Column oven for analytical instruments

Abstract

To provide a column oven of an analyzing device which is equipped with a plurality of columns, and is capable of efficiently performing heat conduction on column basis, recognizing a column cartridge that holds a column, and being easily exchanged on column basis.SOLUTION: A column change mechanism 105 includes a ferrule 206, a movable ferrule connector 207, a pipe 208, a fastener pull 209, a fastener fitting 210, a column cartridge presser 211, a slide guide 212, an RFID reader 214, a fixed wall 215, a column changer heat insulating member 216, a fixed bottom plate 217, a receiver 218, and a fixed fitting 219. A plurality of column cartridges 104 can be installed in the heat block 101, and are in contact with the column heat block 103 to control a temperature in the column cartridges 104. The column cartridge 104 is fixed between right and left column change mechanisms 105, and when the fixed column cartridge 104 is opened, the column change mechanism 105 on the left side is moved leftward and opened.SELECTED DRAWING: Figure 1

Description

Technical Field

[0001] The present invention relates to a column oven of an analyzer for analyzing a sample.

Background Art

[0002] Chromatography is an analytical method using an analytical column. An analytical column (simply referred to as a column) is a cylindrical elongated container filled with a packing material of particles to which various functional groups are bonded at a high pressure on a base material such as silica gel or polymer gel.

[0003] Chromatography is a method of separating each substance by utilizing the fact that substances are distributed at a certain ratio due to the difference in the affinity (interaction) between the stationary phase and the mobile phase flowing in contact with it, and the ratio varies depending on the substance.

[0004] Liquid chromatography uses a liquid as the mobile phase. Generally, in order to obtain good peak shapes in liquid chromatography, it is necessary to control the temperature of the column to an optimal temperature. As the temperature of the mobile phase in the column rises, the viscosity of the mobile phase decreases, resulting in a decrease in pressure.

[0005] Therefore, diffusion of the sample in the piping and the column can be suppressed, and by shortening the retention time, it is possible to obtain good peak shapes. Therefore, the column of liquid chromatography is held in a column oven, and temperature control of the column is essential.

[0006] A general method for temperature control of a column is to install a heat source outside the flow path piping through which the mobile phase at the front stage of the column is fed to control the temperature of the mobile phase, and a mechanism for air conditioning the inside of the column oven to control the temperature of the column.

[0007] Patent Document 1 discloses a column module that houses multiple thermally conductive grooves, each located in a separate thermal zone and individually fine-tuned by one individually controlled thermoelectric chip, with each groove holding one or more columns. In Patent Document 1, when multiple columns are located in separate thermal zones and hold multiple columns, the temperature of the multiple columns is controlled by one thermoelectric chip.

[0008] Patent Document 2 discloses a column cartridge in which at least one column and a second column are mounted in a housing, and piping can be connected to each column from the outside. Furthermore, each cartridge is equipped with a recognizable barcode or RFID tag and has a function to manage data such as temperature, fluid pressure, and fluid flow rate inside the cartridge. In Patent Document 2, since at least one column and a second column are mounted in one cartridge, column cartridges are handled for at least two columns. [Prior art documents] [Patent Documents]

[0009] [Patent Document 1] Patent No. 6194310

[0010] [Patent Document 2] WO2012 / 058515 publication [Overview of the Initiative] [Problems that the invention aims to solve]

[0011] In the technology described in Patent Document 1, when multiple columns are temperature-controlled, multiple heat-conducting grooves are temperature-controlled by a single thermoelectric chip within a single heat zone, and the temperature of multiple columns is controlled by a mechanism that air-conditions the column oven. Since multiple columns are temperature-controlled by air conditioning from a single thermoelectric chip, the multiple columns may not reach an average temperature, and temperature differences may occur between columns.

[0012] In the technology described in Patent Document 2, when multiple columns are temperature-controlled, multiple columns are mounted in a housing, and the temperature is controlled within a column cartridge to which each column can be connected from the outside via piping. In this case, if one of the columns in the cartridge degrades in performance or becomes clogged, the entire cartridge must be replaced when that column needs to be replaced, resulting in the waste of discarding columns that are still usable. This goes against the goals of resource conservation and cost reduction. Furthermore, since each cartridge is equipped with a recognizable barcode or RFID tag, it is not possible to manage each column individually.

[0013] The objective of the present invention is to realize a column oven for an analytical instrument that, when multiple columns are mounted in the column oven, enables efficient heat conduction for each column, allows recognition of the column cartridge that holds the columns, and allows easy replacement of each column individually. [Means for solving the problem]

[0014] To achieve the above objective, the present invention is configured as follows.

[0015] A column cartridge for a column oven in an analytical apparatus having an analytical column, a heat source, and a heat block connected to the heat source and to which heat from the heat source is transferred, The aforementioned analytical column, Column heat block that transfers heat to the aforementioned analytical column and, The column heat block is connected to the heat block, and the heat from the heat source is transferred to the analytical column via the heat block and the column heat block. [Effects of the Invention]

[0016] According to the present invention, when multiple columns are mounted in the column oven, it is possible to realize a column oven for an analytical instrument that enables efficient heat conduction for each column, recognizes the column cartridge that holds the column, and allows for easy replacement of each column individually. [Brief explanation of the drawing]

[0017] [Figure 1] It is an explanatory diagram of the structure of the column oven (column temperature control section) 100 in Example 1. [Figure 2] It is an explanatory diagram of the column change mechanism. [Figure 3] It is an explanatory diagram of the column heat block structure. [Figure 4A] It is a schematic perspective view of the upper surface of the column cartridge. [Figure 4B] It is a schematic perspective view of the lower surface of the column cartridge. [Figure 4C] It is a schematic cross-sectional view of the column cartridge. [Figure 5] It is a schematic configuration diagram of the movable ferrule mechanism. [Figure 6A] It is an explanatory diagram of the column replacement operation procedure. [Figure 6B] It is an explanatory diagram of the column replacement operation procedure. [Figure 6C] It is an explanatory diagram of the column replacement operation procedure. [Figure 6D] It is an explanatory diagram of the column replacement operation procedure. [Figure 6E] It is an explanatory diagram of the column replacement operation procedure. [Figure 7] It is a schematic perspective view of the column housing. [Figure 8] It is an explanatory diagram of the column heat block in Example 2. [Figure 9A] It is an explanatory diagram of the column and heat block in Example 1. [Figure 9B] It is an explanatory diagram of the column and heat block in Example 1. [Figure 10A] It is an explanatory diagram of the column and heat block in Example 3. [Figure 10B] It is an explanatory diagram of the column and heat block in Example 3.

Mode for Carrying Out the Invention

[0018] Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.

[0019] Although the embodiments of this invention primarily focus on liquid chromatography (HPLC), the invention is applicable to analytical instruments in general. For example, the invention can also be applied to gas chromatography, ultrahigh-performance liquid chromatography, HPLC / MS, and clinical testing equipment equipped with column separation units.

[0020] A typical HPLC system consists of a liquid delivery pump, an injector, an analytical column, a column oven for temperature control of the analytical column, and piping connecting the liquid delivery pump, injector, and analytical column.

[0021] The overall configuration of the present invention is a multi-HPLC system that allows multiple HPLC channels to be coupled to a single detector via a stream select valve for switching between HPLC channels, enabling mutual analysis. Each HPLC channel has the same configuration and is arranged in parallel. The timing of the analysis column equilibration, elution, and washing processes, as well as the injector washing process, is adjusted to ensure that the target component is always introduced to the detector from each HPLC stream, eliminating detector downtime.

[0022] This invention relates to a column oven capable of holding multiple analytical columns. [Examples]

[0023] (Example 1) Hereinafter, Embodiment 1 of the present invention will be described in detail with reference to Figures 1 to 7.

[0024] Figure 1 is a diagram illustrating the structure of the column oven (column temperature control unit) 100 in Embodiment 1. In Figure 1, the column temperature control unit 100 comprises a heat block 101, a column 102, a column heat block 103, a column cartridge 104, a column change mechanism 105 (having a fixed part 105A and a movable part 105B), a column cartridge insulation material 106, a heat source unit 107, a temperature sensor 108, a thermal protector 109, a control unit 110, a fan 111, and a heat sink 112. The column heat block 103 is positioned in an opening formed in the column cartridge 104 and is in contact with the heat block 101. In other words, the heat block 101 is in contact with the column 102 via the column heat block 103 positioned in an opening formed in the column cartridge 104.

[0025] The heat block 101 has multiple convex structures. In Embodiment 1 of the present invention, aluminum is used as the material of the heat block 101, but copper, iron, stainless steel, and titanium may also be used. Furthermore, the heat block 101 may be a single piece made of the same material, or it may be made by connecting pieces made of different materials.

[0026] Column 102 is a cylindrical, elongated container packed under high pressure with a packing material consisting of particles on which various functional groups are bound to the surface of a base material such as silica gel or polymer gel. Separation is achieved by adsorption and desorption through interaction between the functional groups and the substance to be measured, and elution at a specific retention time. In this Example 1, silica gel was used as the base material, and an ODS column (0.5 mm ID × 50 mm L, particle size 2.6 μL) in reversed-phase chromatography mode was used as the functional group.

[0027] The separation mode of column 102 may be other, such as normal-phase chromatography, HILIC chromatography, ion-exchange chromatography, gel filtration chromatography, affinity chromatography, or immunoaffinity chromatography. It is also adaptable to columns used for gas chromatography.

[0028] The column cartridge 104 is a rectangular parallelepiped with a length of 75 mm, a width of 20 mm, and a height of 34 mm, and is made of PPEX resin. It consists of a column heat block 103 and a column 102. In this embodiment 1, a column 102 with an inner diameter of 0.5 mm and a length of 50 mm was used, but by changing the internal shape of the column cartridge 104, it is possible to accommodate columns with an inner diameter of 0.3-1.0 mm and a length of 10-70 mm.

[0029] Column heat blocks 103 of the same shape can be used.

[0030] The column cartridge 104 has at least one concave notch (opening) that can contact the convex structure of the heat block 101. As a result, the column 102 is temperature-controlled by contact with the column heat block 103. The heat block 101 and the column 102 may be in direct contact. In that case, it is desirable that the contact portion of the convex structure of the heat block 101 has a curved structure so as to increase the contact area with the cylindrical column 102.

[0031] In this embodiment 1, the column cartridge 104 and the column heat block 103 are separated by an insulating material 106 made of EPTSEAL material. The insulating material 106 may also be glass wool or nylon.

[0032] The temperature control of column 102 will now be described. A heater (not shown) as a heat source unit 107 (10W per column, DC24V driven) and a thermistor (not shown) as a temperature sensor 108 are connected to the heat block 101 via the control unit 110. By using a PID control method and feedback control, the temperature of the heat block 101 is changed from 40°C to 70°C, thereby controlling the temperature of column 102 from 40°C to 70°C via the heat block 101 and column heat block 103.

[0033] In this embodiment 1, a heater was used as the heat source 107, but a Peltier element may also be used. In this embodiment 1, a PID method was used for feedback control, but ON / OFF control or PI control may also be used. In this embodiment 1, a thermistor was used as the temperature sensor 108, but a thermocouple or a platinum resistance thermometer may also be used. Similarly, in this embodiment 1, the connection point of the temperature sensor 108 measured the temperature of the heat block 101 and provided feedback, but the heat block 101, column heat block 103, or column 102 may be measured.

[0034] In this case, if multiple columns 102 are mounted in multiple column ovens 100, the control unit 110 becomes complex because it will measure and feed back the temperature of either the protrusion of the heat block 101, the column heat block 103, or the column 102. The temperature accuracy of the column 102 can be controlled to ±1°C. The thermal protector 109 is connected to the heat source unit 107, and when the temperature exceeds the set temperature of 90°C, the heater turns off and temperature control stops.

[0035] When cooling column 102, an 80mm x 80mm, 25mm thick fan 112 connected to the control unit 110 is turned ON, and cooling of the heat block 101 begins. The heat block 101 may be equipped with an aluminum or copper heatsink 112 to improve cooling efficiency.

[0036] The column cartridge 104 is separated from the column heat block 103 by an insulating material 106, so even if the temperature of the column heat block 103 reaches 70°C, the surface temperature of the cartridge 104 will not rise to 70°C.

[0037] As described later, the column change mechanism 105 shown on the left side of Figure 1 is a movable part 105B, which is movable in the left-right direction in Figure 1, and a column cartridge 104 can be fixed between the fixed part 105A and the movable part 105B of the left and right column change mechanisms 105. To release the column cartridge 104 fixed to the column change mechanism 105 from the column change mechanism 105, the left movable part 105B is moved to the left in Figure 1, releasing the fixation by the column change mechanism 105. This allows the column cartridge 104 to be easily released from the column change mechanism 105, and the column cartridge 104 can be easily attached to and removed from the column change mechanism 105. When the column cartridge 104 is attached to the column change mechanism 105, heat is transferred to the column 102 directly from the heat block 101 or via the column heat block 103, and the temperature of the column 102 can be controlled.

[0038] Next, the column change mechanism 105 will be described using Figures 2 and 3. Figures 2 and 3 are explanatory diagrams of the column change mechanism 105. In Figure 2, the column change mechanism 105 includes a ferrule 206, a movable ferrule connector 207, piping 208, a fastener pull tab 209, a fastener fitting 210, a column cartridge holder 211, a slide guide 212, an RFID reader 214, a fixed wall 215, a column changer insulation material 216, a fixed bottom plate 217, a receiving tray 218, and a fixing fitting 219. The piping 208 is supported by the movable connector ferrule 207.

[0039] Furthermore, the fixed base plate 217 supports the ferrule 206, movable ferrule connector 207, piping 208, fastener pull 209, fastener fitting 210, column cartridge holder 211, slide guide 212, RFID reader 214, fixed wall 215, column changer insulation 216, tray 218, and fixing fitting 219.

[0040] Samples are delivered from piping 208 to column 102 via column change mechanism 105. Similarly, samples are delivered from column 102 to piping 208 of column change mechanism 105.

[0041] The heat block 101 is temperature-controlled to a set temperature, and multiple column cartridges 104 can be installed in the heat block 101. The heat block 103 inside the column cartridges 104 comes into contact with the column heat block 103, thereby regulating the temperature inside the column cartridges 104. For example, the case in which five column cartridges 104 are installed in the heat block 101 will be explained using Figure 3.

[0042] In Figure 3, the heat block 101 comprises a base plate 303 and aluminum blocks 302. The base plate 303 and aluminum blocks 302 are made of aluminum, with the base plate 303 measuring 350 mm × 30 mm × 4 mm and the aluminum blocks 302 measuring 20 mm × 14 mm × 10 mm. The aluminum blocks 302 are evenly arranged on the base plate 303 at 50 mm pitch intervals. During temperature control, the aluminum blocks 302 are in contact with the column heat block 104, and the column heat block 104 is in contact with the column 102. The sheet heater 300 is formed in a sheet shape on which multiple column cartridges 104 can be arranged.

[0043] Therefore, heat is transferred from the heat block 101, which is heated by the heat source sheet heater 300 (corresponding to the heat source 107), to multiple columns 102, allowing for temperature control. In this embodiment 1, a sheet heater 300 is used, but of course, a rubber heater, ceramic heater, or cartridge heater may also be used. The aluminum block 302 may also be made of copper or iron. Although not shown in the diagram, a preheating method may also be used in which the piping 208 connected to the column 102 is temperature-controlled by a heat source. In this case, the piping 208 immediately before it is connected to the column 102 is temperature-controlled by a heat source such as a sheet heater to the same temperature as the column, and the HPLC solution delivered to that piping is then delivered. This reduces the temperature difference between the HPLC solution delivered to the column 102 and the column 102, thereby improving the reproducibility of column separation.

[0044] The column cartridge 104 will be explained using Figures 4A, 4B, and 4C. Figure 4A is a top perspective view of the column cartridge 104, Figure 4B is a bottom perspective view of the column cartridge 104, and Figure 4C is a cross-sectional view of the column cartridge 104.

[0045] In Figures 4A, 4B, and 4C, the column cartridge 104 comprises an upper column cartridge 401, a lower column cartridge 402, a column 102, a column cartridge insulation material 106 for insulating the column, a column heat block 103, and a screw 406.

[0046] The upper column cartridge 401 is a rectangular prism made of PEEK resin with a length of 75 mm, a width of 20 mm, and a height of 10 mm. The lower column cartridge 402 is also a rectangular prism made of PEEK resin with a length of 75 mm, a width of 20 mm, and a height of 24 mm. Both are made of PEEK to suppress the rise in surface temperature of column 102 and to ensure user safety, such as preventing burns during column replacement. The upper column cartridge 401 and the lower column cartridge 402 are fixed together with screws 406 so as to sandwich column 102 from above and below.

[0047] Of course, the column cartridge 104 can be made of PPS resin, which has heat-insulating properties. The upper part 401 and lower part 402 of the column cartridge are structured to hold down the column 102 from above and below, but a structure that holds it down from the left and right is also acceptable.

[0048] The column cartridge insulation material 106 is made of EPT sealer and is positioned to cover the column that is not in contact with the column heat block 103, preventing heat dissipation. The material of the cartridge insulation material 106 may also be glass wool or nylon. The column 102, sandwiched between the upper part 401 and the lower part 402 of the column cartridge, is positioned at least 5 mm inward from the connection part of the column cartridge 104 at both ends. This structure takes into consideration the safety of the user during column replacement, such as preventing burns, and prevents the user from coming into contact with the tip of the column 102, which may be a hot part.

[0049] As shown in Figure 4C, the column heat block 103 has a cylindrical recess at the top to accommodate the cylindrical column 102, and a rectangular parallelepiped protruding from the center of the bottom surface at the bottom so as to contact the heat block (aluminum block) 302. The heating surfaces of this rectangular parallelepiped and the heat block (aluminum block) 302 may be connected on a flat surface, but to improve heat conduction efficiency, a stepped structure may be provided to increase the surface area of ​​the heating surface. Furthermore, the structure of the heating surface does not have to be a rectangular parallelepiped; it may be cylindrical or coiled.

[0050] As shown in Figure 4B, the bottom surface of the column cartridge lower section 402 has an opening where the column heat block 103 is placed, and the structure surrounds the column heat block 103. The bottom surface of the column cartridge lower section 402 (top surface in Figure 4B) is at least 12 mm longer in the downward direction (upward in Figure 4B) than the bottom surface of the column heat block 103 (top surface in Figure 4B). In other words, the surface of the column heat block 103 opposite to the surface that contacts the column 102 is at least 12 mm smaller than the bottom surface of the column cartridge lower section 402. To put it another way, the bottom surface of the column cartridge lower section 402 protrudes at least 12 mm beyond the bottom surface of the column heat block 103.

[0051] To ensure user safety during column replacement, the column heat block 103 is designed to prevent users from coming into contact with the bottom surface, which may be a high-temperature area.

[0052] The bottom of the column cartridge 402 has a notch on one side and no notch on the other, allowing it to be fitted in only one direction onto the heat block (aluminum base) 302, which is accessible from the upper space of the fixed bottom plate 217 of the column change mechanism 105. This ensures that when changing the column, the column cartridge 104 can only be installed in one direction, allowing the column 102 to be installed in the correct inlet (IN) and outlet (OUT) directions.

[0053] The fixed base plate 217 has a slide guide 212 (shown in Figure 2), which allows the column cartridge 104 to be installed and slid when replacing the column 102. Furthermore, depending on the type of column 102, a structure is provided for each type of column cartridge with a different length relative to the width of the bottom of the column cartridge lower part 402, ensuring that the correct column 102 is installed.

[0054] In addition to having a specific structure for the length relative to the width of the joint between the lower part 402 of the column cartridge and the slide guide 212, the structure of the joint may also be provided with circular or elliptical structures for each type of column 102, so that the type of column 102 can be identified by fitting.

[0055] The heat block (aluminum block) 302 is positioned at least 12 mm below the top surface of the fixed base 217. This design ensures user safety during column replacement, preventing burns and other injuries, by preventing the user from coming into contact with the bottom surface of the column heat block 103, which may be a high-temperature area.

[0056] An RFID tag 411 is attached to the side of the column cartridge 104, and when the column is replaced, it is read by the RFID reader 214 to confirm the status of the column 102, such as the type and serial number. The control unit (control PC) 110 counts the number of uses and notifies the user of the column replacement time via the display unit of the control unit 110. When column 102 is replaced, a record that it has been used is written to the replacement column 102 to prevent reuse.

[0057] Next, the movable ferrule connector 207 will be explained using Figure 5. Figure 5 shows the state when the movable ferrule connector 207 is pressed most firmly against the column cartridge 104.

[0058] In Figure 5, the movable ferrule connector 207 comprises a ferrule 206, a movable connector housing 502, a pipe retainer 503, an inner member 504, an outer member 505, a retaining ring 506, a leaf spring 507, a spring washer 508, a stopper 509, and a pipe 208. The movable ferrule connector housing 502 is cylindrical, and its interior has four cylindrical spaces with different inner diameters from the central axis. The pipe 208 is placed in the cylindrical space with the smallest inner diameter inside the movable ferrule connector housing 502 and is held in place by the pipe retainer 503.

[0059] A leaf spring 507 is positioned in the second smallest cylindrical space inside the movable ferrule connector housing 502, which is compressed when the column 102 is fixed, creating a pressing force. A spring washer 508 is positioned in the third smallest cylindrical space inside the movable ferrule connector housing 502, and an inner member 504 is positioned to contact the spring washer 508 and press against the pipe retainer 503. An outer member 505 is positioned to press against the inner member 504. A stopper 509 is positioned in the largest cylindrical space inside the movable ferrule connector housing 502, and when the column 102 is fixed and pushed in the most compressed state, the outer member 505 contacts the stopper 509, stopping the movement of the outer member 505, thus preventing the individual components from being pushed in beyond their specified positions and becoming damaged.

[0060] A retaining ring 506 is positioned on the column 102 side of the cylindrical space with the largest inner diameter inside the movable ferrule connector housing 502. When the column 102 is replaced and not pushed in, the outer member 505 comes into contact with the retaining ring 506, stopping the movement of the outer member 505 and preventing it from popping out of the movable ferrule connector housing 502.

[0061] A ferrule 206 is positioned at the tip of the outer member 505. Spaces are provided in the center of the pipe retainer 503, inner member 504, and outer member 505 for the pipe 208 to pass through, and the pipe 208 is fixed in place by being tightened by the pipe retainer 503. The ferrule 206 is also fixed to the pipe 208 by being tightened, and the amount of protrusion of the pipe 208 from the ferrule 206 is also determined.

[0062] The connection portion of column 102 has a tapered structure, and when column 102 is fixed, the tip of the pipe 208 and the tip of the tapered structure, as well as the ferrule 206 and the tapered structure, are in close contact to create a seal. A movable ferrule connector 207 is provided symmetrically on the outlet (OUT) side of column 102, and the movable connector housing 502 on this side is fixed to the fixed wall 215 using a fixing bracket 219 (see Figure 2). The fixed wall 215 is connected to the fixed bottom plate 217, and below the fixed bottom plate 217, column changer insulation material 216 is positioned to separate the heat block 101 from the fixed bottom plate 217, creating a structure that makes it difficult for heat from the heat block 101 to be transferred to the fixed bottom plate 217, the fixed wall 215, and the movable ferrule connector 207.

[0063] The procedure for changing a column using the column change mechanism 105 will be explained using Figures 6A, 6B, 6C, 6D, and 6E.

[0064] The installation method for column cartridge 204 consists of the following steps: 1) initial state (Figure 6A), 2) installation process of column cartridge 104 (Figure 6B), 3) pressing process of column cartridge 104 (Figure 6C), 4) fastener hooking process (Figure 6D), and 5) fixing process (Figure 6E).

[0065] As shown in Figure 6A, 1) In the initial state, the column cartridge 104 is not installed in the column change mechanism 105. 2) In the column cartridge 104 installation process, the column cartridge 104 is fitted into the heat block 101, which is accessible from the space above the fixed bottom plate 217, from one direction.

[0066] Next, in step 3) pressing the column cartridge 104, the operator rotates the fixing lever 220 of the fastener pull handle 209 of the movable part 105B to release the fastener pull handle 209, while moving the movable part 105B from left to right in Figure 6C along the slide guide 212 provided on the fixed base plate 217, thereby moving the column cartridge 104 to the right and pressing it against the fixed part 105A on the right side. By converting the rotational motion of the fixing lever 220 of the fastener pull handle 209 into a balanced motion, the movable ferrule connector 207 and the column cartridge 104 are pressed against the fixed part 105A on the right side.

[0067] 4) In the fastener hooking process, the fastener pull tab 209 of the movable part 105B on the left side is rotated and hooked onto the fastener fitting 210 of the fixed part 105A on the right side. 3) The column cartridge 104 pressing process and 4) the fastener hooking process can be performed as a series of operations.

[0068] Next, in step 5) fixing, the column 104 is fixed to the column change mechanism 105 by pressing the fixing lever 220 to fix the fastener pull handle 209. The column change mechanism 105 can maintain pressure resistance even when the mobile phase is supplied to the piping 208 at a high flow rate due to the sealing method of the movable ferrule connector 207.

[0069] Column 102 can be removed by performing the steps described above—1) initial state, 2) installation of column cartridge 104, 3) pressing of column cartridge 104, 4) fastening, and 5) fixing—in reverse order.

[0070] In other words, rotate the fixing lever 220 to the right in Figure 6E to release the fastener pull tab 209, detach the fastener pull tab 209 from the fastener fitting 210, rotate it to the left in Figure 6D to return it to the left movable part 105B, and bring it to the state shown in Figure 6C. Then, slide (move) the left movable part 105B to the left in Figure 6C (the direction of separation) so that it separates from the column cartridge 104, thereby releasing the column cartridge 104 that was fixed to the left and right fixing parts 105A and movable part 105B. This allows the released column cartridge 104 to be easily removed.

[0071] In this embodiment 1, when the liquid is delivered at 250 μL / min, a pressure of approximately 100 MPa is applied to the column 102. However, the mechanism maintains pressure resistance without leakage of the mobile phase from the connection between the movable ferrule connector 207 and the column 102.

[0072] The safety mechanism of the column oven 100 will be explained using Figure 7.

[0073] In Figure 7, the column oven enclosure 701 is equipped with a column change mechanism 105, and a column oven cover 702 is installed to maintain temperature control inside the column oven chamber. A handle 703 is installed on the outer wall of the column oven cover 702, allowing it to be opened and closed from front to back. The column oven chamber is equipped with an interlock mechanism 705 with a built-in temperature sensor, which prevents the column oven cover 702 from being opened or closed when the temperature is above the set temperature of 40°C. Whether the cover can be opened or closed can be visually confirmed by the illumination of an LED 704 on the outer wall of the column oven cover 702.

[0074] Thus, with the column oven 100 of Embodiment 1 of the present invention, even when multiple columns 102 are installed in the column oven 100, efficient heat conduction is possible for each column 102, and by incorporating a mechanism that can recognize each column cartridge 104, the set temperature and time can be managed for each column 102.

[0075] In other words, when multiple columns 102 are mounted in the column oven 100, it is possible to realize a column oven for an analytical instrument that allows for efficient heat conduction for each column 102, recognizes the column cartridge 104 that holds the columns 102, and has a mechanism that allows for easy replacement of each column 102.

[0076] (Example 2) Next, Example 2 of the present invention will be described.

[0077] In Example 2, as shown in Figure 8, a sheet heater 800, which is a heat source, is configured for each column 102. The difference between Example 1 and Example 2 is that in Example 1, as shown in Figure 3, a sheet heater 300, which is a heating element, is provided on the base plate 303, allowing for simultaneous temperature control of multiple columns 102, while in Example 2, multiple sheet heaters 800 are provided, each of which is positioned on a column 102.

[0078] The other configurations are the same as those in Example 1 and Example 2.

[0079] In Example 2, similar to Example 1, the heat block 101 is in contact with the column heat block 103 during temperature control, and the column heat block 103 is in contact with the column 102. Therefore, heat is transferred from the heat block 101, which is heated by the heat source, the sheet heater 800, to the column 102, allowing for temperature control.

[0080] In Embodiment 2 of the present invention, temperature control is performed by heat transfer rather than by air conditioning, making it possible to set different temperatures for each column 102.

[0081] In this embodiment 2, the temperature sensor can be connected to the heat block 101, and the temperature of the heat block 101 can be measured and fed back. However, the temperature sensor may also be positioned to measure the temperature of the heat block 101, the column heat block 103, or the column 102. The temperature accuracy of the column 102 can be controlled to ±1°C.

[0082] According to Example 2, in addition to obtaining the same effects as in Example 1, there is the effect that each of the multiple columns 102 can be set to an optimal temperature according to each individual column 102.

[0083] In Examples 1 and 2, as shown in Figure 9A and Figure 9B which shows a cross-section along the line A-A' in Figure 9A, the cylindrical column 102 is in contact with the curved surface of the column heat block 103, which has a curved groove on its upper surface that is approximately the same diameter as the column 102, and the column 102 is heated by heat conduction.

[0084] However, the contact surface between column 102 and column heat block 103 can have a shape other than that described above.

[0085] (Example 3) Next, Example 3 will be described. Example 3 is an example in which the shape of the contact surface between the column 102 and the column heat block 103 is different from the shape shown in Figures 9A and 9B in Examples 1 and 2 described above. The other configurations of Example 3 are the same as those of Example 1 or Example 2.

[0086] Figures 10A and 10B show the column 1001 and column heat block 1002 in Example 3. Figure 10B is a cross-sectional view along the line B-B' in Figure 10A.

[0087] As shown in Figures 10A and 10B, the bottom 1001d of column 1001 is processed to be flat, and is brought into planar contact with the connection portion 1002u of column heat block 1002, which has a flat connection portion 1002u on its upper surface.

[0088] Since the column bottom 1001d and connection portion 1002u are flat, it is possible to achieve high machining accuracy, which reduces heat transfer contact resistance and has the effect of efficiently heating the column 1001.

[0089] The heat block 101, the column heat block 103, and the heat source unit 107 can each be collectively referred to as a heat source. [Explanation of symbols]

[0090] 100: Column oven (column temperature control unit), 101: Heat block, 102: Column, 103: Column heat block, 104: Column cartridge, 105: Column change mechanism, 105A: Fixed part, 105B: Movable part, 106: Column cartridge insulation material, 107: Heat source unit, 108: Temperature sensor, 109: Thermal protector, 110: Control unit, 111: Fan, 112 : Heat sink, 206: Ferrule, 207: Movable ferrule connector, 208: Piping, 209: Fastener pull, 210: Fastener fitting, 211: Column cartridge holder, 212: Slide guide, 214: RFID reader, 215: Fixed wall, 216: Column changer insulation, 217: Fixed base plate, 218: Tray, 219: Fixing fitting, 220: Fixing lever, 300, 800: Sheet heater, 302: Aluminum block, 303: Base plate, 401: Column cartridge top, 402: Column cartridge bottom, 406: Screw, 411: RFID tag, 502: Movable connector housing, 503: Pipe retainer, 504: Inner component, 505: Outer component, 506: Retaining ring, 507: Leaf spring, 508: Spring washer, 509: Stopper, 701: Column oven housing, 702: Column oven cover, 703: Handle, 704: LED, 705: Interlock mechanism, 1001: Column, 1001d: Column bottom, 1002: Column heat block, 1002u: Connection part

Claims

1. A column cartridge for a column oven in an analytical apparatus having an analytical column, a heat source, and a heat block connected to the heat source and to which heat from the heat source is transferred, The aforementioned analytical column, The analysis column is provided with a column heat block that transmits heat to the analysis column, The column cartridge is characterized in that the column heat block is connected to the heat block, and the heat from the heat source is transferred to the analytical column via the heat block and the column heat block.

2. In the column cartridge according to claim 1, A column cartridge characterized by having an opening in which the column heat block is arranged.

3. In the column cartridge according to claim 2, A column cartridge characterized in that the opening is located on the bottom surface of the lower part of the column cartridge.

4. In the column cartridge according to claim 2, A column cartridge characterized in that the surface having the opening protrudes outward from the surface of the column heat block.

5. In the column cartridge according to claim 1, A column cartridge characterized in that it has a notch on one side of the bottom surface of the lower part of the column cartridge, and the other side does not have a notch.

6. In the column cartridge according to claim 1, A column cartridge characterized by having an electronic tag for storing information about the aforementioned analytical column.

7. In the column cartridge according to claim 6, A column cartridge characterized in that a record of use is written to the electronic tag when the analytical column is replaced.

8. In the column cartridge according to claim 1, A column cartridge characterized in that the heat source is a sheet heater.

9. In the column cartridge according to claim 1, The aforementioned analytical column is cylindrical, A column cartridge characterized in that the contact portion between the column heat block and the analytical column has a curved groove with substantially the same diameter as the analytical column.

10. In the column cartridge according to claim 1, A column cartridge characterized in that the contact portion between the analytical column and the column heat block is planar.

11. In the column cartridge according to claim 1, The column cartridge is characterized in that the analytical column is covered with an insulating material except for both ends of the analytical column and the portion in contact with the column heat block.

12. In the column cartridge according to claim 11, The column cartridge is characterized in that the column heat block is covered with the insulating material except for the portion that is in contact with the analytical column and the portion that is in contact with the heat block.

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