Liquid chromatography device

Abstract

The purpose of the present invention is to provide a liquid chromatography device capable of accurately managing and controlling the temperature of an analytical column while suppressing an increase in environmental load. The liquid chromatography device is provided with: a column cartridge provided with a column-side heating block configured so as to transfer heat to an analysis column; and a main body part which is configured so as to be able to mount the column box, and which is provided with a column box-side heating block that is in contact with the column-side heating block and transfers heat to the column-side heating block. The main body part is provided with: a first temperature sensor for measuring the temperature of the column box-side heating block; a second temperature sensor that measures a temperature inside the column box; and a determination unit that determines whether or not the column box-side heating block is in contact with the column-side heating block on the basis of measurement results of the first temperature sensor and the second temperature sensor (referring to fig. 1).

Description

Technical Field

[0001] The present invention relates to a liquid chromatography device. Background Art

[0002] Liquid chromatography is a well-known analytical device for analyzing substances contained in a sample. Liquid chromatographs pressurize a liquid mobile phase using a pump or the like and pass it through an analytical column. Utilizing the difference in interactions with the stationary phase and the mobile phase, they efficiently separate and detect the substances being analyzed.

[0003] In a liquid chromatograph, liquid delivery and temperature conditions are set for each analyte. Within these set conditions, the various components are controlled to separate and detect the analyte. Controlling the temperature of the analytical column to maintain the set temperature conditions is crucial in liquid chromatographs, and therefore, liquid chromatographs are equipped with a column box for temperature regulation.

[0004] However, the column box of conventional liquid chromatography apparatuses regulates the temperature of the analytical column in a constant temperature atmosphere, making it impossible to accurately measure or estimate the temperature of the analytical column. The analytical column is a component that requires replacement, making it difficult to attach a temperature sensor to the separation column.

[0005] For example, Patent Documents 1 and 2 disclose liquid chromatography apparatuses in which sensors and heaters are mounted on the analytical column itself, which is a consumable component. However, when the analytical column itself is equipped with a sensor and heater, if the analytical column needs to be replaced due to performance degradation or clogging, the sensor and heater mounted on the analytical column must also be discarded, resulting in an increased environmental burden.

[0006] Prior art literature

[0007] Patent Literature

[0008] Patent Document 1: Japanese Patent Application Laid-Open No. 2014-157139

[0009] Patent Document 2: Japanese Patent Application Laid-Open No. 2013-195392 Summary of the Invention

[0010] Problems to be solved by the invention

[0011] The present invention provides a liquid chromatograph capable of suppressing an increase in environmental load and accurately managing and controlling the temperature of an analytical column.

[0012] Means for solving problems

[0013] The liquid chromatography apparatus of the present invention comprises: a column cartridge configured to carry an analytical column and comprising a column-side heating block configured to transfer heat to the analytical column; and a main body configured to carry the column cartridge and comprising a column box-side heating block configured to be in contact with and transfer heat to the column-side heating block, the main body comprising: a first temperature sensor configured to measure the temperature of the column box-side heating block; a second temperature sensor configured to measure the temperature inside the column cartridge; and a determination unit configured to determine whether the column box-side heating block is in contact with the column-side heating block based on measurement results of the first temperature sensor and the second temperature sensor.

[0014] Effects of the Invention

[0015] According to the present invention, it is possible to provide a liquid chromatograph capable of accurately managing and controlling the temperature of an analytical column while suppressing an increase in environmental load. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 This is a schematic diagram illustrating the overall structure of the liquid chromatography apparatus 100 according to the first embodiment.

[0017] Figure 2 It is a schematic perspective view illustrating an example of the structure of the column cartridge 1 .

[0018] Figure 3 It is a perspective view showing an example of the structure of the upper surface of the column cartridge 1 .

[0019] Figure 4 It is a perspective view showing an example of the structure of the bottom surface of the column cartridge 1 .

[0020] Figure 5 It is a cross-sectional view for explaining the details of the structure of the column cartridge 1 and the details of the structure of the main body 50 .

[0021] Figure 6 It is a cross-sectional view illustrating the structure of a liquid chromatography apparatus 100 according to the second embodiment.

[0022] Figure 7 It is a cross-sectional view illustrating the structure of a liquid chromatography apparatus 100 according to the third embodiment. DETAILED DESCRIPTION

[0023] The present embodiment is described below with reference to the accompanying drawings. In the accompanying drawings, functionally identical elements are sometimes denoted by the same reference numerals. Furthermore, the accompanying drawings illustrate embodiments and installation examples based on the principles of the present disclosure. These drawings are provided for understanding the present disclosure and are not intended to limit the present disclosure in any way. The descriptions in this specification are merely exemplary and do not in any way limit the claims or application examples of the present disclosure.

[0024] In this embodiment, the description is provided in sufficient detail to enable those skilled in the art to implement the present disclosure. However, other installations and methods are also possible, and it should be understood that changes in structure and construction, as well as replacement of various elements, can be made without departing from the scope and spirit of the technical concept of the present disclosure. Therefore, the following description should not be interpreted as being limited to this.

[0025] [First embodiment]

[0026] Reference Figure 1 The overall structure of a liquid chromatography apparatus 100 according to the first embodiment will be described. As an example, the liquid chromatography apparatus 100 includes a column cartridge 1, an analytical column 10, a liquid delivery pump 20, an injector 30, a detection unit 40, and a main body 50. The liquid delivery pump 20, the injector 30, the column cartridge 1, and the detection unit 40 are connected by piping.

[0027] The liquid delivery pump 20 is located at the most upstream side of the analytical flow path and has the function of drawing up the mobile phase from a container (not shown) containing the mobile phase and delivering the liquid to the injector 30. The injector 30 has the function of aspirating a sample from a sample container containing the sample using, for example, a probe and injecting the aspirated sample into the analytical column 10 provided in the column cartridge 1.

[0028] The column cartridge 1 is a container configured to carry and house an analytical column 10. The analytical column 10 is secured to the housing of the column cartridge 1 using a metal block MB. The metal block MB includes a column-side heating block 7A below it. This column-side heating block 7A is configured to be exposed to the outside through a hole provided in the bottom surface of the column cartridge 1.

[0029] The detection unit 40 analyzes the mobile phase discharged from the analytical column 10 to analyze the target micro-substance. The main body 50 includes a calculation control unit 200. Based on signals from the detection unit 40, the calculation control unit 200 outputs various calculations related to the target substance and also outputs control signals for controlling the liquid delivery pump 20, the ejector 30, and the detection unit 40.

[0030] The main body 50 also includes a column box that generates heat for the column-side heating block 7A. The column box is a mechanism for generating heat to control the temperature of the analytical column 10 to a constant level. For example, it is generally composed of a heater 51 and a column-side heating block 52. The column-side heating block 52 is configured to contact the lower surface of the column-side heating block 7A. Heater 51 is connected to, for example, the lower surface of the column-side heating block 52. Heater 51 generates heat when operated, and this heat is transferred to the column-side heating block 52.

[0031] The liquid chromatography apparatus 100 includes a first temperature sensor 53 and a second temperature sensor 54 as temperature sensors for measuring the temperature of the analytical column 10. The first temperature sensor 53 is embedded in the aforementioned column box heater block 52 and measures the temperature of the column box heater block 52. Meanwhile, the second temperature sensor 54 is positioned and configured to measure the temperature inside the column box 1, for example, the temperature of the metal block MB. As an example, the second temperature sensor 54 can be configured to measure the temperature through a window provided in the column box 1.

[0032] Reference Figure 2 An example of the structure of the column box 1 is described in the schematic perspective view of FIG. Figure 2 As shown, the column cartridge 1 includes a resin upper housing portion 2 and a resin lower housing portion 3. The upper housing portion 2 and the lower housing portion 3 form a housing H that houses the analytical column 10. Specifically, the upper housing portion 2 is positioned above the analytical column 10, while the lower housing portion 3 is positioned below the analytical column 10. The analytical column 10 is housed within the housing H formed by the upper housing portion 2. As will be described later, the analytical column 10 is secured within the housing H by a metal block MB.

[0033] A handle (protrusion) 5 is formed on the upper surface of the housing upper portion 2. A first flow opening 4, serving as one end of an analytical column 10, is formed on the side surface of the housing between the housing upper portion 2 and the housing lower portion 3. The analytical column 10 is retained within the housing H with the first flow opening 4 exposed from the housing H. The mobile phase flows into this first flow opening 4. A second flow opening 9, serving as the other end of the analytical column 10, is formed on the opposite side surface of the housing H. Similarly, the analytical column 10 is retained within the housing H with the second flow opening 9 exposed to the outside of the housing H.

[0034] Reference Figure 3 The perspective view shows an example of the structure of the upper surface of the column box 1. The upper surface of the housing upper portion 2 is provided with windows 6A, 6B, 6C, 6D, and 6E for temperature detection. These windows 6A to 6E are connected to the storage space of the analytical column 10. In addition, the windows 6A, 6B, 6C, 6D, and 6E are arranged along the length direction of the analytical column 10. Figure 3 In the embodiment, some of the windows 6B, 6C, and 6D are formed at the position where the handle 5 is formed, and the other windows 6A and 6E are arranged outside the handle 5 (on the extension line in the longitudinal direction). However, this is an example and is not limited to the embodiment shown in the figure. In addition, the diameters of the windows 6A, 6B, 6C, 6D, and 6E are preferably about 1.4 mm or less.

[0035] Figure 4An example of the bottom surface structure of the column cartridge 1 is shown in FIG. An opening 3A is formed on the bottom surface of the housing lower portion 3. A column-side heating block 7A of the metal block lower portion 7, described later, is inserted into this opening 3A, and the column-side heating block 7A is exposed to the outside through the opening 3A. The column-side heating block 7A contacts the column oven-side heating block 52, receiving heat from the column oven and transferring this heat to the analytical column 10.

[0036] Reference Figure 5 The details of the structure of the column cartridge 1 and the main body 50 will be described. As previously described, the column cartridge 1 includes windows 6A to 6E extending from the top surface to the metal block MB for temperature detection. Infrared temperature sensors 54A to 54E, serving as an example of the second temperature sensor 54, irradiate infrared light from these windows 6A to 6E and detect the reflected light. The infrared temperature sensors 54A to 54E are not located inside the column cartridge 1 but rather outside it and constitute part of the main body 50.

[0037] The analytical column 10 mounted in the column cartridge 1 is connected to a guide block 30A and a guide block 40A at the first flow passage 4 and the second flow passage 9, respectively. The guide blocks 30A and 40A are mounted on guide rails (not shown) extending horizontally in the drawing and are configured to be movable horizontally in the drawing. The analytical column 10 is connected to the aforementioned injector 30 and detection unit 40 via these guide blocks 30A and 40A.

[0038] The detection signals from the first temperature sensor 53 and the second temperature sensor 54 are input to the calculation control unit 200, which estimates the temperature of the analytical column 10. Furthermore, the calculation control unit 200 determines whether the column-side heating block 7A and the column-box-side heating block 52 are in proper contact based on the difference between the detection signals from the first temperature sensor 53 and the second temperature sensor 54. In other words, the calculation control unit 200 functions as a determination unit that determines whether the two heating blocks 7A and 52 are in proper contact based on the difference between the detection signals from the temperature sensors 53 and 54A to 54E.

[0039] When the two heating blocks 7A and 52 are in proper contact, heat from the column-side heating block 52 is transferred to the column-side heating block 7A, preventing a significant temperature difference between the two. On the other hand, when the two heating blocks 7A and 52 are not in proper contact, heat from the column-side heating block 52 is not sufficiently transferred to the column-side heating block 7A, resulting in a significant drop in the temperature of the column-side heating block 7A compared to the temperature of the column-side heating block 52. The calculation control unit 200 can determine whether proper contact between the two heating blocks is achieved based on this temperature difference.

[0040] As described above, according to the liquid chromatography apparatus 100 of the first embodiment, a column cartridge 1 equipped with a column-side heating block 7A is mounted on the main body 50, and the oven-side heating block 52 of the main body 50 is arranged in contact with the column-side heating block 7A. The first temperature sensor 53 mounted on the oven-side heating block 52 and the second temperature sensors 54A to 54E that measure the temperature of the column cartridge 1 enable measurement of the temperature of the analytical column 10 and determination of proper contact between the two heating blocks 7A and 52. Since both temperature sensors 53 and 54 are located on the main body 50, this embodiment provides a liquid chromatograph that can accurately manage and control the temperature of the analytical column while minimizing environmental impact.

[0041] [Second embodiment]

[0042] Next, refer to Figure 6 The liquid chromatography apparatus 100 of the second embodiment will be described. The liquid chromatography apparatus 100 of the second embodiment is the same as that of the first embodiment in terms of its overall structure and the construction of the column cartridge 1 ( Figures 1 to 4 ), and therefore, repeated descriptions are omitted. The second embodiment differs from the first embodiment in that the second temperature sensor 54 is a probe-type temperature sensor 54F including a contact-type probe.

[0043] The probe type temperature sensor 54F includes a contact probe that can be inserted into the windows 6A to 6E. The contact probe contacts the metal block MB, for example, to measure the temperature of the analytical column 10. A plurality of probe type temperature sensors 54F may be provided corresponding to the number of windows 6A to 6E.

[0044] As described above, according to the liquid chromatography apparatus 100 of the second embodiment, similarly to the first embodiment, a liquid chromatograph capable of accurately managing and controlling the temperature of the analytical column while suppressing an increase in environmental load can be provided.

[0045] [Third embodiment]

[0046] Next, refer to Figure 7 The liquid chromatography apparatus 100 of the third embodiment will be described. The liquid chromatography apparatus 100 of the second embodiment is the same as that of the first embodiment in terms of its overall structure and the construction of the column cartridge 1 ( Figures 1 to 4 The third embodiment differs from the first embodiment in that the second temperature sensor 54G is embedded in the column-side heating block 52 and is arranged so as to reach the column-side heating block 7A.

[0047] In this third embodiment, the column-side heater block 52 is thermally separated into a first portion R1 and a second portion R2 by a heat insulating material 57. The heater 51 contacts the first portion R1 and transfers heat only to the first portion R1, not to the second portion R2. Meanwhile, the second temperature sensor 54G described above is embedded in the second portion R2, exposed on its surface, and in contact with or close to the column-side heater block 7A.

[0048] In this configuration, when the column-side heating block 7A and the column-box-side heating block 52 are in proper contact, heat from the heater 51 is first transferred to the first portion R1 of the column-box-side heating block 52 (heating the first portion R1), then to the column-side heating block 7A, and further to the second portion R2. Consequently, no significant temperature difference occurs between the first portion R1 and the second portion R2. This difference is detected by the second temperature sensor 54G and the first temperature sensor 53.

[0049] On the other hand, when the column-side heat block 7A and the oven-side heat block 52 are not in proper contact, the heat transferred from the heater 51 to the first portion R1 of the oven-side heat block 52 is not sufficiently transferred to the column-side heat block 7A, and thus the heat is not sufficiently transferred to the second portion R2. Consequently, the temperature difference between the first portion R1 and the second portion R2 increases, which is detected by the second temperature sensor 54G and the first temperature sensor 53.

[0050] In the third embodiment, both temperature sensors 53 and 54G are located on the column box-side heating block 52. Therefore, even when the analytical column 10 is replaced, the temperature sensors 53 and 54G do not need to be replaced, thereby suppressing an increase in environmental load. Therefore, according to the liquid chromatography apparatus 100 of the third embodiment, similar to the first embodiment, a liquid chromatograph can be provided that can accurately manage and control the temperature of the analytical column while suppressing an increase in environmental load.

[0051] Furthermore, the present invention is not limited to the above-described embodiments and can be modified in various ways. For example, the above-described embodiments are described in detail to facilitate understanding of the present invention, and the present invention is not limited to a method that necessarily includes all of the described structures. In addition, a portion of the structure of a certain embodiment can be replaced with the structure of another embodiment. In addition, the structure of another embodiment can be added to the structure of a certain embodiment. In addition, a portion of the structure of each embodiment can be deleted, or other structures can be added or replaced.

[0052] Description of Reference Numerals

[0053] 1—column box; 2—upper part of the shell; 3—lower part of the shell; 3A—opening; H—shell; 4—first flow path; 5—handle; 6A~6E—window; 7A—column side heating block; MB—metal block; 9—second flow path; 10—analytical column; 20—liquid delivery pump; 30—injector; 40—detection unit; 50—main body; 51—heater; 52—column box side heating block; 53—first temperature sensor; 54, 54A~54G—second temperature sensor; 200—operation control unit.

Claims

1. A liquid chromatography device, characterized in that have: a column cartridge configured to carry an analytical column and comprising a column-side heating block configured to transfer heat to the analytical column; and The main body is configured to be able to carry the column cartridge and includes a column box side heating block that contacts the column side heating block and transfers heat to the column side heating block. The main body comprises: a first temperature sensor for measuring the temperature of the column oven side heating block; a second temperature sensor that measures the temperature within the cartridge; and A determination unit determines whether the column-side heating block is in contact with the column-side heating block based on measurement results of the first temperature sensor and the second temperature sensor.

2. The liquid chromatography device according to claim 1, characterized in that The column cartridge includes a window extending from the surface thereof to the vicinity of the analytical column. The second temperature sensor measures the temperature inside the column cartridge through the window.

3. The liquid chromatography device according to claim 2, characterized in that The second temperature sensor is an infrared temperature sensor that irradiates light from the window portion and measures the temperature inside the column box based on the reflected light.

4. The liquid chromatography device according to claim 2, characterized in that The second temperature sensor is a probe-type temperature sensor including a probe that is inserted from the window and can reach the vicinity of the analytical column.

5. The liquid chromatography device according to claim 1, characterized in that The liquid chromatography device further comprises: a heat insulating member that thermally isolates the first portion from the second portion of the column-side heating block, The first portion is heated by a heater, the first temperature sensor measures the temperature of the first portion, The second temperature sensor is configured to be provided at the second portion and to be in contact with or close to the column-side heating block.

6. A liquid chromatography device, characterized in that The liquid chromatography apparatus is configured to be able to carry a column cartridge and includes a column box-side heating block that contacts a column-side heating block and transfers heat to the column-side heating block. The column cartridge is configured to be able to carry an analytical column and includes a column-side heating block that transfers heat to the analytical column. The liquid chromatography device comprises: a first temperature sensor for measuring the temperature of the column oven side heating block; a second temperature sensor that measures the temperature within the cartridge; and A determination unit determines whether the column-side heating block is in contact with the column-side heating block based on measurement results of the first temperature sensor and the second temperature sensor.

7. The liquid chromatography device according to claim 6, characterized in that The column cartridge includes a window extending from the surface thereof to the vicinity of the analytical column. The second temperature sensor measures the temperature inside the column cartridge through the window.

8. The liquid chromatography device according to claim 7, characterized in that The second temperature sensor is an infrared temperature sensor that irradiates light from the window portion and measures the temperature inside the column box based on the reflected light.

9. The liquid chromatography device according to claim 7, characterized in that The second temperature sensor is a probe-type temperature sensor including a probe that is inserted from the window and can reach the vicinity of the analytical column.

10. The liquid chromatography device according to claim 6, characterized in that The liquid chromatography device further comprises: a heat insulating member that thermally isolates the first portion from the second portion of the column-side heating block, The first portion is heated by a heater, the first temperature sensor measures the temperature of the first portion, The second temperature sensor is configured to be provided at the second portion and to be in contact with or close to the column-side heating block.

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