JP2007327845A - Liquid supplying method and device - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To perform liquid feeding wherein connection/switching is smooth and sure between a feeding stage and a compression stage of a solution by using a structure suited for accurate and sure minute-amount liquid feeding and also suited for large-amount liquid feeding. <P>SOLUTION: A supply flow path for a solution to a plurality of pump units and to an analysis system, and a suction flow path of the solution are connected to a multiway valve. A pressure sensor is previously installed in each of the supply and suction flow paths. The pressure sensors, the pump units, the multiway valve, and a suction valve, are controlled by a control part. While one pump unit is performing liquid feeding, another pump unit performs liquid sucking via the suction valve and suction flow path. After liquid sucking, the suction valve is closed for liquid feeding preparation to build up the pressure of the suction flow path for the pump unit to the pressure of the supply flow path. As liquid feeding by the one pump unit ends, the multiway valve is switched to cause the other pump unit to start liquid feeding. Liquid feeding is subsequently performed by the two pump units alternately in order. <P>COPYRIGHT: (C)2008,JPO&INPIT

Description

  The present invention relates to a liquid supply method and apparatus, and more particularly to a liquid chromatography liquid supply method and apparatus.

In the conventional single syringe liquid feed pump system, it is necessary to alternately repeat suction and discharge. In the inhalation stroke, since the liquid feeding is not performed, it is usual that the liquid feeding amount pulsates. In order to prevent this pulsation, the double syringe system is adopted, and stable liquid feeding without pulsation is performed. However, the installation of the pump flow path switching valve increases the size and complexity of the device, which increases the cost. .
In order to solve this point, in the invention described in Japanese Patent Laid-Open No. 2003-107065, two pumps 1 and 2 are provided, and the pump 1 is connected to the liquid-feed destination flow path using one valve, and the pump 2 Is in the first state where the pump 1 is connected to the supply source flow path and the pump 2 is connected to the liquid supply destination flow path. There has been proposed a device that includes a valve 3 that switches between a third state connected to the valve 1 and that switches the valve 3 in synchronism with the suction and discharge operations of the pumps 1 and 2. (Patent Document 1)

  In this configuration, the entire volume in the pump cylinder is pressurized at a time and flows to the liquid supply destination channel (so-called analysis system). In this configuration, the operation of the pump cylinder is in a start / stop mode, that is, intermittent, and it is inevitable that a so-called transitional action occurs. In liquid chromatography using a capillary column that has been used recently, even if the change in flow rate is negligible in conventional chromatography, the precision used at a minute flow rate is fine. This is a huge disruption for the HPLC system. In the prior art, it is difficult to counteract the technology that requires a fluid flow without a continuous flow rate change using a capillary column.

  In order to avoid volume fluctuations during the so-called transition process as a result of compressing this conventional liquid delivery solution from atmospheric pressure to system pressure, an HPLC pump is used to prevent pressure fluctuations or flow fluctuations for the system system. Japanese Patent No. 3491948 (Patent Document 2) has been proposed as a method of completely isolating the solution compression stage and the solution delivery stage of operation.

  In this invention, the first and second syringe means and the driving means provided respectively are connected to each syringe means so as to operate each independently. The first and second syringe means are connected by a fluid conduit, at least one receiving and delivering fluid to be in fluid communication with the analytical system system. A valve means is provided in the conduit for isolating the first syringe means.

  The first and second syringes are provided with pressure detection means for measuring the internal pressures. Control means for controlling the operation of the first and second syringe means and the valve means are provided, the control means receives the outputs of the first and second pressure detection means, and when the first syringe is isolated, After the first syringe is filled with a pressure equal to the pressure in the second syringe representing the pressure in the receiving system measured by the second pressure detecting means, the valve means is activated to receive the first syringe into the receiving system. A pumping device that communicates and delivers a substantially constant flow rate to the receiving system.

According to the invention, the pumped solution compression stage and the pumped solution delivery stage are completely isolated, so that the solution is compressed from atmospheric pressure to the system pressure (system pressure), resulting in a receiving system, chromatogram. There are no pressure or flow fluctuations in the graphic system.
Further, it is said that it has an effect of avoiding volume fluctuations during the transition process from the offline state to the chromatography system to the solution feeding stage in the online state.
However, in the present invention, the first syringe has the first pressure measuring means, the second syringe has the second pressure measuring means, and each unit has a pressure sensor and a valve means. As a result, the control is complicated, the equipment is enlarged, and the manufacturing cost is increased.

  Further, the most serious problem is the accuracy when two pressure measuring means, that is, two pressure sensors are used. This is because there are individual differences in the pressure sensor, and thus output levels differ even under the same pressure condition. The range of pressure sensors used in high performance liquid chromatography is often 0 to 500 MPa, and there is also a range of 0 to 100 MPa. Pressure sensor calibration can reduce individual differences in pressure sensors to some extent, but individual differences cannot be eliminated over a wide range. Therefore, as in the invention shown in Patent Document 2, when each pressure unit is provided with a pressure sensor and the compression process is controlled based on the pressure value output to the pressure sensor, Based on the sensor, the difference between the internal pressure of each pump unit and the system pressure may be different, and continuous liquid feeding becomes impossible at a stable pressure.

  In Patent Document 2, the control device 49 compares the outputs from the pressure sensor 23a of the main cylinder 3a and the pressure sensor 23b of the accumulator and can perform mutual calibration of both pressure sensors (0043). However, this fluid communication occurs when either one of the main cylinders is ready for feeding “0”, that is, when the piston speed is 0, and the other piston speed is “positive”, It is a measurement at, and accurate values cannot be obtained, and accurate calibration cannot be performed.

Similarly to Patent Document 2, two syringes and two valves are used, and two transducers are simultaneously fed to the chromatography system together with the two syringes. A system that can be calibrated has been proposed (Patent Document 3).
However, in this system, the transducers 23 and 24 as sensors both detect the pressures of the syringe 12 and the syringe 14 and are affected by individual differences between the sensors as in the invention of Patent Document 2. It is inevitable that it will end. In addition, the valves are the rotary valves 16 and 18 in the figure, but the switching valve 20 and the ON / OFF valve 21 are also required for implementation, and four valves are required for continuous liquid feeding, and the structure is complicated. It becomes.
Furthermore, although there is a place where the calibration of the sensor is mentioned, the piping path for the liquid pre-pressurization passes from the pump through the valve 18 to the system 26 or the port 42 of the valve 16 which is not connected. On the other hand, in the case of calibration (FIG. 4), after passing through both the valve 18 and the valve 16, they merge and go to the system 26, so the piping path is different, and a difference is caused by the pressure loss of the piping. There is a problem that cannot be done.

  In liquid chromatography, a gradient method is used in which sample components are separated and eluted while changing the composition of the mobile phase in order to shorten the analysis time, improve separation, and improve peak shape. In this gradient method, there is a low-pressure mixing method (low-pressure gradient), which uses a solenoid valve or the like to change the mixing ratio of the solution while mixing the solvent on the inlet side of the pump and sending it to the chromatography system. It is a method to liquefy.

  Strictly speaking, the low-pressure gradient method using a technique such as an open / close solenoid valve is a step gradient as a mechanical operation. A step gradient is a method in which the composition of a solution to be fed at a specific time is continuously changed step by step. However, since the composition changes step by step, the change in composition can be reduced. Since it is difficult, it was difficult to obtain a linear gradient like a linear gradient.

JP 2003-107065 A Japanese Patent No. 3491948

Chromatographic separation, especially nano- and micro-flows such as those using capillary columns can be performed accurately and reliably, and the means of construction is simple and the cost is low. It is required to adjust the pressure between the liquid feeding mechanisms when using two liquid feeding mechanisms, and to achieve this with a simpler mechanism. It has been.
In addition, it has been pointed out that in a minute flow rate liquid feeding mechanism, a small amount of liquid feeding is emphasized in order to focus on precision, and the configuration is not suitable for a large amount of liquid feeding.
In addition, when introducing a sample, it is required that stable introduction can be achieved while avoiding the influence of diffusion of the sample band.

  The object of the present invention is to provide an accurate and smooth liquid feeding using a plurality of liquid feeding means, while taking a configuration that separates the pump-acting solution compression stage and the pump-acting solution feeding stage, Instead of providing pressure measuring means for each pump as the liquid feeding means, the pumping operation feeding stage and the pumping solution compression stage are separated. For this purpose, one pressure measurement is performed at the feeding stage and one at the compression stage to prevent an error due to a plurality of pressure measurements at the compression stage, the feeding stage and the compression stage are separated, and the feeding stage is separated. The purpose is to ensure a smooth and reliable connection between the feeding stage and the compression stage. For this reason, each liquid feeding means is connected via a valve means to measure the pressure in the compression stage by one pressure measurement, and in the liquid feeding stage, the pressure of the chromatography system to be fed The object is to control the pressure in the compression stage and to supply liquid.

The present invention can obtain the internal pressure value of each pump chamber from the same pressure sensor when compressing the solution in the pump in two or more pump units, and therefore based on the same pressure sensor. Since the controller controls the internal pressure of each pump unit, there is no difference between the internal pressure at the start of discharge and the system pressure, and the object is to enable continuous liquid feeding at a stable pressure.
Further, the present invention provides a system pressure sensor for monitoring the chromatography system pressure and an internal pressure sensor for observing the internal pressures of a plurality of units. The object is to obtain a device that can be calibrated so as to be compatible with the separation and analysis conditions of the chromatography system used.

  In order to solve the above-mentioned problems and achieve the object, the present invention firstly connects a plurality of pump units each having a drive unit to a multi-way valve, and the multi-way valve is connected to a solution suction channel and an analysis system. Connect the solution supply channel, suck the solution in order by each pump unit, supply the solution to the analysis system connected via the multi-way valve, and the pressure provided in the solution supply channel connected to the multi-way valve The sensor and the pressure sensor provided in the suction flow path communicating with either one of the pump units waiting for liquid feeding are sent to the control unit, and the pressure of the supply flow path and the liquid feeding pump unit is adjusted. Proposed is a liquid supply method characterized in that the liquid is fed in a balanced manner.

  Secondly, a liquid supply method is proposed in which the solution is successively sucked by each pump unit and the solution is continuously supplied to an analysis system connected to a multi-way valve.

  Thirdly, a liquid supply method is proposed in which the communication switching of the pump unit for feeding liquid via the multi-way valve and the pump unit waiting for liquid feeding to the supply flow path is controlled by the multi-way valve.

  Fourth, when one pump unit stops liquid feeding, the pressure filled in the suction flow path communicating with the other pump units while liquid feeding is stopped and the pressure in the supply flow path to be communicated are equal pressures. Then, a liquid supply method is proposed in which the multi-way valve is switched and the other pump unit communicates with the analysis system.

  Fifth, one pump unit is connected via a multi-way valve, while the liquid is being fed through the supply channel, the suction flow path is closed, and the other pump unit is connected to the supply flow connected via the multi-way valve. A liquid supply method is proposed in which the passage is closed and communicated with the solution storage tank via the suction valve, and the state of sucking the solution is switched by the suction valve.

  Sixth, the state where one pump unit 1 or 2 is closed via a multi-way valve and the suction flow path is closed during liquid feeding, and the other pump unit 2 or 1 is a supply flow path via a multi-way valve. The pump unit 2 or 1 for sucking the solution is connected to the solution storage tank via the suction valve, and the state in which the solution is sucked into the pump unit 2 or 1 is switched by the suction valve. A liquid supply method is proposed in which the liquid supply is started and liquid supply is started simultaneously with the switching of the multi-way valve.

  Seventh, a plurality of pump units each having a drive unit are connected via a multi-way valve, and a solution suction channel and a solution supply channel to the analysis system are connected to the multi-way valve, and each pump The unit alternately aspirates the solution and supplies the solution to the analysis system connected via the multi-way valve, and a pressure sensor is provided in the solution supply channel to the analysis system, and one of the plurality of pump units. Proposed is a liquid supply device characterized in that a pressure sensor for sensing the pressure of a suction flow path communicating with the suction flow path is provided in the suction flow path.

  Eighth, the multi-way valve feeds the solution from one pump unit to the supply flow path, and the suction flow path from the suction of the solution in the other pump unit to the multi-way valve of the analysis system. A state in which the pressure continues to be compressed, and a solution is supplied from the pump unit communicating with the other compressed suction passage to the supply passage, and the solution is sucked from the end of one supply, and the suction passage is connected to the system. Proposed is a liquid supply apparatus provided with a multi-way valve for switching between a state where compression continues to a pressure.

  Ninth, a liquid supply apparatus is proposed in which a sample introduction unit connected to the multi-way valve is provided in the supply flow path between the pressure sensor provided in the supply flow path of the analysis system and the multi-way valve.

  Tenth, a three-way joint is installed between the pressure sensor provided in the supply flow path to the analysis system and the multi-way valve, and a flow path V is provided between the three-way joint and the suction valve provided in the suction flow path. A liquid supply apparatus is proposed in which a pressure calibration apparatus is configured by providing a pressure sensor.

  Eleventhly, the suction flow path, the supply flow path, and the pump units 1 and 2 are connected to the multi-way valve, and the suction flow path, the solution storage tank, and the discharge flow path are connected to the suction valve. A liquid supply device is proposed, which is provided with a suction valve for selectively switching the communication state between the solution storage tank and the discharge channel for the pump unit 1 or 2 connected to the multi-way valve.

  Twelfthly, two pump units can be connected to the multi-way valve, and the multi-way valve has a supply flow path to the analysis system having the first pressure sensor and a solution storage tank having the second pressure sensor. When one pump unit is connected to the supply flow path via the multi-way valve, the other pump unit is connected to the suction flow path via the suction valve, and by switching the multi-way valve, Proposed is a solution supply device comprising a multi-way valve that alternately connects a supply channel and a suction channel.

  According to the present invention, when compressing the solution in the pump, the internal pressure value of each pump chamber can be obtained from the same pressure sensor, and therefore the internal pressure of each pump unit is determined based on the same pressure sensor. Since it is controlled, the difference between the internal pressure at the start of discharge and the system pressure disappears, and continuous liquid feeding can be performed at a stable pressure. Further, according to the present invention, the system pressure sensor for monitoring the chromatography system pressure and the internal pressure sensor for observing the internal pressures of the plurality of pump units form a flow path that has almost no pressure loss at a predetermined flow rate. Thus, it is possible to obtain an apparatus for calibrating so as to be compatible with the separation / analysis conditions of the chromatography system actually used.

As a result, it has become possible to easily and easily carry out nano- and micro-minute flow rates as in liquid chromatography using a capillary column.
Moreover, as a liquid feeding mechanism, the two pump units are connected via a multi-way valve so as to prevent the adverse effect of separately providing pressure measuring means between the two pump units, and a common supply flow path With this setting, the pressure difference between the pump units is eliminated, and extremely uniform liquid feeding is ensured.

  In addition, by installing a pressure calibration path to correct the pressure difference between the two pump units, it is possible to compare and calibrate the pressure in the same state as in normal use, and to supply liquid with extremely accurate equal pressure. Was to be secured.

  In addition, according to the present invention, by providing the sample introduction unit connected to the valve, it is possible to accurately introduce the sample without adversely affecting the diffusion of the sample band.

In this specification, an analysis system is a measurement, detection, and analysis instrument based on various measurement methods, and is a generalization of the system, but it also includes individual detection, analysis instruments, and accessory equipment such as a sample introduction unit. Shall be included.
The pump unit is composed of one cylinder and a corresponding plunger and an actuator for driving the plunger. As the actuator, a step motor or other conventionally known one is used. Regarding the driving of the cylinder, it is convenient to use a plunger push-out type by rotating the screw by a motor.
System pressure refers to the pressure in the analysis system and / or its flow path.

Hereinafter, the present invention will be described in detail with reference to the embodiment shown in FIG.
An embodiment of the present invention includes a liquid delivery device comprising: pump units 1 and 2, a system pressure sensor 3 for monitoring the pressure of the chromatography system X1 as an analysis system, and an internal pressure sensor for measuring a pressure such as a local pressure of the pump units 1 and 2. 4. Multi-way valve 5 as switching valve, suction valve 6 as switching valve, operation control of solution storage tank 7 for storing solution 71 and pump units 1 and 2, and multi-way valve 5 and suction valve 6 (here, 8 directions respectively) And a control unit 8 that performs switching control of a valve and a four-way valve.

  The pressure sensors 3 and 4 are a detection unit made of a semiconductor element or a piezo element (piezoelectric element) for converting pressure into an electrical signal, a case for casing the detection unit, and a built-in circuit for outputting and amplifying the detected signal. It is composed of The pressure sensor has a flow path through which a fluid flows, an inlet and an outlet, and a pipe connection portion. The pressure sensor may be connected as a part of a pipe used for a flow path to measure pressure, and measures the pressure applied to the pipe and outputs it as an electrical signal.

  The control unit 8 stores the pressure information from the pressure sensor (signal from the sensor), the position information of the plunger (signal from the drive unit), and the input information (signal from the interface) such as the flow rate specified by the user. A computer that combines the whole of the mechanisms that perform calculations inside and output signals for operating the linear actuators 9 and 10 and the switching valves 5 and 6 that drive the plunger is called a control unit 8.

  The pump units 1 and 2 are constituted by plungers 13 and 14 having reciprocating motions in the pump chambers 11 and 12 and having pump seals 15 and 16 and linear actuators 9 and 10 for driving the plungers 13 and 14, respectively. The In these pump units 1 and 2, the linear actuators 9 and 10 for driving the plungers 13 and 14 use a step motor, a micro step motor, etc., and a linear feed conversion mechanism using a reduction gear module, a bearing, a nut, etc. This is performed using various known mechanisms.

The pump units 1 and 2 are connected to ports C and G, respectively, of the switching valve 5. The switching valve 5 uses an 8-way valve which is a multi-way valve here. A supply flow path X to a chromatography system X 1 as a receiving device is connected to a port A of the switching valve 5 via a system pressure sensor 3.
The switching valve 5 has a port E connected to the port a and a suction passage Y connected to the switching valve 6 via the internal pressure sensor 4. The switching valve 6 is connected to a port e of a discharge flow path Z, for example, a drain tube, and a port c communicating with the port a is connected to a solution storage tank 7 to open and close the suction flow path Y. Do it.

The system pressure sensor 3 senses the pressure of the supply flow path X connected to the switching valve 5, that is, the pressure of an analysis system such as chromatography. The internal pressure sensor 4 is installed in the suction flow path Y, is connected to the pump unit 1 and the pump unit 2 via the switching valve 5, and observes the pressures of the pump unit 1, the pump unit 2, and the suction flow path Y, It is connected to the control unit 8.
The control unit 8 controls the switching valve 6 for communication and isolation between the suction flow path Y and the solution storage tank 7 and communication between the suction flow path Y and the discharge flow path Z.

  The control unit 8 for controlling the operation of the pump units 1 and 2 obtains the stroke lengths of the plungers 13 and 14 that reciprocate the pump chambers 11 and 12 based on the observation values of the system pressure sensor 3 and the internal pressure sensor. Thus, the driving of the linear actuators 9 and 10 for driving them is controlled. The ports B and D and the ports F and H of the switching valve 5 are connected by tubes 51 and 52, respectively. The 8-way switching valve of the switching valve 5 can also use a 4-way switching valve 50 (see FIG. 2). The ports b and d of the switching valve 6 are conveniently closed with plugs.

行程１〜６を繰り返し連続で行なう事により、単一溶媒を連続的に送液する事が可能である。尚、状態０−１及び０−２は初期化行程であるため、送液開始時に一度だけ実行される。 Hereinafter, the pump operation of the embodiment of the present invention device is shown in a table.
The valve position of the multi-way valve 5 is abbreviated as shown below.
Valve position “1”: Ports A, B, C, D, E, F, G, H are in communication state Valve position “2”: Ports B, C, D, E, F, G, H, A are in communication state

By performing steps 1 to 6 repeatedly and continuously, a single solvent can be continuously fed. Since states 0-1 and 0-2 are initialization steps, they are executed only once at the start of liquid feeding.

Next, the operation and control of the above apparatus will be described.
(1) First, initialization is performed. The multi-way valve 5 is switched to a state in which the ports F and G, A and H, B and C, and D and E communicate with each other under the control of the control unit 8. After the multi-way valve 5 is switched, the control unit 8 immediately switches the switching valve 6 to the state in which the ports a and c are communicated with each other, and the pump unit 1 is moved by the retraction of the plunger 13 by the operation of the actuator 9. The solution 71 is aspirated from the storage tank 7. After the pump unit 1 finishes the suction, the plunger 13 stops and at the same time, the multi-way valve 5 is switched, between the ports G and H, between the ports E and F, between the ports A and B, and between the ports C and D. Communicated. The suction valve 6 is not switched, and the pump unit 2 sucks the solution 71 from the solution storage tank 7 by the retraction of the plunger 14 while the ports a and c are in communication. After the pump unit 2 finishes the suction, the plunger 14 stops.

(2) In a state where the ports C and D and A and B of the multi-way valve 5 are in communication with each other, the actuator 9 is operated by the control unit 8, and the plunger 13 of the pump unit 1 is moved forward to move inside the pump chamber 11. The solution 71 is continuously delivered to the supply channel X to the chromatography system. (Liquid feeding stage)
(3) At the same time, the suction valve 6 is closed from the state where the ports a and c are communicated with each other, and is switched to the state where the port a and the (seally closed) d are communicated. As the pump unit 1 feeds the liquid, it is sent to the supply channel X and the system pressure continues to rise, and the measured value of the system pressure sensor 3 is transmitted to the control unit 8. On the other hand, the pump unit 2 continues to compress the solution in the pump chamber 12 by the advance of the plunger 14. The pressure in the pump chamber 12 is sensed by the sensor 4, and after the pressure reaches the system pressure sensed by the pressure sensor 3, the control unit 8 stops the plunger 14 via the actuator 10 and makes it stand by. (Compression stage)

(4) At the moment when the plunger 13 of the pump unit 1 reaches top dead center and stops, the multi-way valve 5 is connected between ports C and D, between A and B, between G and H, and between E and F. The state is switched from F to G, between A and H, between B and C, and between D and E.
(5) At the same time when the multi-way valve 5 is switched, the pump unit 2 immediately delivers the solution in the pump chamber 12 to the chromatography system X1 by the advance of the plunger 14. (Liquid feeding stage)

(6) After the multi-way valve 5 is switched, the switching valve 6 is immediately switched from the state in which the ports a and d are communicated to the state in which the ports a and c are in communication. The solution 71 is aspirated from the solution storage tank 7 by the retreat of.
(7) After the suction of the pump unit 1 is completed, the suction valve 6 is switched, the port a and the (tightly plugged) d are communicated, and the pump unit 1 is moved into the pump chamber 11 by the advance of the plunger 13. Continue to compress solution 71 and after reaching system pressure, stop plunger 13 and wait. (Compression stage)

(8) At the moment when the plunger 14 of the pump unit 2 reaches top dead center and stops, the multi-way valve 5 communicates between ports F and G, between A and H, between B and C, and between D and E. Is switched to a state in which the ports C and D, A and B, G and H, and E and F are in communication.
(9) At the same time as the multi-way valve 5 is switched, the pump unit 1 immediately sends out the solution 71 in the pump chamber 11 to the chromatography system X1 by the advance of the plunger 13. (Liquid feeding stage)

(10) After the multi-way valve 5 is switched, the suction valve 6 is immediately switched from the state where the ports a and d are communicated to the state where the ports a and c are communicated, and the pump unit 2 is moved to the plunger. The solution 71 is sucked from the solution storage tank 7 by the retreat of 14.
(11) After suction by the pump unit 2, the suction valve 6 is switched, the port a and the (tightly plugged) d are communicated, and the pump unit 2 is moved into the pump chamber 12 by the advance of the plunger 14. The solvent is kept compressed, and when the pressure of the internal sensor 4 reaches the system pressure, the plunger 14 is stopped and waited. (Compression stage)

(12) The pump unit 1 and the pump unit 2 are controlled by the control unit 8 as logically assembled as described above, and the system pressure is stabilized by repeating the operations (4) to (11). Stable continuous liquid feeding was made possible while maintaining the state.

(13) Further, after the pump unit 1 or the pump unit 2 is sucked, the suction valve 6 is switched from the state where the ports a and c are communicated to the state where the ports a and e are communicated, and the pump unit 1 or The pump unit 2 sends the solution in the pump chamber 11 or 12 to the discharge channel Z (drain line) by the advance of the plunger. After bubbles are sucked in the case where bubbles are present in the pump chamber 11 or 12 of the pump unit 1 or the pump unit 2 or when the previously used solution remains in the pump chamber 11 or 12 and the suction flow path Y, By immediately repeating (purging) the flow to the discharge flow path Z (drain line), bubbles existing in the pump chamber 11 or 12 can be quickly removed, and the solution used last time can be replaced quickly. . After the purge is completed, the solution sucked by the pump unit 1 or the pump unit 2 is compressed, and when the system pressure is reached, the plunger is stopped and waits.

  Since FIG. 2 is different only by using a four-way valve 50 instead of the eight-way valve 5, details thereof will be omitted.

  In the embodiment shown in FIGS. 3 and 4, the sample introduction unit 17 is installed in the supply channel X from the system pressure sensor 3 and the multi-way valve 5 or 50. As the sample introduction unit 17, a manual injector connected to a valve or an autosampler capable of automatically injecting a sample into the chromatography X1 is suitable. The sample loaded into the sample introduction unit 17 is introduced into the chromatography X1 by the solution (mobile phase) sent from the pump unit 1 or 2 by the sample introduction unit 17. This mechanism allows sample introduction without adversely affecting the diffusion of the sample band.

  Next, mutual calibration and control of the pressure sensor will be described. The basic mechanism is the same as the apparatus shown in FIGS. 1 and 2, but a three-way joint 19 is connected between the multi-way valve 5 and the system pressure sensor 3, and between the three-way joint 19 and the port b of the intake valve 6. The detour channel V is installed. (FIGS. 5 and 6) The calibration principle of the pressure sensor is as follows: “By connecting the sensors 3 and 4 through the calibration channel, the actual pressure becomes the same, and the sensor output at that time is defined as the same pressure. The sensors 3 and 4 are calibrated. "

  Since the pressure loss in the piping prevents the same pressure from being applied to the sensors 3 and 4 and the sensor is displaced, the necessary conditions for the three-way joint 19 and the bypass channel V are as follows. There is a need to have a joint with a form that there is almost no. Basically, a commonly used T-shaped or Y-shaped three-way joint can be used for the three-way joint 19. The mutual calibration of the pressure sensor 3 and the pressure sensor 4 is performed by performing display calibration for eliminating the display difference when the internal pressure sensor 4 and the system pressure sensor 3 communicate with each other. For example, it can be automatically performed by a program based on the following procedure.

1) The multi-way valve 5 is switched to a state in which the ports F and G, A and H, B and C, and D and E communicate with each other. After the multi-way valve 5 is switched, the suction valve 6 is also immediately switched to the state where the ports a and c are communicated, and the pump unit 1 sucks the solution 71 from the solution storage tank 7 by the retraction of the plunger 13.

2) After the pump unit 1 finishes the suction, the plunger 13 stops, and at the same time, the multi-way valve 5 is switched, and the ports G and H and the ports E and F communicate with each other. The suction valve 6 is not switched, and the pump unit 2 sucks the solution 71 from the solution storage tank 7 by the retraction of the plunger 14 while the ports a and c are in communication. After the pump unit 2 finishes the suction, the plunger 14 stops.

3) The suction valve 6 is switched from a state where the ports a and c are communicated to a state where a and b are communicated.

4) Either or both of pump unit 1 and pump unit 2 continuously deliver solutions of either or both of pump chamber 11 and pump chamber 1 to the chromatography system.

5) Since the system pressure sensor 3 and the internal pressure sensor 4 communicate with each other, both sensors sense the same system pressure. After the system pressure is stabilized, the output measurement values of the system pressure sensor 3 and the internal pressure sensor 4 are compared with the control unit 8 at 8 and the display is calibrated to the same output.

FIG. 1 is a schematic block diagram of an embodiment of the present invention. General description block diagram of other embodiments of the present invention General description block diagram of other embodiments of the present invention General description block diagram of other embodiments of the present invention General description block diagram of other embodiments of the present invention General description block diagram of other embodiments of the present invention

Explanation of symbols

DESCRIPTION OF SYMBOLS 1 Pump unit 2 Pump unit 3 System pressure sensor 4 Internal pressure sensor 5 Multi-way valve 6 Suction valve 7 Solution storage tank 8 Control part 9 Linear actuator 10 Linear actuator 11 Pump chamber 12 Pump chamber 13 Plunger 14 Plunger 15 Pump seal 16 Pump Seal 17 Sample introduction unit 19 Three-way joint 50 Switching valve 51 Tube 52 Tube 71 Solution A port B port C port D port E port F port G port H port X supply flow channel X1 chromatography system Y suction flow channel Z discharge flow channel V Detour channel a port b port c port d port e port

Claims (12)

  A plurality of pump units each having a drive unit are connected to a multi-way valve, and the multi-way valve is connected to a solution suction channel and a solution supply channel to the analysis system, and each pump unit sucks the solution in order. In addition to supplying the solution to the analysis system connected via the multi-way valve, the pressure sensor provided in the solution supply flow path connected to the multi-way valve is provided in the suction flow path that communicates with the one pump unit waiting for liquid delivery. A liquid supply method comprising: supplying each pressure sensed by the pressure sensor to the control unit and balancing the pressures of the supply flow path and the liquid feed pump unit.   2. The liquid supply method according to claim 1, wherein the solution is successively sucked by each pump unit and continuously supplied to an analysis system connected to a multi-way valve.   3. The liquid supply method according to claim 1, wherein communication switching to the supply flow path of the pump unit that sends liquid through the multi-way valve and the pump unit that waits for liquid supply is controlled by the multi-way valve.   After one pump unit stops liquid supply, the pressure filled in the suction flow path communicating with the other pump units in the liquid supply stop and the pressure in the supply flow path to be communicated become equal, 4. The liquid supply method according to claim 1, wherein the valve is switched to allow the other pump unit and the analysis system to communicate with each other.   While one pump unit is feeding through the supply flow path via the multi-way valve, the suction flow path is closed, and the other pump unit closes the supply flow path connected via the multi-way valve, 5. The liquid supply method according to claim 1, wherein a state in which the solution is sucked in communication with the solution storage tank is alternately switched by a suction valve.   One pump unit 1 or 2 is closed via the multi-way valve and the suction flow path is closed during liquid feeding, and the other pump unit 2 or 1 is closed with the supply flow path via the multi-way valve and the suction valve is closed. When the pump unit 2 or 1 that communicates with the solution storage tank is switched to the state where the pump unit 2 or 1 sucks the solution with the suction valve, the pump unit 2 or 1 that sucks the solution reaches the system pressure and waits. 6. The liquid supply method according to claim 1, wherein liquid feeding is started simultaneously with switching of the multi-way valve.   A plurality of pump units each having a drive unit are connected via a multi-way valve, and a solution suction channel and a solution supply channel to the analysis system are connected to the multi-way valve. A suction flow path that supplies a solution to an analysis system connected through a multi-way valve, has a pressure sensor in the solution flow path to the analysis system, and communicates with one of a plurality of pump units A liquid supply device, characterized in that a pressure sensor for detecting the pressure is provided in the suction flow path.   The multi-way valve feeds the solution from one pump unit to the supply flow path, and continues to compress the suction path from the solution sucked to the multi-way valve to the pressure of the analysis system in the other pump unit. A state in which the solution is fed from the pump unit communicating with the other compressed suction channel to the supply channel, the solution is sucked from the end of one supply, and the suction channel is continuously compressed to the system pressure; 8. A liquid supply apparatus according to claim 7, further comprising a multi-way valve for switching between the two.   9. The liquid supply apparatus according to claim 7, wherein a sample introduction unit connected to the multi-way valve is provided in a supply flow path between the pressure sensor provided in the supply flow path of the analysis system and the multi-way valve.   A pressure calibration device by installing a three-way joint between a pressure sensor provided in a supply flow path to the analysis system and a multi-way valve, and providing a flow path V between the three-way joint and a suction valve provided in the suction flow path. The liquid supply device according to claim 7, wherein the liquid supply device is configured.   A pump unit in which the suction flow path, the supply flow path, and the pump units 1 and 2 are connected to the multi-way valve, and the suction flow path, the solution storage tank, and the discharge flow path are connected to the suction valve and connected to the multi-way valve through the suction flow path. 11. The liquid supply apparatus according to claim 7, further comprising a suction valve that selectively switches a communication state between one of the solution storage tank and the discharge channel with respect to 1 or 2.   Two pump units can be connected to a multi-way valve, and the multi-way valve is connected to a supply flow path to an analysis system having a first pressure sensor and a suction flow path to a solution storage tank having a second pressure sensor. At the same time, when one pump unit is connected to the supply flow path via the multi-way valve, the other pump unit is connected to the suction flow path via the suction valve, and the supply flow path and the suction flow path are switched by switching the multi-way valve. A solution supply apparatus comprising a multi-way valve for alternately connecting the two.

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