CN117571897A - Liquid chromatograph-mass spectrometer and switching device - Google Patents

Liquid chromatograph-mass spectrometer and switching device Download PDF

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Publication number
CN117571897A
CN117571897A CN202311525896.0A CN202311525896A CN117571897A CN 117571897 A CN117571897 A CN 117571897A CN 202311525896 A CN202311525896 A CN 202311525896A CN 117571897 A CN117571897 A CN 117571897A
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CN
China
Prior art keywords
liquid
fixedly connected
driving
chassis
valve body
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Application number
CN202311525896.0A
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Chinese (zh)
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CN117571897B (en
Inventor
刘传兴
韩文念
张曼玉
杲立博
牛天渭
董丹丹
公翠娟
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Qingdao Huiankang Bioengineering Co ltd
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Qingdao Huiankang Bioengineering Co ltd
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Priority to CN202311525896.0A priority Critical patent/CN117571897B/en
Priority claimed from CN202311525896.0A external-priority patent/CN117571897B/en
Publication of CN117571897A publication Critical patent/CN117571897A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/16Injection
    • G01N30/20Injection using a sampling valve
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/62Detectors specially adapted therefor
    • G01N30/72Mass spectrometers
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N2030/022Column chromatography characterised by the kind of separation mechanism
    • G01N2030/027Liquid chromatography

Abstract

The invention discloses a liquid chromatograph-mass spectrometer and a switching device, which relate to the technical field of analysis equipment and comprise a waste liquid barrel and a switching mechanism, wherein the waste liquid barrel is fixedly connected with a waste liquid pipe, the switching mechanism comprises a frame body, a valve core, an upper valve body, a lower valve body, a chassis and a switching piece for driving the valve core and the chassis to rotate, the upper valve body is fixedly connected with the frame body, the lower valve body is rotationally connected with the frame body, a plurality of feeding cavities are formed in the upper valve body, the feeding cavities are arranged along the circumferential angle of the upper valve body, a discharging cavity and a waste liquid cavity are formed in the lower valve body, a plurality of liquid inlets, liquid outlets and waste liquid outlets are formed in the valve core, the liquid inlets are arranged at equal-angle equal intervals along the upper end of the valve core, the liquid outlets and the waste liquid outlets are symmetrically arranged at the lower end of the valve core about the vertical axis of the valve core, a first pipeline is communicated between one liquid inlet and the liquid outlet, the waste liquid outlets are communicated with the waste liquid pipeline, the rest liquid inlets are communicated with the waste liquid pipeline, the lower valve body is fixedly connected with the chassis, and the waste liquid pipe. The method has the effect of improving the actual working time of the mass spectrometer.

Description

Liquid chromatograph-mass spectrometer and switching device
Technical Field
The invention relates to the technical field of analysis equipment, in particular to a liquid chromatograph-mass spectrometer and a switching device.
Background
The mass spectrometer is an instrument for separating and detecting different isotopes, namely, according to the principle that charged particles can deflect in an electromagnetic field, a process of detecting substances is carried out according to the mass difference of substance atoms, molecules or molecular fragments, and can effectively analyze constituent elements and components of the substances.
When the mass spectrometer works, the detected substances are ionized under the high vacuum condition, ionized molecules are further broken into fragment ions and neutral particles with smaller mass, and average kinetic energy with the same energy is obtained under the action of an accelerating electric field and enters the mass analyzer.
When analyzing to same sample, the liquid chromatograph is generally longer to the separation of sample and analysis process time spent, and when chromatograph and mass spectrometer are parallelly connected one to one, the actual analysis time of mass spectrometer is shorter, is in idle state and mass spectrometer continuously keeps operating condition always for the utilization ratio of mass spectrometer is lower, and actual operating time duty ratio is too low, has caused the waste on the resource.
Disclosure of Invention
In order to improve the actual working time of a mass spectrometer, the application provides a liquid chromatograph-mass spectrometer and a switching device.
In a first aspect, the present application discloses a switching device, which adopts the following technical scheme:
the utility model provides a switching device, includes waste liquid bucket and switching mechanism, waste liquid bucket fixedly connected with waste liquid pipe, switching mechanism includes the support body, the case, go up the valve body, lower valve body, the chassis and drive case and chassis pivoted switchover piece, go up valve body and support body fixed connection, lower valve body and support body rotation are connected, go up the valve body and seted up a plurality of feed chambers, the feed chamber sets up along last valve body circumference angle, discharge chamber and waste liquid chamber have been seted up to lower valve body, a plurality of feed inlets, liquid outlet and waste liquid mouth have been seted up to the case, the equal angle equidistance of feed inlet along case upper end sets up, liquid outlet and waste liquid mouth set up in the case lower tip about the vertical axis symmetry of case, the intercommunication has pipeline one between one of them feed inlet and the liquid outlet, the waste liquid mouth intercommunication has the waste liquid pipeline, remaining feed inlet all is linked together with the waste liquid pipeline, lower valve body and chassis fixed connection, waste liquid pipe and chassis fixed connection.
Through adopting above-mentioned technical scheme, the feed liquor mouth of case can rotate along with the case together for the feed liquor mouth constantly takes place to switch with the intercommunication condition of feed cavity, wherein a liquid chromatograph that finishes after working carries to the liquid outlet department after getting into pipeline one with the feed liquor mouth that is linked together of pipeline one with the sample after, the liquid outlet then is linked together with the mass spectrometer, accomplish the process of introducing sample to the mass spectrometer, and other liquid chromatographs that are working are then in with mobile phase discharge waste liquid pipeline through other feed liquor mouths, make mobile phase get into the waste liquid bucket in, the switchover piece can drive the case and rotate, make the feed liquor mouth that is linked together with pipeline one carry out cyclic switching between different feed cavities, different liquid chromatographs can carry out alternate feed to the mass spectrometer through this feed liquor mouth, the actual operating time of mass spectrometer has been increased, the waste of resource has been reduced.
Optionally, the switching piece includes driving motor, bull stick, is used for driving the chassis and rotates along with the synchronous driving piece of case and be used for the reset piece that resets of chassis, bull stick and the coaxial fixed connection of case, bull stick coaxial fixed connection have from the driving wheel, driving motor output shaft fixedly connected with action wheel one, action wheel one meshes with from the driving wheel.
Through adopting above-mentioned technical scheme, driving motor can drive the bull stick through action wheel one and follow the driving wheel and rotate, accomplishes the unidirectional rotation of case, and the driving piece drives chassis and lower valve body and rotates along with the case together for feed cavity one, inlet one, pipeline one and feed liquor pipe communicate each other all the time, establish inlet quantity for N, after the case carries out (N-1) switching, reset piece drives chassis and lower valve body and resets, makes feed liquor pipe and waste liquid pipe be difficult for intertwine each other.
Optionally, the driving piece includes action wheel two and drive ring, and drive ring cover locates the lower valve body outside and sets up with the chassis is coaxial, and the rotation radius of action wheel two is the same with the rotation radius of action wheel one, and drive ring and follow driving wheel are the same, action wheel two and driving motor output shaft sliding connection, driving motor output shaft fixedly connected with spacing, action wheel two have seted up the spacing groove with spacing looks adaptation, action wheel two meshes with drive ring, and drive ring fixedly connected with lug, and the recess with lug looks adaptation is seted up to the chassis.
Through adopting above-mentioned technical scheme, driving motor accessible spacing and the cooperation of spacing groove drive action wheel two rotates, and then drive the driving ring and rotate, action wheel two and action wheel one rotate the radius the same, the driving ring is the same with the radius of rotation from the driving wheel, make driving motor can drive from driving wheel and driving ring and rotate with synchronous equiangular, the cooperation of driving ring accessible lug and recess drives chassis and lower valve body and rotates, the rotation angle of chassis and case has been guaranteed to be the same, after chassis and lower valve body carry out the switching many times along with the case, establish inlet quantity and be N, then (N-1) time after switching, reset piece drives the chassis and resets, make the chassis resume initial state, and the case then continues to rotate, resume initial state's corresponding condition between case and the chassis, circulation and the switching of next cycle can continue.
Optionally, the piece that resets includes stopper, dog, torsional spring and is used for driving the moving part that drive ring and action wheel second removed along self axis direction in step, torsional spring fixed connection between support body and chassis, stopper and support body fixed connection, dog and chassis lower terminal surface fixed connection.
Through adopting above-mentioned technical scheme, the moving part can drive the actuating ring and remove for after lug and recess separation, under the elasticity effect of torsional spring, reverse rotation takes place for chassis and lower valve body, and the dog rotates together with the chassis and inconsistent with the stopper, and the stopper is spacing to the dog, makes the chassis can accurately resume initial condition.
Optionally, the moving part includes movable motor, threaded rod, gag lever post and movable block, movable motor output shaft and threaded rod coaxial fixed connection, the threaded rod wear to establish the movable block and with movable block threaded connection, gag lever post and support body fixed connection, the gag lever post wear to establish the movable block and with movable block sliding connection, the spout with drive ring looks adaptation is seted up to the movable block, the drive ring is located the spout and offsets with the movable block and contacts, drive ring is along two annular baffles of circumference fixedly connected with, action wheel two lie in between two annular baffles and with annular baffle inconsistent.
Through adopting above-mentioned technical scheme, mobile motor drives the threaded rod and rotates for the movable block removes along threaded rod length direction, and the spout is spacing to the drive ring, makes the movable block drive the drive ring and removes, and two annular baffles are inconsistent with the action wheel, make the second driving wheel move along with the drive ring, separate lug and recess, the torsional spring of being convenient for drive the drive ring and carry out reverse rotation.
Optionally, the frame body is provided with a controller, and the driving motor and the moving motor are electrically connected with the controller.
By adopting the technical scheme, the controller can set time to enable the mobile motor and the driving motor to periodically work, and the switching of the valve core and the resetting of the chassis are completed.
Optionally, the upper valve body is provided with a cleaning cavity, the upper valve body is fixedly connected with a cleaning pipe communicated with the cleaning cavity, and the other end of the cleaning pipe is communicated with a cleaning tank filled with cleaning liquid.
Through adopting above-mentioned technical scheme, when the switching mechanism live time is longer, the washing liquid accessible washs the pipe in the wash tank and gets into and washs the chamber, rotates the case and makes pipeline one be linked together with wasing the chamber, can wash pipeline one.
Optionally, the feed liquor pipe fixedly connected with branch pipe one, the wash pipe fixedly connected with branch pipe two, the other end fixedly connected with blowing equipment of branch pipe one, branch pipe one is equipped with the check valve one that cuts off liquid and flow from the feed liquor pipe to blowing equipment, and the wash pipe is equipped with the check valve two that cuts off gas and flow from the wash pipe to wash jar, and the feed liquor pipe is equipped with the check valve three that cuts off gas and flow from the branch pipe to the mass spectrometer, and branch pipe two is connected with the stagnant water clamp.
Through adopting above-mentioned technical scheme, the inert gas after the gas blowing equipment can blow in to branch pipe I, and gas is restricted by check valve two and check valve three, flows through branch pipe I, feed liquor pipe, case, wash pipe and branch pipe two in proper order, can blow out the residual liquid in the route of flowing through for the drying rate of route of flowing through, check valve one can make the sample be difficult for flowing out from branch pipe one, and the stagnant water presss from both sides can make the washing liquid be difficult for flowing out from branch pipe two, is favorable to reducing the waste of sample and washing liquid.
In a second aspect, the application discloses a liquid chromatograph-mass spectrometer, which adopts the following scheme:
a liquid chromatograph-mass spectrometer, comprising a switching device, a plurality of liquid chromatographs and mass spectrometers according to any one of claims 1-8, wherein the liquid chromatographs are fixedly connected with liquid outlet pipes, the mass spectrometers are fixedly connected with liquid inlet pipes, the liquid outlet pipes are in one-to-one correspondence with the feed cavities and are mutually communicated, and the liquid inlet pipes are fixedly connected with a chassis and are symmetrically arranged with the waste liquid pipes.
Through adopting above-mentioned technical scheme, all liquid chromatograph all communicate with auto-change over device, and auto-change over device can realize the intercommunication between mass spectrometer and the different liquid chromatograph through the auto-change over piece for liquid chromatograph can carry the sample after the analysis in the mass spectrometer according to order alternative circulation, has reduced the work sky window period of mass spectrometer, and then has reduced the waste of resource.
In summary, the present application includes at least one of the following beneficial technical effects:
1. through setting up the shifter, the feed liquor mouth of case can rotate along with the case together for the feed liquor mouth constantly takes place to switch with the intercommunication condition of feed cavity, wherein a liquid chromatograph that finishes after working carries to the liquid outlet department after getting into pipeline one through the feed liquor mouth that is linked together with pipeline one with the sample after, the liquid outlet then is linked together with the mass spectrometer, accomplish the process of introducing into the mass spectrometer, and other liquid chromatographs that are working then in will mobile phase through other feed liquor mouths in the waste liquid pipeline, make mobile phase get into in the waste liquid bucket, the shifter can drive the case and rotate, make the feed liquor mouth that is linked together with pipeline one carry out cyclic switching between different feed cavities, different liquid chromatographs can carry out alternate feeding to the mass spectrometer through this feed liquor mouth, the actual operating time of mass spectrometer has been increased, the waste of resource has been reduced.
Drawings
Fig. 1 is a schematic diagram of the overall structure of a liquid chromatograph-mass spectrometer and a switching device.
Fig. 2 is a schematic overall structure of the switching mechanism.
Fig. 3 is a schematic perspective view of the upper valve body, the lower valve body and the valve core in an initial state.
Fig. 4 is a schematic view of a part of the structure aimed at highlighting the blowing device, the branch pipe one and the branch pipe two.
Reference numerals illustrate: 1. a first liquid chromatograph; 11. a liquid outlet pipe I; 2. a second liquid chromatograph; 21. a liquid outlet pipe II; 3. a third liquid chromatograph; 31. a liquid outlet pipe III; 4. a mass spectrometer; 41. a liquid inlet pipe; 411. a third check valve; 5. a waste liquid barrel; 51. a waste liquid pipe; 6. a switching mechanism; 61. a frame body; 611. a controller; 62. a valve core; 621. a first liquid inlet; 622. a liquid inlet II; 623. a liquid inlet III; 624. a liquid outlet; 625. a waste liquid port; 626. a first pipeline; 627. a second pipeline; 628. a third pipeline; 629. a waste liquid pipeline; 63. an upper valve body; 631. a first feeding cavity; 632. a second feeding cavity; 633. a third feeding cavity; 634. cleaning the cavity; 635. cleaning the tube; 6351. a second check valve; 636. a cleaning tank; 637. a branch pipe I; 6371. a first check valve; 638. a branch pipe II; 6381. a water stop clamp; 639. a blowing device; 64. a lower valve body; 641. a discharge cavity; 642. a waste liquid chamber; 65. a chassis; 7. a switching member; 71. a driving motor; 711. a first driving wheel; 72. a rotating rod; 721. driven wheel; 731. a driving wheel II; 732. a drive ring; 733. a limit bar; 734. a limit groove; 74. a reset member; 741. a limiting block; 742. a torsion spring; 743. a stop block; 744. a moving member; 7441. a moving motor; 7442. a threaded rod; 7443. a limit rod; 7444. a moving block; 7445. a chute; 7446. an annular baffle.
Detailed Description
The present application is described in further detail below with reference to the accompanying drawings.
The embodiment of the application discloses a liquid chromatograph-mass spectrometer and a switching device.
In this embodiment, the number of liquid chromatographs is preferably 3, which is sequentially set as a first liquid chromatograph 1, a second liquid chromatograph 2 and a third liquid chromatograph 3, the liquid outlet is sequentially set as a first liquid outlet 11, a second liquid outlet 21 and a third liquid outlet 31, the liquid inlet is sequentially set as a first liquid inlet 621, a second liquid inlet 622 and a third liquid inlet 623, and the feeding cavity is sequentially set as a first feeding cavity 631, a second feeding cavity 632 and a third feeding cavity 633, wherein a first pipeline 626 is communicated between the first liquid inlet 621 and the liquid outlet 624, a second pipeline 627 is communicated with the second liquid inlet 622, a third pipeline 628 is communicated with the third liquid inlet 623, and both the second pipeline 627 and the third pipeline 628 are communicated with the waste liquid pipeline 629.
Referring to fig. 1 and 2, a liquid chromatograph-mass spectrometer includes a first liquid chromatograph 1, a second liquid chromatograph 2, a third liquid chromatograph 3, a mass spectrometer 4 and a switching device, the switching device includes a waste liquid barrel 5 and a switching mechanism 6, the liquid chromatograph can separate and analyze an initial sample, the first liquid chromatograph 1, the second liquid chromatograph 2 and the third liquid chromatograph 3 can separate and analyze three different samples, and parameters are manually set so that sample discharge times of the first liquid chromatograph 1, the second liquid chromatograph 2 and the third liquid chromatograph 3 are staggered, namely, in one period, the discharge time of the second liquid chromatograph 2 is after the first liquid chromatograph 1, the storage time of the third liquid chromatograph 3 is after the second liquid chromatograph 2, and the discharge time of the first liquid chromatograph 1 in the next period is after the third liquid chromatograph 3 in the current period, the first liquid chromatograph 1, the second liquid chromatograph 2 and the third liquid chromatograph 3 are alternately discharged, so as to provide analysis samples for the mass spectrometer 4.
Referring to fig. 1 and 2, a first liquid chromatograph 1 is fixedly connected with a first liquid outlet pipe 11, a second liquid chromatograph 2 is fixedly connected with a second liquid outlet pipe 21, a third liquid chromatograph 3 is fixedly connected with a third liquid outlet pipe 31, the first liquid chromatograph 1 discharges a mobile phase and an analysis sample outwards through the first liquid outlet pipe 11, the second liquid chromatograph 2 discharges the mobile phase and the analysis sample outwards through the second liquid outlet pipe 21, and the third liquid chromatograph 3 discharges the liquid chromatograph and the analysis sample outwards through the third liquid outlet pipe 31.
Referring to fig. 2 and 3, the switching mechanism 6 includes a frame 61, a valve core 62, an upper valve body 63, and a lower valve body 64, the upper valve body 63 is fixedly connected with the frame 61, the lower valve body 64 is rotatably connected with the frame 61, the valve core 62 is located between the upper valve body 63 and the lower valve body 64, and the upper valve body 63 is in contact with the lower valve body 64. The upper valve body 63 is provided with a first feeding cavity 631 communicated with the first liquid outlet pipe 11, a second feeding cavity 632 communicated with the second liquid outlet pipe 21 and a third feeding cavity 633 communicated with the third liquid outlet pipe 31, a sample or a mobile phase in the first liquid chromatograph 1 enters the first feeding cavity 631 through the first liquid outlet pipe 11, a sample or a mobile phase in the second liquid chromatograph 2 enters the second feeding cavity 632 through the second liquid outlet pipe 21, and a sample or a mobile phase in the third liquid chromatograph 3 enters the third feeding cavity 633 through the third liquid outlet pipe 31.
Referring to fig. 1 and 3, the valve core 62 is provided with a first liquid inlet 621, a second liquid inlet 622, a third liquid inlet 623, a liquid outlet 624 and a liquid outlet 625, wherein the first liquid inlet 621, the second liquid inlet 622 and the third liquid inlet 623 are equidistantly arranged along the upper end of the valve core 62 at equal angles, that is, when the first liquid inlet 621 is communicated with the first feeding cavity 631, the second liquid inlet 622 is communicated with the second feeding cavity 632, and the third liquid inlet 623 is communicated with the third feeding cavity 633, which is the initial state of the valve core 62.
Referring to fig. 1 and 3, a mass spectrometer 4 is fixedly connected with a liquid inlet pipe 41, a sample can enter the mass spectrometer 4 through the liquid inlet pipe 41 for analysis, a waste liquid barrel 5 is fixedly connected with a waste liquid pipe 51, a mobile phase can flow into the waste liquid barrel 5 through the waste liquid pipe 51 for storage, a liquid outlet 624 and a waste liquid outlet 625 are formed in the lower end part of a valve core 62, a first pipeline 626 is communicated between the first liquid inlet 621 and the liquid outlet 624, and the sample can flow out of the first liquid chromatograph 1 and sequentially flows through the first liquid outlet pipe 11, the first liquid inlet 621, the first pipeline 626 and the liquid outlet 624.
Referring to fig. 1 and 3, the lower valve body 64 is provided with a discharge cavity 641 and a waste liquid cavity 642, in an initial state, the liquid outlet 624 is communicated with the discharge cavity 641, the lower valve body 64 is fixedly connected with a chassis 65, the liquid inlet tube 41 and the waste liquid tube 51 are fixedly connected with the chassis 65, the liquid inlet tube 41 is communicated with the discharge cavity 641 at this time, so that a sample flows through the discharge cavity 641 and enters the liquid inlet tube 41, and the sample injection process of the sample to the mass spectrometer 4 is completed.
Referring to fig. 1 and 3, the second liquid inlet 622 is communicated with a second pipeline 627, the third liquid inlet 623 is communicated with a third pipeline 628, the waste liquid inlet 625 is communicated with a waste liquid pipeline 629, at this time, the second liquid inlet 622 is communicated with the second feeding cavity 632, the third liquid inlet 623 is communicated with the third feeding cavity 633, so that mobile phases discharged during operation of the second liquid chromatograph 2 and the third liquid chromatograph 3 are respectively discharged through the second liquid outlet 21 and the third liquid outlet 31 and enter the second feeding cavity 632 and the third feeding cavity 633 which are communicated, the lower end parts of the second pipeline 627 and the third pipeline 628 are communicated with the upper end part of the waste liquid pipeline 629, and the mobile phases are converged into the waste liquid pipeline 629 along the second pipeline 627 and the third pipeline 628.
Referring to fig. 1 and 3, the liquid outlet 624 and the liquid outlet 625 are symmetrically arranged about the vertical axis of the valve core 62, so when the liquid outlet 624 is communicated with the discharge cavity 641, the liquid outlet 625 is communicated with the liquid outlet cavity 642, so that the mobile phase in the liquid outlet pipeline 629 finally enters the liquid outlet cavity 642 through the liquid outlet 625, flows through the liquid outlet 51 and enters the liquid outlet barrel 5 for storage, and the discharge time of the first liquid chromatograph 1, the second liquid chromatograph 2 and the third liquid chromatograph 3 are staggered, so that the first feeding cavity 631 feeds samples, and the second feeding cavity 632 and the third feeding cavity 633 discharge the mobile phase, which is the initial flowing condition of the valve core 62 and the valve body.
Referring to fig. 2 and 3, the switching mechanism 6 further includes a switching member 7 for driving the valve core 62 and the chassis 65 to rotate, the switching member 7 includes a driving motor 71 and a rotating rod 72, an output shaft of the driving motor 71 is fixedly connected with a driving wheel one 711, the driving motor 71 can drive the driving wheel one 711 to rotate, the rotating rod 72 is coaxially and fixedly connected with a driven wheel 721, the driving wheel one 711 is meshed with the driven wheel 721, the driven wheel 721 rotates along with the driving wheel one 711, and the rotating rod 72 is coaxially and fixedly connected with the valve core 62, so that the driving motor 71 can drive the driving wheel one 711 and the valve core 62 to rotate through the driven wheel 721 when working.
Referring to fig. 2 and 3, the switching member 7 further includes a driving member for driving the chassis 65 to rotate synchronously with the valve core 62, where the chassis 65 and the lower valve body 64 rotate synchronously with the valve core 62, and at this time, the first inlet 621, the first pipeline 626, the discharge cavity 641, the liquid outlet 624 and the liquid inlet 41 are still communicated with each other, and the second inlet 622, the second pipeline 627, the third inlet 623, the third pipeline 628, the liquid waste pipeline 629, the liquid waste port 625, the liquid waste cavity 642 and the liquid waste pipe 51 are also communicated with each other due to the same rotation of the chassis 65, the lower valve body 64 and the valve core 62.
Referring to fig. 2 and 3, as the valve core 62 rotates, the first inlet 621 is switched from the first feeding chamber 631 to the second feeding chamber 632, the second inlet 622 is switched from the second feeding chamber 632 to the third feeding chamber 633, the third inlet 623 is switched from the third feeding chamber 633 to the first feeding chamber 631, the second liquid chromatograph 2 (see fig. 1) is connected to the second feeding chamber 632 through the second liquid outlet 21, the third liquid chromatograph 3 (see fig. 1) is connected to the third feeding chamber 633 through the third liquid outlet 31, the first liquid chromatograph 1 (see fig. 1) is connected to the first feeding chamber 631 through the first liquid outlet 11, the second liquid chromatograph 2 is connected to the mass spectrometer 4, the third liquid chromatograph 3 and the first liquid chromatograph 1 are connected to the waste liquid barrel 5, and the samples are separated and analyzed in the same period, and the first state after the first switching is set as the first state.
Referring to fig. 2 and 3, the driving member drives the chassis 65 and the lower valve body 64 to continue to rotate, the communication states of the valve core 62, the lower valve body 64 and the chassis 65 are still unchanged, at this time, the first liquid inlet 621 is switched from the second feeding chamber 632 to the third feeding chamber 633, the second liquid inlet 622 is switched from the third feeding chamber 633 to the first feeding chamber 631, the third liquid inlet 623 is switched from the first feeding chamber 631 to the second feeding chamber 632, at this time, the third liquid chromatograph 3 (refer to fig. 1) introduces a sample into the third feeding chamber 633 through the third liquid outlet pipe 31, the first liquid chromatograph 1 (refer to fig. 1) and the second liquid chromatograph 2 (refer to fig. 1) convey the mobile phase into the waste liquid barrel 5 and perform separation analysis processing on the sample, and the second state after the second switching is set as the second state in the same period.
Referring to fig. 2 and 3, the driving member includes a second driving wheel 731 and a driving ring 732, the second driving wheel 731 is slidably connected with the output shaft of the driving motor 71, the output shaft of the driving motor 71 is fixedly connected with a limiting strip 733, the second driving wheel 731 is provided with a limiting slot 734 adapted to the limiting strip 733, and the limiting slot 734 limits the limiting strip 733, so that when the output shaft of the driving motor 71 rotates, the second driving wheel 731 can be driven to rotate, and the rotation radius of the second driving wheel 731 is the same as that of the first driving wheel 711, and therefore, when the driving motor 71 works, the angular speed and the linear speed of the first driving wheel 711 and the second driving wheel 731 are the same.
Referring to fig. 2 and 3, the driving ring 732 is sleeved on the outer side of the lower valve body 64 and is coaxially arranged with the chassis 65, the driving wheel two 731 is meshed with the driving ring 732, the driving wheel two 731 can drive the driving ring 732 to rotate, the rotation radiuses of the driving ring 732 and the driven wheel 721 are the same, so that the angular speeds and the linear speeds of the driving ring 732 and the driven wheel 721 are the same, the rotation angles of the driving ring 732 and the driven wheel 721 are the same, the driving ring 732 is fixedly connected with a protruding block, the chassis 65 is provided with a groove matched with the protruding block, the protruding block is inserted into the groove, when the driving ring 732 rotates, the protruding block is limited by the groove, the chassis 65 can rotate along with the driving ring 732, the angular speeds of the chassis 65 and the driving ring 732 are the same, namely the rotation angles of the chassis 65, the lower valve body 64 and the valve core 62 are the same, and the three can synchronously rotate.
Referring to fig. 2 and 3, when the switching member 7 is matched with the driving member, and the valve core 62, the lower valve body 64 and the chassis 65 are switched twice, the first liquid chromatograph 1 (refer to fig. 1), the second liquid chromatograph 2 (refer to fig. 1) and the third liquid chromatograph 3 (refer to fig. 1) all complete a process of conveying samples to the mass spectrometer 4 (refer to fig. 1), and at this time, the switching member 7 drives the valve core 62 to continue to rotate, so that the first liquid inlet 621 is switched from the third feeding cavity 633 to the first feeding cavity 631, and the valve core 62 is restored to the initial state and enters the cycle of the next period.
Referring to fig. 2 and 3, the switching member 7 further includes a reset member 74 for resetting the chassis 65, the reset member 74 drives the chassis 65 and the lower valve body 64 to reversely rotate at this time, in the process that the chassis 65 is switched from the initial state to the second state, the chassis 65 is switched twice, and the reset member 74 drives the chassis 65 and the lower valve body 64 to reversely rotate 240 °, so that the chassis 65 and the lower valve body 64 also recover the initial state, and the liquid inlet pipe 41 and the liquid outlet pipe 51 connected with the chassis 65 are reset together with the chassis 65, so that the liquid inlet pipe 41 and the liquid outlet pipe 51 cannot mutually wind due to continuous unidirectional rotation of the chassis 65, and smooth and normal use of the liquid inlet pipe 41 and the liquid outlet pipe 51 is ensured.
Referring to fig. 2 and 3, the reset member 74 includes a limiting block 741, a stop block 743, a torsion spring 742, and a moving member 744 for driving the driving ring 732 and the driving wheels two 731 to move synchronously along the self axis direction, the moving member 744 can drive the driving ring 732 to move along the self axis direction, and the protruding block moves along with the driving ring 732, so that the protruding block can be separated from the groove, and at this time, no connection limit exists between the driving ring 732 and the chassis 65. The torsional spring 742 is fixedly connected between the frame 61 and the chassis 65, when the chassis 65 and the lower valve body 64 rotate together with the valve core 62, the torsional spring 742 is stretched, after the convex block is separated from the groove, the chassis 65 and the lower valve body 64 rotate reversely under the action of the elastic force of the torsional spring 742, the limiting block 741 is fixedly connected with the frame 61, the stop block 743 is fixedly connected with the lower end face of the chassis 65, the stop block 743 rotates together with the chassis 65, when the chassis 65 rotates reversely to an initial state, the stop block 743 is abutted against the limiting block 741, the torsional spring 742 is still in a stretched state, and the limiting block 741 limits the stop block 743, so that the chassis 65 can be accurately reset to the position of the initial state.
Referring to fig. 2 and 3, the moving member 744 includes a moving motor 7441, a threaded rod 7442, a limiting rod 7443 and a moving block 7444, the limiting rod 7443 is fixedly connected with the frame 61, the limiting rod 7443 penetrates through the moving block 7444 and is slidably connected with the moving block 7444, the limiting rod 7443 limits the moving block 7444, the moving block 7444 can move along the length direction of the limiting rod 7443, an output shaft of the moving motor 7441 is fixedly connected with the threaded rod 7442 coaxially, the threaded rod 7442 penetrates through the moving block 7444 and is in threaded connection with the moving block 7444, and when the threaded rod 7442 rotates, the limiting rod 7443 limits the moving block 7444, so that the moving block 7444 can move along the length direction of the threaded rod 7442.
Referring to fig. 2 and 3, the moving block 7444 is provided with a sliding groove 7445 adapted to the driving ring 732, the driving ring 732 is located in the sliding groove 7445 and abuts against the moving block 7444, and when the moving block 7444 moves along the length direction of the threaded rod 7442, the sliding groove 7445 limits the driving ring 732, so that the driving ring 732 moves together with the moving block 7444. The driving ring 732 is fixedly connected with two annular baffles 7446 along the circumferential direction, the driving wheel two 731 is located between the two annular baffles 7446 and is in conflict with the annular baffles 7446, when the driving ring 732 moves, the two annular baffles 7446 drive the driving wheel two 731 to move, so that the driving wheel two 731 moves along the length direction of the output shaft of the driving motor 71, the driving ring 732 and the driving wheel two 731 can synchronously move, and the driving ring 732 and the driving wheel two 731 are ensured to be meshed with each other all the time.
Referring to fig. 2 and 3, when the moving member 744 drives the driving ring 732 and the driving wheel two 731 to move, the driving ring 732 moves in a direction away from the chassis 65, at this time, the protrusion is separated from the groove, the driving ring 732 acts on the chassis 65 infinitely, and after the chassis 65 is reset under the action of the elastic force of the torsion spring 742, at this time, the chassis 65 and the lower valve body 64 are in an initial state.
Referring to fig. 2 and 3, after the driving ring 732 is separated from the chassis 65, the driving motor 71 drives the first driving wheel 711 and the second driving wheel 731 to rotate, so that the rotating rod 72, the valve core 62 and the driving ring 732 synchronously rotate, after the valve core 62 rotates 120 ° again, the valve core 62 is in an initial state, and the driving ring 732 is also in an initial state, at this time, since the driving ring 732 and the chassis 65 are both in the initial state, the protrusions and the grooves correspond to each other, the moving motor 7441 reversely rotates, and drives the moving block 7444 to move in a direction close to the chassis 65, so that the driving ring 732 is close to the chassis 65, the protrusions are inserted into the grooves, at this time, the circulation and switching of a whole period are completed, and the valve core 62, the lower valve body 64, the driving ring 732 and all the communication conditions of the pipelines recover to the initial state, so that the circulation of the next period can be repeated.
Referring to fig. 2 and 3, the frame 61 is provided with a controller 611, the driving motor 71 and the moving motor 7441 are electrically connected to the controller 611, the controller 611 can control the on-off time of the driving motor 71 and the moving motor 7441, and a worker can set time parameters to realize the timing operation of the driving motor 71 and the moving motor 7441 in the above process, so as to complete the whole process of switching the switching mechanism 6 from the initial state to the first state, from the first state to the second state, and from the second state to the initial state.
Referring to fig. 1 and 3, the upper valve body 63 is provided with a cleaning chamber 634, the upper valve body 63 is fixedly connected with a cleaning tube 635 communicated with the cleaning chamber 634, the other end of the cleaning tube 635 is communicated with a cleaning tank 636 filled with cleaning liquid, the cleaning liquid in the cleaning tank 636 can be distilled water or organic solvent, such as propanol, and the like, and staff can select according to the properties of the sample. The cleaning chamber 634 is disposed between the second feeding chamber 632 and the third feeding chamber 633, and the cleaning chamber 634 is symmetrically disposed with the first feeding chamber 631.
Referring to fig. 2 and 3, when the first pipeline 626 is required to be cleaned, the rotatable valve core 62 enables the first inlet 621 to be communicated with the cleaning chamber 634, and at this time, since the cleaning chamber 634 is symmetrically arranged with the first inlet 631, the lower end of the first pipeline 626 is switched from the inlet chamber to the waste liquid chamber 642, and the cleaning liquid flows through the first inlet 621, the first pipeline 626 and the waste liquid chamber 642 and is discharged into the waste liquid barrel 5 (refer to fig. 1) through the waste liquid pipe 51, so that the cleaning process of the cleaning liquid is completed. At this time, the valve core 62 is switched by the driving motor 71, but the moving member 744 drives the driving ring 732 to separate from the chassis 65, the chassis 65 and the lower valve body 64 do not rotate together with the valve core 62, the chassis 65 is in the initial state, and the valve core 62 rotates 180 ° to enable the first liquid inlet 621 to be communicated with the cleaning cavity 634, so as to complete the cleaning process.
Referring to fig. 2 and 3, when the second and third pipelines 627 and 628 are cleaned, the protrusions are inserted into the grooves, so that the bottom plate 65 and the lower valve body 64 rotate together with the valve core 62, the valve core 62 rotates to the second or third inlet 622 or 623 to be communicated with the cleaning chamber 634, and at this time, since the bottom plate 65 and the lower valve body 64 rotate together with the valve core 62, the waste liquid pipeline 629, the waste liquid port 625 and the waste liquid pipe 51 are always communicated, the cleaning liquid flows through the second or third pipeline 627 or 628, then enters the waste liquid pipeline 629, and finally enters the waste liquid barrel 5 (refer to fig. 1) through the waste liquid pipe 51. Because the cleaning chamber 634 is located between the second feeding chamber 632 and the third feeding chamber 633, when any one of the first inlet 621, the second inlet 622 and the third inlet 623 corresponds to and communicates with the cleaning chamber 634, the other two are not communicated with the first feeding chamber 631, the second feeding chamber 632, the third feeding chamber 633 and the cleaning chamber 634, and no liquid is introduced into the switching mechanism 6 except cleaning liquid.
Referring to fig. 3 and 4, the liquid inlet pipe 41 is fixedly connected with a first branch pipe 637, the other end of the first branch pipe 637 is fixedly connected with a blowing device 639, the blowing device 639 can introduce compressed inert gas such as nitrogen, helium and the like into the first branch pipe 637, before the blowing device 639 works, a bump is inserted into a groove, the driving motor 71 works to drive the valve core 62, the bottom plate 65 and the lower valve body 64 to rotate together, so that the liquid inlet pipe 41 is communicated with the cleaning pipe 635 through a first pipeline 626, and compressed gas enters the cleaning pipe 635 through a first pipeline 626 after entering the first branch pipe 637, enters the feeding cavity along the liquid inlet pipe 41, finally flows through the cleaning cavity 634 and enters the cleaning pipe 635. The purge tube 635 is fixedly connected with a second branch 638 through which compressed gas is discharged, and the compressed gas can blow out the liquid remaining in the flow path from the second branch 638, so that the flow path is dried rapidly, and the sample injection path can be used rapidly.
Referring to fig. 1 and 4, the first branch pipe 637 is provided with a first check valve 6371 that cuts off the flow of liquid from the liquid inlet pipe 41 to the air blowing device 639, and the first check valve 6371 makes the liquid flowing through the liquid inlet pipe 41 less likely to enter the air blowing device 639, protecting the air blowing device 639; the cleaning pipe 635 is provided with a second check valve 6351 for blocking the flow of the gas from the cleaning pipe 635 to the cleaning tank 636, and the second check valve 6351 makes the compressed gas in the flowing path not easy to enter the cleaning tank 636, so that the cleaning liquid is not easy to be polluted by the liquid carried by the compressed gas, and the purity of the cleaning liquid is guaranteed.
Referring to fig. 1 and 4, the liquid inlet pipe 41 is provided with a third check valve 411 for blocking the flow of gas from the first branch pipe 637 to the mass spectrometer 4, and the third check valve 411 makes the gas not easy to enter the mass spectrometer 4 from the liquid inlet pipe 41, thereby being beneficial to protecting the mass spectrometer 4; the branch pipe II 638 is connected with a water stop clamp 6381, when the air blowing device 639 is filled with air, the water stop clamp 6381 can be taken down to facilitate air exhaust, and when the air blowing device 639 is not used, the branch pipe II 638 is closed by the water stop clamp 6381, so that cleaning liquid is not easy to flow out of the branch pipe II 638, and waste of the cleaning liquid is reduced.
The implementation principle of the liquid chromatograph-mass spectrometer and the switching device in the embodiment of the application is as follows: the liquid chromatograph I1, the liquid chromatograph II 2 and the liquid chromatograph III 3 carry out separation analysis processing on different samples, and make the appearance time of three stagger each other, the switching mechanism 6 drives case 62 and chassis 65 through switching piece 7 and rotates, make switching mechanism 6 cooperate the transform of above-mentioned three operating condition and switch, when one instrument carries the sample to mass spectrometer 4, the mobile phase that two other instruments were discharged in the analysis process is discharged into waste liquid bucket 5, because the sample introduction time of three staggers each other, make the three can carry the sample after the separation to mass spectrometer 4 in proper order, the actual operating time of mass spectrometer 4 has been increased, the idle state of mass spectrometer 4 has been reduced, and then the waste of resource has been reduced.
The foregoing are all preferred embodiments of the present application, and are not intended to limit the scope of the present application in any way, therefore: all equivalent changes in structure, shape and principle of this application should be covered in the protection scope of this application.

Claims (9)

1. A switching device, characterized in that: comprises a waste liquid barrel (5) and a switching mechanism (6), the waste liquid barrel (5) is fixedly connected with a waste liquid pipe (51), the switching mechanism (6) comprises a frame body (61), a valve core (62), an upper valve body (63), a lower valve body (64), a chassis (65) and a switching piece (7) for driving the valve core (62) and the chassis (65) to rotate, the upper valve body (63) is fixedly connected with the frame body (61), the lower valve body (64) is rotationally connected with the frame body (61), the upper valve body (63) is provided with a plurality of feeding cavities, the feeding cavities are arranged along the circumferential angle of the upper valve body (63), the lower valve body (64) is provided with a discharging cavity (641) and a waste liquid cavity (642), the valve core (62) is provided with a plurality of liquid inlets, a liquid outlet (624) and a waste liquid outlet (625), the liquid inlet is arranged at equal angle and equidistant along the upper end part of the valve core (62), the liquid outlet (624) and the waste liquid outlet (625) are symmetrically arranged at the lower end part of the valve core (62) about the vertical axis, one of the liquid inlet and the liquid outlet (625) is communicated with the liquid outlet (624), the left liquid inlet (629) is communicated with the waste liquid outlet (629) and the waste liquid (629) is fixedly connected with the waste liquid pipe (64), the waste liquid pipe (51) is fixedly connected with the chassis (65).
2. A switching device according to claim 1, characterized in that: the switching piece (7) comprises a driving motor (71), a rotating rod (72), a driving piece for driving the chassis (65) to synchronously rotate along with the valve core (62) and a resetting piece (74) for resetting the chassis (65), the rotating rod (72) is fixedly connected with the valve core (62) coaxially, the rotating rod (72) is fixedly connected with a driven wheel (721) coaxially, an output shaft of the driving motor (71) is fixedly connected with a driving wheel I (711), and the driving wheel I (711) is meshed with the driven wheel (721).
3. A switching device according to claim 2, characterized in that: the driving piece comprises a driving wheel II (731) and a driving ring (732), the driving ring (732) is sleeved on the outer side of the lower valve body (64) and is coaxially arranged with the chassis (65), the rotation radiuses of the driving wheel II (731) and the driving wheel I (711) are the same, the rotation radiuses of the driving ring (732) and the driven wheel (721) are the same, the driving wheel II (731) is in sliding connection with an output shaft of the driving motor (71), the output shaft of the driving motor (71) is fixedly connected with a limiting strip (733), the driving wheel II (731) is provided with a limiting groove (734) matched with the limiting strip (733), the driving wheel II (731) is meshed with the driving ring (732), the driving ring (732) is fixedly connected with a protruding block, and the chassis (65) is provided with a groove matched with the protruding block.
4. A switching device according to claim 3, characterized in that: the reset piece (74) comprises a limiting block (741), a stop block (743), a torsion spring (742) and a moving piece (744) for driving the driving ring (732) and the driving wheel II (731) to synchronously move along the axis direction of the reset piece, the torsion spring (742) is fixedly connected between the frame body (61) and the chassis (65), the limiting block (741) is fixedly connected with the frame body (61), and the stop block (743) is fixedly connected with the lower end face of the chassis (65).
5. A switching device according to claim 4, wherein: the moving part (744) comprises a moving motor (7441), a threaded rod (7442), a limiting rod (7443) and a moving block (7444), an output shaft of the moving motor (7441) is fixedly connected with the threaded rod (7442) in a coaxial mode, the threaded rod (7442) penetrates through the moving block (7444) and is in threaded connection with the moving block (7444), the limiting rod (7443) is fixedly connected with the frame body (61), the limiting rod (7443) penetrates through the moving block (7444) and is in sliding connection with the moving block (7444), a sliding groove (7445) matched with a driving ring (732) is formed in the moving block (7444), the driving ring (732) is located in the sliding groove (7445) and is in interference with the moving block (7444), two annular baffles (7446) are fixedly connected with each other along the circumferential direction, and a driving wheel II (7446) is located between the two annular baffles (7446) and is in interference with the annular baffles (7446).
6. A switching device according to claim 5, wherein: the frame body (61) is provided with a controller (611), and the driving motor (71) and the moving motor (7441) are electrically connected with the controller (611).
7. A switching device according to claim 1, characterized in that: the upper valve body (63) is provided with a cleaning cavity (634), the upper valve body (63) is fixedly connected with a cleaning pipe (635) communicated with the cleaning cavity (634), and the other end of the cleaning pipe (635) is communicated with a cleaning tank (636) filled with cleaning liquid.
8. A switching device according to claim 7, wherein: the liquid inlet pipe (41) is fixedly connected with a first branch pipe (637), the cleaning pipe (635) is fixedly connected with a second branch pipe (638), the other end of the first branch pipe (637) is fixedly connected with a blowing device (639), the first branch pipe (637) is provided with a first check valve (6371) for cutting off the flow of liquid from the liquid inlet pipe (41) to the blowing device (639), the cleaning pipe (635) is provided with a second check valve (6351) for cutting off the flow of gas from the cleaning pipe (635) to the cleaning tank (636), the liquid inlet pipe (41) is provided with a third check valve (411) for cutting off the flow of gas from the first branch pipe (637) to the mass spectrometer (4), and the second branch pipe (638) is connected with a water stop clamp (6381).
9. A liquid chromatograph-mass spectrometer, characterized in that: the liquid chromatograph comprises a switching device, a plurality of liquid chromatographs and a mass spectrometer (4) according to any one of claims 1-8, wherein the liquid chromatographs are fixedly connected with liquid outlet pipes, the mass spectrometer (4) is fixedly connected with liquid inlet pipes (41), the liquid outlet pipes are in one-to-one correspondence with the feeding cavities and are mutually communicated, and the liquid inlet pipes (41) are fixedly connected with a chassis (65) and are symmetrically arranged with a waste liquid pipe (51).
CN202311525896.0A 2023-11-15 Liquid chromatograph-mass spectrometer and switching device Active CN117571897B (en)

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Application Number Priority Date Filing Date Title
CN202311525896.0A CN117571897B (en) 2023-11-15 Liquid chromatograph-mass spectrometer and switching device

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Application Number Priority Date Filing Date Title
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JP2015115555A (en) * 2013-12-13 2015-06-22 東京エレクトロン株式会社 Changeover valve and liquid processing apparatus
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KR20210141308A (en) * 2020-05-14 2021-11-23 주식회사 엘지화학 On-line system for improving detection level of analytes by liquid chromatography and analysis method using the same
CN114127551A (en) * 2018-12-10 2022-03-01 株式会社日立高新技术 Liquid chromatography mass spectrometry device
JP2023117677A (en) * 2022-02-14 2023-08-24 旭有機材株式会社 Waste liquid selector valve

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2003202332A (en) * 2002-01-08 2003-07-18 Shimadzu Corp High-performance liquid chromatograph
JP2002340876A (en) * 2002-04-12 2002-11-27 Jasco Corp Multiple liquid chromatograph
JP2005069817A (en) * 2003-08-22 2005-03-17 Shimadzu Corp Liquid chromatograph mass spectrometer
JP2015115555A (en) * 2013-12-13 2015-06-22 東京エレクトロン株式会社 Changeover valve and liquid processing apparatus
CN111868517A (en) * 2018-01-11 2020-10-30 株式会社日立高新技术 Analytical device with multiple chromatographs
CN112740030A (en) * 2018-09-21 2021-04-30 株式会社日立高新技术 Analysis device with liquid chromatograph and analysis method of liquid chromatograph
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JP2023117677A (en) * 2022-02-14 2023-08-24 旭有機材株式会社 Waste liquid selector valve

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