism control unit 24 is configured to determine an applied voltage value to the pressing mechanism 16 using the applied electric signal information held in the applied electric signal information holding unit 26.
  • the applied electrical signal information is, for example, as shown in Table 1 below.
  • the applied electrical signal information shown in Table 1 divides the pressure value in the flow path detected by the pressure sensor into four levels, and defines the applied voltage value to the pressing mechanism 16 corresponding to each pressure level.
  • the pressing mechanism control unit 24 determines which pressure level in the applied electric signal information the pressure in the flow path detected by the pressure sensor corresponds to, and applies a voltage corresponding to the corresponding pressure level to the pressing mechanism 16. Apply to.
  • the pressing mechanism control unit 24 reads an output signal from the pressure sensor (step S1), and the pressure level in the flow path connected to the connection port 4 is any of the applied electric signal information as shown in Table 1. It is determined whether it corresponds to the pressure level (step S2), and an applied voltage (applied electric signal) to the pressing mechanism is determined (step S3). Then, the voltage applied to the pressing mechanism 16 is adjusted to the determined value (step S4).
  • the control unit 22 takes in the output signal from the pressure sensor at regular intervals, and adjusts the voltage applied to the pressing mechanism 16 by the above operation each time. Thereby, for example, even when the pressure in the flow path connected to the connection port 4 changes with time by gradient analysis, the applied voltage to the pressing mechanism 16 changes according to the pressure change in the flow path. However, the pressure resistance performance changes.
  • the pressing mechanism 16 may be formed of a cylindrical piezo element as shown in FIG. 2, or a plurality of piezo elements 16a, 16b, and 16c may be rotor shafts as shown in FIG. It may be arranged around 10. 2 and 3, in consideration of the visibility of the shape of the pressing mechanism 16, the illustration of the bearing 14 and the like interposed between the holding portion 11 and the pressing mechanism 16 is omitted.
  • the pressing mechanism 16 is configured by the three piezoelectric elements 16a to 16c.
  • the number of piezoelectric elements when the pressing mechanism is configured by a plurality of piezoelectric elements is not limited to this.
  • the pressing mechanism 16 is constituted by a cylindrical piezo element as shown in FIG. 2, the rotor 8 can be pressed uniformly toward the stator 6 side.
  • the rotor 8 is made different by changing the voltage applied to one of the piezo elements 16a, 16b, 16c from the others.
  • the pressure resistance performance can be distributed in the contact surface of the stator 6.
  • the pressure resistance performance between the stator 6 and the rotor 8 is determined by the pressure in the flow path connected to each connection port 4. Accordingly, the required pressure resistance may vary depending on the portion in the contact surface between the stator 6 and the rotor 8.
  • the pressing mechanism 16 includes a plurality of piezo elements 16a to 16c, the pressure resistance performance on the contact surface between the rotor 8 and the stator 6 can be improved for each position where the piezo elements 16a to 16c are provided. Can be variably adjusted.
  • FIG. 5 shows a flow channel configuration when the sample is sucked from the sample container
  • FIG. 6 shows a flow channel configuration when the sucked sample is introduced into the analysis flow channel.
  • the flow path switching valve 2 includes six ports “a” to “f” as connection ports 4. Ports “a” to “f” are arranged in that order counterclockwise on the same circumference.
  • the rotor 8 (see FIG. 1) of the flow path switching valve 2 is provided with three flow paths that connect three adjacent pairs of ports, and the ports “a”-“ f ”,“ b ”-“ c ”, and“ d ”-“ e ”communicated with each other (state shown in FIG. 5), between ports“ a ”-“ b ”,“ c ”-“ d ”and“ e ”-“ f ”are in communication with each other (the state shown in FIG. 6).
  • the injection port 34 is connected to the port “a” of the flow path switching valve 2.
  • the injection port 34 is for inserting the needle 28 and communicating the flow path provided in the needle 28 with the port “a”.
  • the needle 28 is provided at the distal end of the sampling channel 32, and the proximal end of the sampling channel 32 is connected to the port “d” of the channel switching valve 2.
  • the needle 28 can be moved by a driving mechanism (not shown), and can be moved to the position of the container for containing the sample to be analyzed or the position of the injection port 34.
  • a sample loop 30 is provided on the proximal end side of the needle 28 on the sampling flow path 32, and the sample sucked from the tip of the needle 28 is held in the sample loop 30.
  • the ports “b” and “f” adjacent to the port “a” are connected to the downstream analysis channel 50 and the drain channel 56 leading to the drain, respectively.
  • the upstream analysis flow path 42 and the syringe flow path 36 are connected to the ports “c” and “e” adjacent to the port “d”, respectively.
  • the syringe flow path 36 is connected to the syringe pump 40 via a three-way valve 38.
  • the flow path switching valve 2 When the flow path switching valve 2 is brought into a state where the ports “d” and “e” are communicated (the state shown in FIG. 5), the sampling flow path 32 and the syringe flow path 36 are communicated to drive the syringe pump 40.
  • the syringe pump 40 can be connected to a container that stores the cleaning liquid by switching the three-way valve 38, and supplies the cleaning liquid sucked by the syringe pump 40 to the sampling flow path 32. It is comprised so that the inside can be cleaned.
  • the upstream analysis flow path 42 includes a liquid feeding device 44.
  • the liquid feeding device 44 includes a liquid feeding pump 46 that assembles the solvent from a container in which a predetermined solvent is stored and sends the liquid as a mobile phase, and a pressure sensor 48 that detects a liquid feeding pressure by the liquid feeding pump 46.
  • the downstream analysis flow path 50 includes a separation column 52 and a detector 54.
  • the separation column 52 is for separating the sample for each component
  • the detector 54 is for detecting the sample component separated by the separation column 52.
  • the flow path switching valve 2 is brought into communication between the ports “a”-“f”, “b”-“c”, and “d”-“e” (the state shown in FIG. 5) and the needle 28 Is inserted into the sample container, and the syringe pump 40 is inhaled to hold the sample in the sample loop 30. Thereafter, the flow path switching valve 2 is switched to a state where the ports “a”-“b”, “c”-“d”, and “e”-“f” are in communication (the state in FIG. 6).
  • the mobile phase fed by the liquid delivery device 44 flows through the sampling flow path 32, and the sample held in the sample loop 30 is introduced into the downstream analysis flow path 50 together with the mobile phase.
  • the sample introduced into the downstream analysis flow path 50 is separated for each component in the separation column 52, and each component is detected by the detector 54.
  • the pressure in the upstream analysis flow path 42 to which the mobile phase is always sent is the highest pressure. Therefore, the flow path switching valve 2 is required to have a pressure resistance performance corresponding to the pressure in the upstream analysis flow path 42. Therefore, the output signal from the pressure sensor 48 is taken into the control unit 22 having a function of adjusting the pressure resistance performance of the flow path switching valve 2.
  • the pressing mechanism control unit 24 of the control unit 22 applies a voltage to the pressing mechanism 16 (see FIG. 1) of the flow path switching valve 2 based on the pressure value in the upstream analysis flow path 42 detected by the pressure sensor 48. Configured to adjust.
  • the pressing mechanism control unit 24 of the control unit 22 adjusts the voltage applied to the pressing mechanism 16 of the flow path switching valve 2 in accordance with the pressure in the upstream analysis flow path 42, Excessive load on the contact surface of the rotor 8 (see FIG. 1) is suppressed.
  • the pressing mechanism control unit 24 determines the pressure in the upstream analysis flow path 42 that changes with the change in the composition of the mobile phase. Accordingly, the applied voltage to the pressing mechanism 16 of the flow path switching valve 2 is also changed, so that an excessive load on the contact surface between the stator 6 and the rotor 8 of the flow path switching valve 2 is suppressed, and the stator 6 and the rotor 8 are suppressed. It is possible to reduce wear.
  • the present inventors maintain the pressure resistance performance of the flow path switching valve 2 at a constant level in a state corresponding to the maximum value during a series of analysis operations of the liquid feeding pressure by the liquid feeding pump 46, and by the pressure sensor 48. About the case where it adjusted according to the liquid feeding pressure detected, it verified about durability of the flow-path switching valve 2.
  • FIG. As a result, when the pressure resistance performance is maintained constant in a state corresponding to the maximum value of the liquid feeding pressure by the liquid feeding pump 46, liquid leakage occurs between the stator 6 and the rotor 8 in about 25000 switching operations.
  • the pressure resistance performance was adjusted according to the liquid feeding pressure detected by the pressure sensor 48, no liquid leakage occurred between the stator 6 and the rotor 8 even after about 50000 switching operations. From this, it was confirmed that the durability of the flow path switching valve 2 was improved by adjusting the pressure resistance performance of the flow path switching valve 2 according to the liquid feeding pressure.
  • a portion of the contact surface between the stator 6 and the rotor 8 of the flow path switching valve 2 where the ports “b” and “c” are provided always has a high pressure.
  • no high pressure is applied to the portion where the ports “e” and “f” are provided. Therefore, the pressure resistance performance of the portion where the high pressure is applied in the contact surface between the stator 6 and the rotor 8 is variably adjusted based on the output signal from the pressure sensor 48, and the pressure resistance performance of the portion where the high pressure is not applied is kept low and constant. May be.
  • the distribution of the pressure resistance performance in the contact surface between the stator 6 and the rotor 8 is realized by configuring the pressing mechanism 16 of the flow path switching valve 2 with a plurality of piezoelectric elements as shown in FIG. can do. If the pressure resistance performance is distributed in the contact surface between the stator 6 and the rotor 8, an excessive load applied to the contact surface between the stator 6 and the rotor 8 (see FIG. 1) can be suppressed.

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  • General Health & Medical Sciences (AREA)
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Abstract

L'invention concerne une valve de commutation de circuit d'écoulement comprenant : plusieurs orifices de liaison qui relient des circuits d'écoulement ; un stator qui possède plusieurs trous communiquant avec les orifices de liaison respectifs ; un rotor qui possède une surface de contact en contact avec le stator et qui possède, dans la surface de contact, un circuit d'écoulement permettant de communiquer entre les orifices de liaison ; un mécanisme d'entraînement qui entraîne en rotation le rotor ; un mécanisme de pression qui est disposé au niveau d'une position opposée au stator, le rotor étant intercalé entre le mécanisme de pression et le stator, et le mécanisme de pression presse le rotor vers le côté stator au moyen d'une contrainte correspondant à un signal électrique appliqué ; et une unité de commande de mécanisme de pression qui est configurée pour lire une valeur de signal de sortie à partir d'un capteur de pression détectant la pression dans le circuit d'écoulement relié à l'orifice de liaison et pour appliquer un signal électrique correspondant à la valeur de signal de sortie au mécanisme de pression.
PCT/JP2017/019844 2017-05-29 2017-05-29 Valve de commutation de circuit d'écoulement et chromatographe en phase liquide WO2018220664A1 (fr)

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PCT/JP2017/019844 WO2018220664A1 (fr) 2017-05-29 2017-05-29 Valve de commutation de circuit d'écoulement et chromatographe en phase liquide

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PCT/JP2017/019844 WO2018220664A1 (fr) 2017-05-29 2017-05-29 Valve de commutation de circuit d'écoulement et chromatographe en phase liquide

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111561585A (zh) * 2020-05-25 2020-08-21 王伟 一种电动冷热水恒温混水阀芯

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01307575A (ja) * 1988-06-03 1989-12-12 Shimadzu Corp 切換えバルブ
JPH0590067U (ja) * 1992-05-06 1993-12-07 横河電機株式会社 回転式マイクロバルブ
JP2012159460A (ja) * 2011-02-02 2012-08-23 Gl Sciences Inc 切換バルブ
JP2017067484A (ja) * 2015-09-28 2017-04-06 株式会社島津製作所 液体分注装置及び液体分注方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01307575A (ja) * 1988-06-03 1989-12-12 Shimadzu Corp 切換えバルブ
JPH0590067U (ja) * 1992-05-06 1993-12-07 横河電機株式会社 回転式マイクロバルブ
JP2012159460A (ja) * 2011-02-02 2012-08-23 Gl Sciences Inc 切換バルブ
JP2017067484A (ja) * 2015-09-28 2017-04-06 株式会社島津製作所 液体分注装置及び液体分注方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111561585A (zh) * 2020-05-25 2020-08-21 王伟 一种电动冷热水恒温混水阀芯
CN111561585B (zh) * 2020-05-25 2021-10-15 王伟 一种电动冷热水恒温混水阀芯

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