WO2021192929A1 - 送液装置および送液方法 - Google Patents

送液装置および送液方法 Download PDF

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Publication number
WO2021192929A1
WO2021192929A1 PCT/JP2021/008759 JP2021008759W WO2021192929A1 WO 2021192929 A1 WO2021192929 A1 WO 2021192929A1 JP 2021008759 W JP2021008759 W JP 2021008759W WO 2021192929 A1 WO2021192929 A1 WO 2021192929A1
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Prior art keywords
acceleration
liquid feeding
plunger
feeding device
suction
Prior art date
Legal status (The legal status 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 status listed.)
Ceased
Application number
PCT/JP2021/008759
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English (en)
French (fr)
Japanese (ja)
Inventor
大介 秋枝
修大 塚田
祐介 用田
橋本　雄一郎
前田　淳
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Hitachi High Tech Corp
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Hitachi High Tech Corp
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Publication date
Application filed by Hitachi High Tech Corp filed Critical Hitachi High Tech Corp
Priority to EP21774409.3A priority Critical patent/EP4130474B1/en
Priority to CN202180017192.5A priority patent/CN115190942B/zh
Priority to US17/911,469 priority patent/US12153026B2/en
Priority to JP2022509493A priority patent/JP7307271B2/ja
Publication of WO2021192929A1 publication Critical patent/WO2021192929A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B49/00—Control, e.g. of pump delivery, or pump pressure of, or safety measures for, machines, pumps, or pumping installations, not otherwise provided for, or of interest apart from, groups F04B1/00 - F04B47/00
    • F04B49/02—Stopping, starting, unloading or idling control
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B1/00—Multi-cylinder machines or pumps characterised by number or arrangement of cylinders
    • F04B1/02—Multi-cylinder machines or pumps characterised by number or arrangement of cylinders having two cylinders
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B13/00—Pumps specially modified to deliver fixed or variable measured quantities
    • F04B13/02—Pumps specially modified to deliver fixed or variable measured quantities of two or more fluids at the same time
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B49/00—Control, e.g. of pump delivery, or pump pressure of, or safety measures for, machines, pumps, or pumping installations, not otherwise provided for, or of interest apart from, groups F04B1/00 - F04B47/00
    • F04B49/06—Control using electricity
    • F04B49/065—Control using electricity and making use of computers
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B49/00—Control, e.g. of pump delivery, or pump pressure of, or safety measures for, machines, pumps, or pumping installations, not otherwise provided for, or of interest apart from, groups F04B1/00 - F04B47/00
    • F04B49/20—Control, e.g. of pump delivery, or pump pressure of, or safety measures for, machines, pumps, or pumping installations, not otherwise provided for, or of interest apart from, groups F04B1/00 - F04B47/00 by changing the driving speed
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B49/00—Control, e.g. of pump delivery, or pump pressure of, or safety measures for, machines, pumps, or pumping installations, not otherwise provided for, or of interest apart from, groups F04B1/00 - F04B47/00
    • F04B49/22—Control, e.g. of pump delivery, or pump pressure of, or safety measures for, machines, pumps, or pumping installations, not otherwise provided for, or of interest apart from, groups F04B1/00 - F04B47/00 by means of valves
    • 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
    • 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
    • G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B2201/00—Pump parameters
    • F04B2201/02—Piston parameters
    • F04B2201/0202—Linear speed of the piston
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B2201/00—Pump parameters
    • F04B2201/02—Piston parameters
    • F04B2201/0203—Acceleration of the piston
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
    • F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
    • F04B2205/00—Fluid parameters
    • F04B2205/01—Pressure before the pump inlet
    • 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
    • G01N2030/326—Control of physical parameters of the fluid carrier of pressure or speed pumps
    • 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
    • G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
    • G01N2030/347—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient mixers

Definitions

  • the present invention relates to a liquid feeding device and a liquid feeding method.
  • liquid feeding device As a liquid feeding device, for example, it is used for a liquid chromatograph (LC, Liquid Chromatograph).
  • the liquid chromatograph is a chromatograph that uses a liquid as the mobile phase for delivering the sample to be measured, and is introduced into a liquid feeder that sends out a solvent that becomes the mobile phase, an injection device that introduces the sample into the analysis flow path, and an analysis flow path. It consists of a column that separates the sample to be measured into components, and a detection device for detecting each separated component.
  • the separation column that separates the sample to be measured is filled with a filler having physical or chemical properties as a stationary phase, and the difference in affinity between the stationary phase of the separation column and the mobile phase delivered by the liquid feeder
  • the sample to be measured is separated for each component using the above, and each separated component is detected using a detector such as an ultraviolet / visible absorptiometer, a fluorescence photometer, or a mass analyzer.
  • the measurement data of the liquid chromatograph is output as a peak indicating the relationship between the sample separation time (holding time) and the detection signal intensity of the detector, and the holding time is the peak top time, and if the analysis conditions are the same, the sample Since each component shows almost the same value, it is used as information for identifying the separated component.
  • the degree of separation is calculated from the retention time between the components and may be used as an index of separation performance.
  • an analysis method called the gradient elution method is often used.
  • the gradient elution method is a method in which the composition ratio of the mobile phase sent from the liquid feeder is changed over time and sent to the analysis flow path or the separation column, and the affinity between the stationary phase and the solvent which is the mobile phase. By changing, it becomes possible to adjust the separation performance and separation time of the sample components.
  • the method for realizing the gradient elution method is a low-pressure gradient mixing method in which multiple types of mobile phases are mixed on the upstream side of one liquid feeder, and two liquid feeders feed different mobile phases and feed the liquid.
  • a specified volume is sucked from a plurality of types of mobile phases by opening and closing a switching valve called a proportioning valve connected to each mobile phase in synchronization with the suction process of the liquid feeder. It is known that the opening / closing control of the switching valve affects the performance of the gradient elution method and the composition performance of the mixing ratio of the mobile phase.
  • Patent Document 1 discloses operation control of the plunger in the opening / closing operation section of the switching valve, and moves in the section in which the switching valve is opening / closing in order to reduce the influence of variation in the opening / closing operation time of the switching valve. A method of reducing the operating speed of the plunger that sucks the phase or stopping the plunger has been proposed.
  • the method of opening and closing the switching valve during the suction operation of the cylinder is mixed because there is a considerable amount of time that the mobile phase does not flow temporarily due to the influence of pumping that the mobile phase moves back and forth due to the opening and closing operation of the switching valve. It is known that there are events that affect the variation in ratio accuracy, and there are problems that cannot be improved by controlling the opening and closing of the switching valve alone.
  • improving the driving performance of the switching valve in order to improve the mechanical opening / closing time can be considered as one method, but in reality, the machine It is difficult to completely eliminate the variation, and there is a demerit that the cost increases due to the performance confirmation and selection of the switching valve.
  • An object of the present invention is to realize a liquid feeding device and a liquid feeding method capable of delivering a liquid with high accuracy.
  • the present invention is configured as follows.
  • the liquid feeding device has a liquid feeding part having a cylinder that sucks and discharges the solvent by sliding the plunger, and a pressure that is installed on the downstream side of the liquid feeding part and detects the pressure of the discharged solvent.
  • a sensor, at least one switching valve for switching a plurality of the suction and discharge solvents, and a control unit for controlling the operation of the liquid feeding unit and the switching valve are provided, and the control unit is a mixture of the plurality of solvents.
  • the operation of the switching valve is controlled in synchronization with the suction operation of the plunger so that the ratio changes, the plunger is controlled to operate at at least the first acceleration and the second acceleration different from each other, and the plunger is sucked by the plunger. Suppresses the fluctuation of the solvent.
  • a liquid feeding unit having a cylinder that sucks and discharges the solvent by sliding the plunger, a pressure sensor installed on the downstream side of the liquid feeding part and detecting the pressure of the discharged solvent, and suction and discharging.
  • a liquid feeding method of a liquid feeding device including one or more switching valves for switching a plurality of the discharged solvents and a liquid feeding unit and a control unit for controlling the operation of the switching valve, the plurality of solvents are mixed.
  • the switching valve is operated in synchronization with the suction operation of the plunger so that the ratio changes.
  • FIG. 5 is a schematic view of a plunger speed and an opening / closing timing of a switching valve of a liquid feeding device having a low-voltage gradient mixing system according to Example 1 of the present invention.
  • FIG. 5 is a schematic view of a plunger speed and an opening / closing timing of a switching valve of a liquid feeding device having a low-voltage gradient mixing system according to a second embodiment of the present invention.
  • FIG. 5 is a schematic view of a plunger speed and an opening / closing timing of a switching valve of a liquid feeding device having a low-voltage gradient mixing system according to a third embodiment of the present invention.
  • the present invention is not limited to the examples, and is not limited to, for example, regardless of the type and quantity of the switching valve which is a proportioning valve, the type of the liquid feeding device in which the cylinders of the liquid feeding device are connected in series or in parallel, and the like. It is applicable and can be applied within the scope of its technical idea.
  • FIG. 1 is a schematic configuration diagram of an example of a liquid chromatograph device to which the liquid feeding device of the first embodiment is applied.
  • the liquid chromatograph device shown in FIG. 1 has a low-pressure gradient liquid feeding device of a low-pressure gradient mixing system in which one liquid feeding device 105 can supply one or a plurality of mobile phases (solvents). It is a liquid chromatograph device.
  • the liquid chromatograph device includes a liquid feeding device 105 having a sending section (liquid feeding section) 104 that sucks, compresses and discharges a plurality of mobile phases 10101a, 101b, 101c, 101d used for transporting and separating samples.
  • a separation column 107 connected to the sample introduction device 106 on the downstream side of the sample introduction device 106 by a flow path and separating the sample to be measured introduced from the sample introduction device 106 into each component, and a separation column 107 are housed and kept at a constant temperature.
  • a column temperature control device 108 for controlling the state and a detection device 109 for detecting each component of the separated sample connected to the downstream portion of the column temperature control device 108 are provided.
  • the liquid feeding device 105 has switching valves 102a, 102b, 102c, 102d connected to each of the plurality of mobile phases 101a to 101d and switching the plurality of mobile phases, and a confluence point 103 of each mobile phase.
  • the liquid feeding device 105 has a control unit (control unit) 218.
  • the liquid feeding device 105 is a low-pressure gradient liquid feeding device.
  • FIG. 2 is a diagram showing the internal configuration of the delivery unit 104 shown in FIG.
  • the delivery section 104 shown in FIG. 2 is an example of a delivery section in a low-pressure gradient liquid feeding device, and the first cylinder 205 is responsible for suction and delivery of the mobile phase by sliding and reciprocating the plungers 207 and 208.
  • a series type device in which two second cylinders 206 are arranged in series.
  • linear motion mechanisms 213 and 214 for converting rotational motion into linear motion are connected to motors 215 and 216, and plungers 207 and 208 fixed to the linear motion mechanisms 213 and 214 are attached to the sealing materials 211 and 212.
  • the reciprocating motion is repeated in the closed first cylinder 205 and the second cylinder 206.
  • the sending unit 104 sucks the mobile phases 101a to 101d and sends them out.
  • Check valves 209 and 210 for limiting the flow direction of the mobile phases 101a to 101d are connected to the first cylinder 205 that sucks the mobile phases 101a to 101d, and the mobile phase sent out is connected to the downstream portion of the second cylinder 206.
  • a pressure sensor 217 for detecting the pressure of the above is installed.
  • the control unit 218 adjusts the motor speeds of the motors 215 and 216 according to the transmission pressure value detected by the pressure sensor 217 and the set transmission flow rate, and transmits the mobile phases 101a to 101d.
  • the plunger 207 starts the suction operation according to the linear motion mechanism 213 operated by the motor 215, and the pressure in the first cylinder 205 is reduced from the transmission pressure to the atmospheric pressure. ..
  • the closed suction side check valve 209 opens, and suction of the mobile phases 101a to 101d to the first cylinder 205 is started.
  • the control unit 218 determines the opening / closing timing and opening / closing time of the switching valves 102a to 102d according to the set mixing ratio of the mobile phases 101a to 101d, and determines the opening / closing state of the switching valves 102a to 102d according to the determined result. Switch.
  • the first cylinder 205 is sucked so as to realize an arbitrary mixing ratio.
  • the sucked mobile phases 101a to 101d flow into the first cylinder 205 via the confluence 103.
  • the first cylinder 205 finishes the suction step of the mobile phases 101a to 101d, it starts a compression step of compressing the mobile phases 101a to 101d to the delivery pressure.
  • the discharge side check valve 210 is opened and the mobile phases 101a to 101d are sent out by the first cylinder 205. The process is started.
  • the plunger 208 in the second cylinder 206 operates to complement the operation of the first cylinder 205, and the first cylinder 205 is used for the suction step of the mobile phases 101a to 101d and the compression step of the mobile phases 101a to 101d up to the delivery pressure.
  • the second cylinder 206 is responsible for the delivery process.
  • the first cylinder 205 starts sending out the mobile phases 101a to 101d
  • the second cylinder 206 becomes a standby step until the filling step of the mobile phases 101a to 101d into the second cylinder 206 and the sending step of the next cycle.
  • FIG. 3 is a schematic explanatory view of a plunger speed and an opening / closing timing of a switching valve of a liquid feeding device having a low-pressure gradient mixing method according to an example different from the present invention.
  • the switching valve A changes from the closed state to the open state, and after a certain period of time, the switching valve A changes to the closed state. Subsequently, the switching valve B goes from the closed state to the open state, goes to the closed state after a certain period of time, the switching valve C goes from the closed state to the open state, and goes to the closed state after a certain time. The switching valve D is maintained in the closed state.
  • the switching valves A, B, C, and D are opened and closed according to the mixing ratio set in the suction process of the plunger that sucks the mobile phase at a constant speed. Switch the state. As a result, the mobile phase corresponding to the set mixing ratio is sucked into the cylinder.
  • FIG. 4 is a diagram for explaining the pulsation (oscillation) of the mobile phase generated in the suction step in an example different from the present invention.
  • the waveform shown in FIG. 4 shows the operating speed of the plunger at the time of suction of the mobile phase, the change in the flow rate at which the solvent is sucked, and the switching timing of the switching valve, which are obtained from the microfluidic simulation.
  • FIG. 5 is a schematic view of the plunger speed and the opening / closing timing of the switching valves 102a, 102b, 102c, 102d of the liquid feeding device having the low-pressure gradient mixing method according to the first embodiment of the present invention.
  • the control unit 218 controls and opens the target switching valves 102a, 102b, 102c, 102d in synchronization with the suction step.
  • the suction operation of the plungers 207 and 208 is started after a sufficient standby time required for the target of the switching valves 102a, 102b, 102c and 102d to be completely opened, and the mobile phases 101a and 101b, respectively.
  • the plunger operating speed is decelerated at an acceleration of a certain value or less to stop the suction operation.
  • the target switching valves 102a, 102b, 102c and 102d are closed. If there are switching valves 102a, 102b, 102c, 102d to be opened next, the target switching valves 102a, 102b, 102c, 102d are opened, and the suction of the mobile phase is executed in the same process.
  • A, B, C, and D shown in FIG. 5 indicate switching valves 102a, 102b, 102c, and 102d.
  • the movement control of the plungers 207 and 208 shown in FIG. 5 is performed by the control unit 218.
  • the switching valve A changes from the closed state to the open state. Then, the plunger 207 or 208 moves while accelerating from the time point t 1 to the time point t 2, and reaches a constant speed.
  • the acceleration at this time is defined as the first acceleration.
  • the acceleration at this time is defined as the second acceleration.
  • the second acceleration becomes a negative acceleration. Therefore, the second acceleration is synonymous with deceleration.
  • the time from the time point t 1 to the time point t 2 which is the first acceleration is shorter than the time from the time point t 3 to the time point t 4 which is the second acceleration. That is, the absolute value of the first acceleration is larger than the absolute value of the second acceleration, and as shown in FIG. 5, the tilt angle of the first acceleration is larger than that of the second acceleration. It has become.
  • the tilt angle of the second acceleration is about half the tilt angle of the first acceleration.
  • the operation of the switching valves B and C and the operation of the plunger 207 or 208 are performed.
  • the switching valve C remains closed.
  • the operation of the switching valve C changes from the first acceleration to the second acceleration without the plunger 207 or 208 having a constant speed as in the switching valves A and B.
  • the suction operation is followed by the discharge operation, but detailed description will be omitted.
  • a more accurate mobile phase can be obtained by setting the acceleration so that the mobile phase does not fluctuate. Suction can be achieved.
  • the accelerations of the plungers 207 and 208 are set so that the mobile phase does not swing at the end of the final suction process. Therefore, it becomes possible to accurately suck the mobile phase to be sucked in the latter half of the suction process.
  • the first embodiment of the present invention it is possible to realize a liquid feeding device and a liquid feeding method capable of feeding a liquid with high accuracy.
  • Example 2 Next, Example 2 will be described.
  • Example 2 is an example of a low-pressure gradient liquid feeding device of a low-pressure gradient mixing method, as in the case of Example 1.
  • the target switching valve is opened, and a necessary and sufficient waiting time is required until the switching valve is completely opened. After that, the suction operation of the plunger is started.
  • the acceleration is changed stepwise or continuously, and finally the plunger operating speed is set to an acceleration below a certain value. Decelerate and stop the suction operation.
  • Example 2 The difference between Example 2 and Example 1 is the operating acceleration of the plungers 207 and 208.
  • FIG. 6 is a schematic view of the plunger speed and the opening / closing timing of the switching valves 102a, 102b, 102c, and 102d of the liquid feeding device having the low-pressure gradient mixing method according to the second embodiment of the present invention.
  • the operation of the plunger 207 or 208 is the same as the operation shown in FIG. 5 from the time point t 0 to the time point t 3.
  • Example 2 the plunger 207 or 208, from time t 3 to time t 31 to move in the third acceleration from time t 31 to time t 4, the second acceleration as in Example 1 Moving.
  • the third acceleration is a negative acceleration because the plunger 207 or 208 decelerates.
  • the absolute value of the third acceleration is larger than the absolute value of the second acceleration.
  • the plunger 207 or 208 is gradually decelerated.
  • the operation of the plunger 207 or 208 in the opening / closing operation of the switching valve B is the same as the operation of the plunger 207 or 208 in the opening / closing operation of the switching valve A.
  • Operation from time t 5 to time t 6 has the same in the example of FIG. From time t 6 to time t 7, the plunger 207 or 208 to move the third acceleration from time t 7 to the time t 8, moves in the second acceleration.
  • the plunger 207 or 208 is in a decelerated state, and the second acceleration and the third acceleration have negative values. Therefore, the second acceleration and the third acceleration can be defined as the second deceleration and the third deceleration.
  • the second embodiment is an example in which the deceleration of the plunger 207 or 208 is changed stepwise, the deceleration of the plunger 207 or 208 at the start of deceleration is set to be large, and the speed of the plunger 207 or 208 is constant.
  • the time required to stop the plunger 207 or 208 is shortened as compared with the case of the first embodiment while suppressing the fluctuation of the mobile phase when the plunger 207 or 208 is stopped. This makes it possible to appropriately determine the opening / closing time of the switching valve in the mobile phase suction process in which there is a time constraint.
  • Example 3 Next, Example 3 will be described.
  • Example 3 is an example of a low-pressure gradient liquid feeding device of a low-pressure gradient mixing method, as in the first and second embodiments.
  • the target switching valve is opened, and it is necessary and sufficient until the switching valve is completely opened. After a long waiting time, the suction operation of the plunger is started.
  • the acceleration is changed stepwise or continuously, and finally the plunger operating speed is set to an acceleration below a certain value. Decelerate and stop the suction operation.
  • the operating acceleration of the plunger 207 or 208 changes with the first acceleration, the second acceleration, and the third acceleration as in the second embodiment.
  • Example 3 The difference between Example 3 and Example 2 is the set time of the operating dynamic acceleration of the plungers 207 and 208.
  • the switching valves 102a, 102b, 102c, The target of 102d is opened, and the suction operation of the plunger 207 or 208 is started after a necessary and sufficient waiting time until the switching valve is completely opened.
  • suction suction
  • the acceleration is changed stepwise or continuously in order to shorten the time until the plunger 207 or 208 is stopped, and finally constant.
  • the operating speed of the plunger 207 or 208 is decelerated at an acceleration equal to or less than the value to stop the suction operation.
  • the target of the switching valves 102a, 102b, 102c, 102d is closed. If there is a switching valve to be opened next, the target switching valve is opened and suction of the mobile phase is performed in the same process.
  • FIG. 7 is a schematic view of the plunger operating speed and the opening / closing timing of the switching valves 102a, 102b, 102c, 102d of the liquid feeding device having the low-voltage gradient mixing method according to the third embodiment of the present invention.
  • the time point t 1 to the time point t 2 are set longer than the example of FIG. 6, and the time point t 2 to the time point t 3 are set shorter than the example of FIG. Also, from time t 5 to time t 6 is set to be shorter than the example of FIG. 6, from the time t 6 to time t 61, the operation speed of the plunger 207 or 208 is fixed period is set.
  • the suction speed of the plunger 207 or 208 is set according to the mixing ratio, and the acceleration of the plunger 207 or 208 during deceleration is changed stepwise. Then, the acceleration (third acceleration) at the start of deceleration of the plunger 207 or 208 is set to be large, the operating speed of the plunger 207 or 208 becomes equal to or less than a certain value, and then the acceleration is reduced to be the second acceleration.
  • Example 1 the speed at which the speed is constant and the speed changes from the first acceleration to the second acceleration or the third acceleration in the suction operation of any of the solvents 101a, 101b, 101c, and 101d.
  • the speed is the same, in Example 3, the constant speed is changed depending on the type of solvent, and the suction time by the switching valve C is set to be longer than that of Examples 1 and 2.
  • the same effect as that of the second embodiment can be obtained, and the above-mentioned effect can be obtained.
  • the operating speeds of the plunger 207 or 208 are set to three accelerations of the first acceleration, the second acceleration, and the third acceleration, but a fourth acceleration can also be set. Is.
  • the operating speed of the plunger 207 or 208 is changed in a plurality of accelerations in a stepwise manner, but the accelerations are changed in a curve and continuously changed (changed). It is also possible.
  • the configuration is provided with a plurality of switching valves, but a configuration in which a plurality of mobile phases (solvents) of one switching valve are switched may be used.

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  • Pathology (AREA)
  • Computer Hardware Design (AREA)
  • Automatic Analysis And Handling Materials Therefor (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Control Of Positive-Displacement Pumps (AREA)
  • Sampling And Sample Adjustment (AREA)
PCT/JP2021/008759 2020-03-24 2021-03-05 送液装置および送液方法 Ceased WO2021192929A1 (ja)

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CN202180017192.5A CN115190942B (zh) 2020-03-24 2021-03-05 送液装置以及送液方法
US17/911,469 US12153026B2 (en) 2020-03-24 2021-03-05 Liquid feeding apparatus and liquid feeding method
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JP2023117988A (ja) * 2022-02-14 2023-08-24 株式会社島津製作所 液体クロマトグラフ

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JP2023097906A (ja) * 2021-12-28 2023-07-10 株式会社日立ハイテク 送液ポンプ
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US20230091683A1 (en) 2023-03-23
US12153026B2 (en) 2024-11-26
EP4130474A1 (en) 2023-02-08
CN115190942B (zh) 2025-12-02
JP7307271B2 (ja) 2023-07-11
JPWO2021192929A1 (https=) 2021-09-30
CN115190942A (zh) 2022-10-14
EP4130474B1 (en) 2025-10-08

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