Liquid chromatograph and method of controlling liquid chromatograph

Abstract

A liquid chromatograph capable of inhibiting mixing of bubbles into a flow path is provided with a mobile phase to a reservoir bottle without stopping analysis and liquid feeding. A liquid chromatograph (100) includes a liquid feeding device (104) that feeds a mobile phase, a sample injection section (105) that injects a sample into the mobile phase fed from the liquid feeding device (104), a column (106) that separates the sample carried by the mobile phase fed from the sample injection section (105), and a detection device (108) that detects the sample separated by the separation column (106). Further, the liquid chromatograph (100) includes a reservoir bottle (102) that stores the mobile phase carried by the liquid feeding device (104), a mobile phase supply bottle (101) that supplies the mobile phase to the reservoir bottle (102), a mobile phase supply pump (103) that supplies the mobile phase stored in the mobile phase supply bottle (101) to the reservoir bottle (102), and a control section (111) that controls the operation of the mobile phase supply pump (103) and determines the amount of the mobile phase supplied from the mobile phase supply bottle (101) to the reservoir bottle (102).

Description

Technical Field

[0001] This invention relates to a liquid chromatograph and a control method for the liquid chromatograph. Background Technology

[0002] Liquid chromatography (LC) is an analytical method in which a liquid sample, the object of analysis, is introduced into a column through which a liquid mobile phase separates the sample into its constituent components. The separated components are then detected by a detector connected to the downstream side of the column. To detect the components of the liquid sample separated by the column, detection units such as UV / Vis spectrophotometers, fluorometers, and mass spectrometers are connected to the downstream side of the column.

[0003] A major portion of the separation performance of LC depends on the type of packing material used in the column. As an example, in recent years, throughput has been increased by using ultra-high performance liquid chromatography (UHPLC) with high separation and high sensitivity analysis by packing columns with small packing materials less than 2 μm in diameter.

[0004] In LC, the mobile phase delivered from the liquid delivery device not only has the function of transporting the sample to be measured, but also has the function of separating the sample into its components by the difference in affinity with the stationary phase packed in the column. LC uses various types of mobile phases such as ultrapure water, organic solvents, and buffer solvents. The operator selects the mobile phase used in the LC system according to the purpose of the measurement and the type of liquid sample.

[0005] Therefore, the mobile phase used in LC has the function of transporting the sample while also affecting the measurement results. For example, the measurement results can sometimes change significantly due to air bubbles in the mobile phase entering the delivery device or the downstream flow path. Therefore, LC operators monitor the mobile phase level to prevent air bubbles from entering the LC's analytical flow path, and when the level falls below a certain threshold, the mobile phase is replaced or supplied to continue the analysis.

[0006] In chromatographic analysis (LC), the mobile phase is continuously supplied to the column and detector throughout the analysis. Therefore, if the remaining mobile phase decreases, the operator must stop the LC cycle and change the mobile phase. Thus, the experiment must be conducted while simultaneously checking the volume of mobile phase consumed and the set solvent level. To prevent air intake due to insufficient solvent in the solvent supply bottle, LC systems sometimes employ level sensors or weight sensors to detect the remaining solvent level, and incorporate features to prevent air bubbles from entering the apparatus.

[0007] As a method for monitoring or managing the mobile phase used in LC, Patent Document 1 discloses a method for calculating the consumed volume and remaining amount of the mobile phase based on discharge flow rate, time, and mixing conditions of the mobile phase in the liquid delivery device of LC.

[0008] In addition, Patent Document 2 shows a system that monitors the margin by installing a sensor for monitoring the margin in the setting part of the mobile phase used in LC, and notifies the operator when the margin is below a certain value.

[0009] In addition, Patent Document 3 shows a system that monitors the consumption and balance of each solvent type based on sensor output values ​​set in multiple LCs connected on a network to monitor mobile phase conditions and mobile phase balance.

[0010] By integrating such a monitoring system into the LC, operators can identify a decrease in the mobile phase balance before impact analysis, and can perform mobile phase replacement or supply operations.

[0011] Here, we provide a brief explanation of the solvent replacement process for the mobile phase in an LC system. Generally, the mobile phase is placed in the LC system in a glass or resin vial. If the amount of mobile phase in the vial decreases, the LC analysis is stopped, the liquid delivery system is shut down, and a new vial filled with mobile phase is replaced.

[0012] As mentioned above, if air bubbles are introduced into the delivery system, the mobile phase cannot be delivered stably, which can sometimes affect analytical results. Therefore, LC operators must exercise meticulous care when changing mobile phase vials and adding more mobile phase to them to prevent air bubbles from entering the supply line. However, it is difficult to completely eliminate the possibility of air bubble introduction. This is not only due to operator errors such as missing air bubbles, but also to the operator's experience, the setup environment of the apparatus, and the type of solvent used.

[0013] Therefore, in most cases, as a preparation for operation, regardless of whether air bubbles are mixed in, after the mobile phase bottle is replaced and the mobile phase is added to the bottle, a bubble removal process to remove air bubbles from the piping is performed as a general step.

[0014] Existing technical documents

[0015] Patent documents

[0016] Patent Document 1: Japanese Patent Application Publication No. 2000-298122

[0017] Patent Document 2: Japanese Patent No. 4778748

[0018] Patent Document 3: WO2020 / 183771A1 Summary of the Invention

[0019] The technical problem that the invention aims to solve

[0020] In recent years, automation has been advanced in many functional aspects of LC, such as the technologies described in Patent Documents 1-3, which also provide automatic monitoring of the mobile phase balance and notification systems to operators.

[0021] However, when actually changing the mobile phase bottle or adding mobile phase to the bottle, the LC analysis and liquid delivery device needs to be stopped once. The change operation and the preparation for operation after the change must be carried out by the operator.

[0022] Since the operation depends on the operator, the operator is limited to a certain amount of time after being notified that the mobile phase balance has decreased, due to the preparation operations that include changing bottles and supplying mobile phase.

[0023] Furthermore, operator intervention carries the risk of introducing air bubbles and other problems into the flow path. From an analysis time perspective, this not only reduces throughput due to the time the LC cannot be used, but also leads to situations where analysis may be halted for an even longer period if the operator fails to recognize notifications of reduced mobile phase balance.

[0024] The purpose of this invention is to provide a liquid chromatograph and a control method for the liquid chromatograph that can provide a mobile phase to a storage bottle without stopping analysis and liquid delivery, and can suppress the mixing of air bubbles into the flow path.

[0025] Technical means for solving technical problems

[0026] To achieve the above objectives, the present invention is configured as follows.

[0027] A liquid chromatograph, comprising a liquid delivery device for discharging the mobile phase, a sample injection unit for injecting a sample into the mobile phase, a column for separating the sample delivered by the mobile phase, and a detection device for detecting the separated sample, includes: a storage bottle for storing the mobile phase delivered by the liquid delivery device, a mobile phase supply bottle for supplying the mobile phase to the storage bottle, a mobile phase supply pump for supplying the mobile phase stored in the mobile phase supply bottle to the storage bottle, and a control unit for determining the amount of mobile phase supplied from the mobile phase supply bottle to the storage bottle.

[0028] In a control method for a liquid chromatograph, which includes a liquid delivery device for discharging the mobile phase, a sample injection unit for injecting a sample into the mobile phase, a column for separating the sample delivered by the mobile phase, and a detection device for detecting the separated sample, the mobile phase delivered by the liquid delivery device is stored in a storage bottle, the mobile phase is stored in a mobile phase supply bottle that supplies the mobile phase to the storage bottle, the amount of mobile phase supplied from the mobile phase supply bottle to the storage bottle is determined, the operation of the mobile phase supply pump is controlled, and the mobile phase stored in the mobile phase supply bottle is supplied to the storage bottle.

[0029] Invention Effects

[0030] According to the present invention, a liquid chromatograph and a control method thereof are available that can provide a mobile phase to a storage bottle without stopping analysis and liquid delivery, and can suppress the mixing of air bubbles into the flow path. Attached Figure Description

[0031] Figure 1 This is a simplified structural diagram of the liquid chromatograph in Example 1.

[0032] Figure 2 This is a flowchart of the process of supplying mobile phase from the mobile phase supply bottle to the storage bottle in Example 1.

[0033] Figure 3 This is a simplified structural diagram of the liquid chromatograph used in Example 2.

[0034] Figure 4 This is a flowchart of the mobile phase supply process in Example 2.

[0035] Figure 5 This is an action illustration diagram of Example 3.

[0036] Figure 6 This is a simplified structural diagram of the liquid chromatograph used in Example 4. Detailed Implementation

[0037] Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. The drawings illustrate embodiments based on the principles of the present invention, but are typical examples for understanding the principles of the present invention and do not limit the present invention.

[0038] [Example]

[0039] (Example 1)

[0040] Reference Figure 1 Embodiment 1 of the present invention will be described below.

[0041] Figure 1 This is a simplified structural diagram of the liquid chromatograph 100 as an embodiment 1 of the present invention.

[0042] exist Figure 1 In the liquid chromatograph 100, there are: a delivery device 104 for discharging a mobile phase; a sample injection unit 105 for introducing a test sample (also referred to as the sample) into the analytical flow path; a separation column 106 for separating the test sample, which is introduced into the analytical flow path and transported by the mobile phase delivered by the delivery device 104, into individual components; and a detection device 108 for detecting the individual components contained in the test sample separated by the separation column 106.

[0043] In addition, the liquid chromatograph 100 includes: a storage bottle 102 for storing mobile phase disposed upstream of the liquid delivery device 104; a monitoring sensor 109 for detecting the mobile phase balance in the storage bottle 102; a mobile phase supply bottle 101 for storing mobile phase to supply mobile phase to the storage bottle 102; a mobile phase supply pump 103 for supplying mobile phase from the mobile phase supply bottle 101 to the storage bottle 102; and a control unit 111 for monitoring and supplying the mobile phase balance.

[0044] Vents 110 are provided on the mobile phase supply bottle 101 and the storage bottle 102 to equalize the pressure inside the bottle with atmospheric pressure. Therefore, one end of the vent 110 is located inside the storage bottle 102, and the other end of the vent 110 is open to the atmosphere.

[0045] The separation column 106 of the liquid chromatograph 100 is housed in a thermostat 107 to maintain a constant temperature around the column. However, the separation column 106 may also be used without being housed in the thermostat 107.

[0046] When the liquid chromatograph 100 is in operation, the liquid delivery device 104 transports the analyte sample introduced from the sample injection unit 105 to the separation column 106, so that it dissolves from the separation column 106, and delivers the mobile phase corresponding to the analysis in order to transport it to the detection unit 108.

[0047] Figure 2 This is a flowchart of the process of supplying mobile phase from mobile phase supply bottle 101 to storage bottle 102 based on the decrease in mobile phase during operation of liquid chromatograph 100.

[0048] The liquid delivery device 104 draws the mobile phase from the storage bottle 102 and provides the mobile phase to the LC analysis system, thereby reducing the amount of mobile phase remaining in the storage bottle 102. When the mobile phase remaining amount detected by the monitoring sensor 109 is below a specified value, the control unit 111 determines that the amount of mobile phase remaining in the storage bottle 102 is low (step S201).

[0049] The monitoring sensor 109 used to monitor the balance of the mobile phase can be a weight sensor, a float sensor, an electrostatic sensor, an optical sensor, etc.

[0050] When the monitoring sensor 109 detects that the mobile phase balance is below a specified value, the control unit 111 starts the mobile phase supply process (step S202). Then, by driving the mobile phase supply pump 103, the mobile phase is supplied from the mobile phase supply bottle 101 to the storage bottle 102 (step S203).

[0051] When the mobile phase supply pump 103 supplies mobile phase to the storage bottle 102, the control unit 111 determines whether the amount of mobile phase in the storage bottle 102 is above a certain level based on the remaining amount of mobile phase detected by the monitoring sensor 109 (step S204). When the control unit 111 determines that the amount of mobile phase in the storage bottle 102 is above a certain level, the control unit 111 stops the mobile phase supply pump 103 and stops supplying mobile phase from the mobile phase supply bottle 101 to the storage bottle 102 (step S205). Then, the mobile phase supply process is stopped (ended) (step S206).

[0052] As described above, according to Embodiment 1 of the present invention, the amount of mobile phase remaining in the storage bottle 102 is monitored by the monitoring sensor 109. When the amount of mobile phase remaining in the storage bottle 102 is below a predetermined value, the control unit 111 drives the mobile phase supply pump 103 to supply mobile phase from the mobile phase supply bottle 101 to the storage bottle 102. Therefore, it is not necessary for the operator to identify the decrease in the mobile phase remaining amount and supply mobile phase, and it is also possible to avoid the introduction of air bubbles into the flow path due to the operator's operation.

[0053] That is, according to Example 1, a liquid chromatograph and a liquid chromatograph control method can be realized that can provide a mobile phase to the storage bottle 102 without stopping analysis and liquid delivery, and can suppress the mixing of bubbles into the flow path.

[0054] In this embodiment 1, the stopping timing of the mobile phase supply pump 103 is determined based on the remaining amount of mobile phase in the storage bottle 102 as determined by the monitoring sensor 109. For example, the same mobile phase supply process can also be achieved by calculating the driving time of the mobile phase supply pump 103 based on the discharge flow rate of the mobile phase supply pump 103 and the volume of mobile phase to be supplied to the storage bottle 102, and then operating and stopping the mobile phase supply pump 103 according to the calculated driving time.

[0055] Additionally, the control unit 111 can calculate the remaining volume of the mobile phase in the storage bottle 102 based on the delivery volume per unit time and the operating time of the delivery device 104. If the volume is below a predetermined value, the control unit 111 can drive the mobile phase supply pump 103 to start supplying the mobile phase from the mobile phase supply bottle 101 to the storage bottle 109. In this case, as described above, by configuring the control unit 101 to calculate the driving time of the mobile phase supply pump 103 based on the discharge flow rate of the mobile phase supply pump 103 and the volume of mobile phase to be supplied to the storage bottle 102, and stopping the mobile phase supply pump 103 based on the calculated driving time, the monitoring sensor 109 can be omitted.

[0056] (Example 2)

[0057] Next, refer to Figure 3 Example 2 of the present invention is described below.

[0058] exist Figure 3 The sample inlet 105, the temperature control device 107, and the detection device 108 downstream of the liquid delivery device 104 are not shown in the diagram. The liquid chromatograph 100A is located upstream of the liquid delivery device 104 and includes: a storage bottle 102 for storing the mobile phase; a monitoring sensor 109 for detecting the mobile phase balance in the storage bottle 102; a mobile phase supply bottle 101 for supplying the mobile phase to the storage bottle 102; an information storage unit 301 provided in the mobile phase supply bottle 101; an information reading unit 302 for reading information recorded in the information storage unit 301; a mobile phase supply pump 103 for supplying the mobile phase from the mobile phase supply bottle 101 to the storage bottle 102; a bubble detection sensor 303 for detecting bubbles in the piping between the mobile phase supply pump 103 and the mobile phase supply bottle 101; a display unit 306; and a control unit 111 for monitoring and supplying the mobile phase balance.

[0059] The interiors of the mobile phase supply bottle 101 and the storage bottle 102 are connected by a gas conduit 304 configured to equalize the pressure within the bottles. Specifically, the gas conduit 304 connects the storage bottle 102 and the mobile phase supply bottle 101, maintaining a constant pressure between the storage bottle 102 and the mobile phase supply bottle 101. Furthermore, a vent 110 is provided inside the mobile phase supply bottle 101 to equalize the pressure within it with atmospheric pressure. The other end of the vent 110, located on the outer side of the mobile phase supply bottle 101, is connected to a filter 305. This filter 305 prevents the mobile phase within the supply bottle 101 from diffusing to the outside and prevents dust or other contaminants from entering the mobile phase supply bottle 101.

[0060] The information holding unit 301 of the mobile phase supply bottle 101 stores information related to the mobile phase, such as the type and manufacturing date of the mobile phase contained in the mobile phase supply bottle 101. The control unit 111 determines whether the mobile phase supply bottle 101 is properly set up based on the information contained in the information holding unit 301 read by the information reading unit 302, the presence or absence of the mobile phase supply bottle 101, the determination of incorrect setting, the service life, etc.

[0061] For the information retention unit 301, barcodes or RFID tags can be considered.

[0062] Figure 4 This is a flowchart of the mobile phase supply process in Embodiment 2 of the present invention.

[0063] When the remaining amount of mobile phase determined by the monitoring sensor 109 is below a specified value, the control unit 111 determines that the remaining amount of mobile phase in the storage bottle 102 is low (step S401) and starts the mobile phase supply process (step S402).

[0064] After the mobile phase supply process begins in step S402, the control unit 111 reads the information stored in the information storage unit 301 of the mobile phase supply bottle 101 via the information reading unit 302, and confirms that the mobile phase supply bottle 101 is properly set (step S403). At this time, if the mobile phase supply bottle 101 has been set and the mobile phase supply is exhausted, or if it is determined that the remaining amount of mobile phase in the mobile phase supply bottle 101 is low, an instruction for setting or replacing the mobile phase supply bottle 101 is displayed on the display unit 306 (step S404).

[0065] When the control unit 111 determines that the mobile phase supply bottle 101 is in an appropriate state, the control unit 111 drives the mobile phase supply pump 103 to start supplying mobile phase from the mobile phase supply bottle 101 to the storage bottle 102 (step S405).

[0066] If the bubble sensor 303 detects bubbles in the piping connecting the mobile phase supply pump 103 and the mobile phase supply bottle 101 during the discharge of the mobile phase by the mobile phase supply pump 103 (step S406), the control unit 111 supplies all the mobile phase in the mobile phase supply bottle 101 to the storage bottle 102, determines that the mobile phase supply bottle 101 is empty, and stops the mobile phase supply pump 103 (step S408).

[0067] Next, in step S408, the control unit 111 displays a replacement instruction for the mobile phase supply bottle 101 on the display unit 306 (step S410), and ends the mobile phase supply process (step S412).

[0068] In step S406, if the bubble sensor 303 does not detect any bubbles in the piping, proceed to step S407. In step S407, the monitoring sensor 109 performs overflow monitoring during the period when the mobile phase supply pump 103 supplies mobile phase to the storage bottle 102, to ensure that the mobile phase in the storage bottle 102 does not exceed the storage limit capacity of the storage bottle 102. If the monitoring sensor 109 does not detect any overflow, return to step S406.

[0069] In step S407, if the mobile phase reaches a predetermined value or higher based on the output value of the monitoring sensor 109, the control unit 111 determines that the risk of overflow is high and, as an overflow detection, stops the mobile phase supply pump 103, ending the mobile phase supply (step S409). In the case of stopping due to overflow detection, the control unit 111 calculates the remaining mobile phase in the mobile phase supply bottle 101 based on the drive time and flow rate of the mobile phase supply pump 103, updates the remaining amount, and records it (step S411). Then, the mobile phase supply process ends (S412).

[0070] According to Embodiment 2 of the present invention, in addition to achieving the same effects as in Embodiment 1, the following effects can also be obtained.

[0071] In Example 2, since the interior of the mobile phase supply bottle 101 and the interior of the storage bottle 102 are connected by a gas conduit 304, the pressure inside the mobile phase supply bottle 101 and the interior of the storage bottle 102 are equal. This avoids errors in detecting the remaining amount of mobile phase in the storage bottle 102 due to pressure differences, and enables more accurate remaining amount detection.

[0072] Furthermore, in Embodiment 2, the mobile phase supply bottle 101 is configured to have an information storage unit 301 that records information such as the type and manufacturing date of the mobile phase contained in the mobile phase supply bottle 101. The information reading unit 302 reads the information recorded in the information storage unit 301, and the control unit 111 performs checks on the presence or absence of the mobile phase supply bottle 101, determines if it is incorrectly installed, and determines its expiration date, confirming that the mobile phase supply bottle 101 is properly installed. Therefore, it is possible to identify whether an appropriate mobile phase supply bottle 101 is installed before the mobile phase is supplied to the liquid chromatograph 100.

[0073] Furthermore, in Embodiment 2, since a filter 305 is connected to the vent 110 of the mobile phase supply bottle 101, the mobile phase inside the mobile phase supply bottle 101 can be prevented from diffusing to the outside, and dust and other particles around the mobile phase supply bottle 101 can be prevented from entering the mobile phase supply bottle 101.

[0074] Alternatively, a monitoring sensor (the same sensor as monitoring sensor 109) can be provided to detect the remaining amount of mobile phase in the mobile phase supply bottle 101. The control unit 111 identifies the remaining amount of mobile phase in the mobile phase supply bottle 101 and displays it on the display unit 306.

[0075] (Example 3)

[0076] Next, Embodiment 3 of the present invention will be described.

[0077] In the examples shown in Examples 1 and 2, as a pre-stage before the monitoring sensor 109 detects a decrease in the mobile phase balance in the storage bottle 102 and drives the mobile phase supply pump 103, the following steps are taken: Figure 5 This section explains the functions of facilitating the preparation and setup of the mobile phase supply bottle 101.

[0078] The liquid chromatograph in Example 3 has the same structure as that in Example 1 or Example 2, therefore, illustrations and detailed descriptions are omitted. However, it is assumed that the same display unit 306 as in Example 2 was added to Example 1.

[0079] Figure 5 This is an operational illustration diagram of Example 3, showing an example of the shift in the remaining amount of mobile phase in the storage bottle 102 calculated based on the output value of the monitoring sensor 109. The vertical axis represents the remaining amount of mobile phase, and the horizontal axis represents the number of days elapsed.

[0080] exist Figure 5 In this process, after the mobile phase is supplied from the mobile phase supply bottle 101 to the storage bottle 102, the storage bottle 102 is in a state 501 filled with mobile phase. When the mobile phase is consumed by the analytical operation of the liquid chromatograph 100 or 100A, the remaining mobile phase in the storage bottle 102 decreases. At this time, an operation preparation mobile phase balance VA is set to urge the operation preparation of the mobile phase supply bottle 101 before the control unit 111 reaches the mobile phase balance state 503 that enables the mobile phase supply pump 103 to operate.

[0081] When the remaining amount of mobile phase in the storage bottle 102, calculated based on the detection value of the monitoring sensor 109, reaches the mobile phase remaining amount VA for operation preparation, the control unit 111 causes the display unit 306 to display the operation preparation of the mobile phase supply bottle 101 at that moment (state 502).

[0082] When the liquid chromatograph in Example 3 is configured with the same structure as in Example 2, the control unit 111 can be configured to read the information stored in the information holding unit 301 of the mobile phase supply bottle 101 by the information reading unit 302, and at the moment (state 502) before the operation preparation mobile phase balance VA is reached before the state 503 of the mobile phase supply pump 103 is operated, identify the presence or absence of the mobile phase supply bottle 101 and the mobile phase balance in the mobile phase supply bottle 101, and if there is no mobile phase required for supplying to the storage bottle 102, cause the display unit 306 to output the setting instruction and replacement instruction of the mobile phase supply bottle 101.

[0083] According to Embodiment 3, in addition to obtaining the same effects as Embodiments 1 and 2, since the operation preparation of the mobile phase supply bottle 101 can be displayed before the control unit 111 reaches the operation preparation mobile phase balance state 503 for operating the mobile phase supply pump 103, the replacement preparation of the mobile phase supply bottle 101 can be performed before the mobile phase balance of the mobile phase supply bottle 101 becomes the amount required for supplying to the storage bottle 102.

[0084] (Example 4)

[0085] Next, using Figure 6 Embodiment 4 of the present invention will be described below.

[0086] In the example described in Example 2, the liquid chromatograph 100B of Example 4 is housed in a housing 601 with high light-shielding properties, and a deuterium lamp 602 is provided inside the housing 601.

[0087] The control unit 111 illuminates the deuterium lamp 602 to sterilize the contents of the storage bottle 102. At this time, it is preferable that the deuterium lamp 602 is always on, but the ultraviolet rays emitted by the deuterium lamp 602 not only have a sterilization effect, but can also cause material deterioration. Therefore, a control algorithm that irradiates the material for a certain period of time, such as every 24 hours, can be used to address this.

[0088] In addition, in this embodiment 4, the method of irradiating ultraviolet light from the outside of the storage bottle 102 by the deuterium lamp 602 was described, but the same effect can also be expected by directly irradiating the inside of the storage bottle 102 by connecting a small deuterium lamp to the cap of the storage bottle 102.

[0089] In addition, in this embodiment 4, a sterilization function based on a deuterium lamp 602 is proposed for the storage bottle 102, which is likely to store the mobile phase for a long time. However, the same function can also be provided by equipping the mobile phase supply bottle 101 with a deuterium lamp that irradiates ultraviolet light.

[0090] According to Example 4, in addition to achieving the same effect as in Example 2, the mobile phase in the storage bottle 102 can be kept in a sterilized state for a long time.

[0091] Label Explanation

[0092] 100, 100A, 100B…Liquid chromatograph, 101…Mobile phase supply bottle, 102…Storage bottle, 103…Mobile phase supply pump, 104…Liquid delivery device, 105…Sample injection unit, 106…Separation column, 107…Thermostat, 108…Detection device, 109…Monitoring sensor, 110…Ventilator, 111…Control unit, 301…Information storage unit, 302…Information reading unit, 303…Bubble detection sensor, 304…Gas conduit, 305…Filter, 306…Display unit, 601…Light-shielding housing, 602…Deuterium lamp.

Claims

1. A liquid chromatograph, comprising: The liquid chromatograph comprises: a delivery device for discharging a mobile phase, a sample injection unit for injecting a sample into the mobile phase delivered from the delivery device, a separation column for separating the sample delivered from the mobile phase delivered from the sample injection unit, and a detection device for detecting the sample separated by the separation column. A storage bottle for storing the mobile phase delivered by the liquid delivery device; A mobile phase supply bottle that supplies the mobile phase to the storage bottle; The mobile phase stored in the mobile phase supply bottle is supplied to the mobile phase supply pump in the storage bottle; and A control unit that controls the operation of the mobile phase supply pump and determines the amount of mobile phase supplied from the mobile phase supply bottle to the storage bottle. It also includes a monitoring sensor to detect the remaining amount of the mobile phase stored in the storage bottle. When the control unit detects that the remaining amount of mobile phase in the storage bottle is below a predetermined value based on the monitoring sensor's readings, it drives the mobile phase supply pump to supply the mobile phase from the mobile phase supply bottle to the storage bottle. When the control unit determines that the amount of mobile phase in the storage bottle is above a certain level based on the remaining amount of mobile phase detected by the monitoring sensor, it stops the mobile phase supply pump. Also includes: A bubble detection sensor is used to detect bubbles in the piping between the mobile phase supply bottle and the mobile phase supply pump. A gas conduit connecting the storage bottle and the mobile phase supply bottle to maintain a constant pressure in both the storage bottle and the mobile phase supply bottle; and The filter connected to the vent of the mobile phase supply bottle, The control unit drives the mobile phase supply pump to supply the mobile phase from the mobile phase supply bottle to the storage bottle. The bubble detection sensor detects bubbles in the piping, thereby determining that the mobile phase supply bottle is empty and stopping the mobile phase supply pump.

2. The liquid chromatograph as described in claim 1, characterized in that, The mobile phase supply bottle has an information storage unit that stores information related to the mobile phase contained within the mobile phase supply bottle. This includes an information reading unit that reads the information stored in the information storage unit. The control unit determines whether the mobile phase supply bottle is set to an appropriate state based on the information read by the information reading unit and stored in the information storage unit.

3. The liquid chromatograph as described in claim 1, characterized in that, Including the display section, When the remaining amount of the mobile phase in the storage bottle reaches the operational readiness level before driving the mobile phase supply pump, the control unit causes the display unit to display the operational readiness of the mobile phase supply bottle.

4. The liquid chromatograph as described in claim 1, characterized in that, This includes a deuterium lamp that irradiates the storage bottle or the mobile phase supply bottle with ultraviolet light.

5. A method for controlling a liquid chromatograph, the liquid chromatograph comprising: The control method of the liquid chromatograph is characterized by comprising a liquid delivery device for discharging the mobile phase, a sample injection unit for injecting a sample into the mobile phase discharging from the liquid delivery device, a column for separating the sample delivered by the mobile phase discharging from the sample injection unit, and a detection device for detecting the sample separated by the separation column. The mobile phase delivered by the liquid delivery device is stored in a storage bottle. The mobile phase is stored in a mobile phase supply bottle that supplies the mobile phase to the storage bottle. The amount of mobile phase supplied from the mobile phase supply bottle to the storage bottle is determined. The operation of the mobile phase supply pump is controlled to supply the mobile phase stored in the mobile phase supply bottle to the storage bottle. The remaining amount of the mobile phase stored in the storage bottle is also detected by a monitoring sensor. If, based on the detection value of the monitoring sensor, the remaining amount of the mobile phase in the storage bottle is below a predetermined value, the mobile phase supply pump is activated to supply the mobile phase from the mobile phase supply bottle to the storage bottle. Based on the remaining amount of the mobile phase detected by the monitoring sensor, it is determined that the amount of mobile phase in the storage bottle is above a certain level. Stop the mobile phase supply pump. Bubbles are also detected in the piping between the mobile phase supply bottle and the mobile phase supply pump using a bubble detection sensor. The storage bottle and the mobile phase supply bottle are connected by a gas conduit to maintain a constant pressure in both the storage bottle and the mobile phase supply bottle. The mobile phase supply pump is driven to supply the mobile phase from the mobile phase supply bottle to the storage bottle. The bubble detection sensor detects bubbles in the piping, thereby determining that the mobile phase supply bottle is empty, and the mobile phase supply pump is stopped.

6. The control method for a liquid chromatograph as described in claim 5, characterized in that, The mobile phase supply bottle has an information storage unit that stores information related to the mobile phase contained within the mobile phase supply bottle. Based on the information read by the information reading unit stored in the information storage unit, it is determined whether the mobile phase supply bottle is set to an appropriate state.

7. The control method for a liquid chromatograph as described in claim 5, characterized in that, When the remaining amount of the mobile phase in the storage bottle reaches the operating preparation mobile phase balance before driving the mobile phase supply pump, the display unit displays the operating preparation of the mobile phase supply bottle.

8. The control method for a liquid chromatograph as described in claim 5, characterized in that, The storage bottle or the mobile phase supply bottle is irradiated with ultraviolet light using a deuterium lamp.

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