阅读说明：本技术 超临界流体装置用流动相调温装置及超临界流体装置 (Mobile phase temperature adjusting device for supercritical fluid device and supercritical fluid device ) 是由 高良智寻 于 2019-06-11 设计创作，主要内容包括：超临界流体装置用流动相调温装置是在包括分离柱的超临界流体装置中使用,且包括筒式加热器、流路部、以及第一温度传感器。筒式加热器具有棒状。流路部卷绕于筒式加热器,且利用流路部将流动相导向超临界流体装置的分离柱。流动相至少在分离柱中成为超临界状态。第一温度传感器安装于流路部,且利用第一温度传感器检测流路部的温度。(The mobile phase temperature control device for a supercritical fluid device is used in a supercritical fluid device including a separation column, and includes a cartridge heater, a flow path section, and a first temperature sensor. The cartridge heater has a rod shape. The flow path section is wound around the cartridge heater, and the mobile phase is guided to the separation column of the supercritical fluid device by the flow path section. The mobile phase becomes supercritical at least in the separation column. The first temperature sensor is attached to the flow path section, and detects the temperature of the flow path section by the first temperature sensor.)

1. A mobile phase temperature control device for a supercritical fluid device, which is used in a supercritical fluid device including a separation column to which a mobile phase in a supercritical state is supplied, characterized by comprising:

a rod-shaped cartridge heater;

a flow path section wound around the cartridge heater and guiding the mobile phase to the separation column; and

and a first temperature sensor that is attached to the flow path section and detects the temperature of the flow path section.

2. The mobile phase temperature regulating device for supercritical fluid apparatus according to claim 1, wherein the cartridge heater has an outer shape of a cylindrical shape.

3. The mobile phase temperature adjustment device for supercritical fluid devices according to claim 1 or 2, wherein the flow path section includes an upstream end portion and a downstream end portion that are in contact with the cartridge heater, and wherein

The first temperature sensor is attached to the flow path portion at a position closer to the downstream end portion than the upstream end portion.

4. The mobile phase temperature adjusting apparatus for supercritical fluid apparatus according to claim 1 or 2, characterized in that the cartridge heater is provided in plurality,

a plurality of cartridge heaters are arranged in parallel,

the flow path portion is wound around the plurality of cartridge heaters.

5. The mobile phase attemperating device for supercritical fluid apparatus according to claim 4, wherein the plurality of cartridge heaters are electrically connected in series.

6. The mobile phase temperature adjustment apparatus for supercritical fluid apparatus according to claim 4, wherein the first temperature sensor is installed at a position closer to the cartridge heater disposed most downstream than the cartridge heater disposed most upstream among the plurality of cartridge heaters.

7. The mobile phase temperature control device for a supercritical fluid device according to claim 1 or 2, further comprising a second temperature sensor that is attached to the flow path section and detects the temperature of the flow path section, further upstream from the first temperature sensor.

8. A supercritical fluid apparatus, comprising:

a separation column;

a first supply unit configured to supply a first mobile phase that is in a supercritical state at least in the separation column;

a second supply unit for supplying a second mobile phase used as a modifier;

a mixing section that mixes the first mobile phase supplied from the first supply section with the second mobile phase supplied from the second supply section and guides the mixed phase to the separation column; and

mobile phase tempering device for supercritical fluid apparatus according to claim 1 or 2, arranged to adjust the temperature of at least one of said first mobile phase and said second mobile phase.

9. A supercritical fluid apparatus, comprising:

a separation column;

a mobile phase supply unit for supplying a mobile phase;

the mobile phase temperature adjustment device for a supercritical fluid device according to claim 7, wherein the temperature of the mobile phase supplied from the mobile phase supply unit is adjusted and guided to the separation column; and

a control unit for controlling the operation of the mobile phase temperature adjusting device for the supercritical fluid device,

the control section includes:

a determination unit that determines whether or not the mobile phase flows through the flow path unit based on detection results obtained by the first temperature sensor and the second temperature sensor of the mobile phase temperature adjustment device for a supercritical fluid device;

a first operation control unit that controls operation of the cartridge heater so that a temperature of the mobile phase becomes a preset temperature when the determination unit determines that the mobile phase flows through the flow path unit; and

and a second operation control unit that controls operation of the cartridge heater so that on/off of the cartridge heater is regularly repeated when the determination unit determines that the mobile phase does not flow in the flow path unit.

Technical Field

The invention relates to a mobile phase temperature adjusting device for a supercritical fluid device and the supercritical fluid device.

Background

In a Supercritical Fluid apparatus such as a Supercritical Fluid Chromatograph (SFC) or a Supercritical Fluid extraction apparatus (Supercritical Fluid Extractor (SFE)), a sample is analyzed or collected using a Supercritical Fluid as a mobile phase. For example, in the SFC described in patent document 1, liquefied carbon dioxide is supplied as a mobile phase to a mobile phase flow path by a liquid-feeding pump. Further, the sample is injected into the mobile phase channel by the sample injection section.

The mobile phase and the sample pass through a separation column disposed in the mobile phase flow path. Here, the pressure in the mobile phase flow path is maintained by a back pressure valve and the temperature of the separation column is maintained by a column oven so that the mobile phase becomes at least in a supercritical state in the separation column. The sample is separated for each sample component by passing through the separation column, and is detected by a detector.

Patent document 1: japanese patent laid-open publication No. 2016-173343

Disclosure of Invention

[ problems to be solved by the invention ]

In the supercritical fluid apparatus, since the mobile phase is cooled to a low temperature and a large amount of the mobile phase is supplied to the column, a temperature gradient is likely to occur in the mobile phase in the separation column due to the influence of the temperature of the surrounding environment or the like. Here, when a temperature gradient occurs in the mobile phase, the accuracy of separation of the sample by the separation column and the accuracy of detection by the detector are degraded. In particular, in SFE, since a mobile phase of a larger capacity is used, the problem becomes remarkable. Therefore, it is desirable to suppress the occurrence of a temperature gradient in the mobile phase in the separation column.

The purpose of the present invention is to provide a mobile phase temperature adjustment device for a supercritical fluid device and a supercritical fluid device, which can suppress the occurrence of a temperature gradient in a mobile phase in a separation column.

[ means for solving problems ]

An aspect according to an aspect of the present invention relates to a mobile phase temperature adjustment device for a supercritical fluid device, which is used in a supercritical fluid device including a separation column to which a mobile phase in a supercritical state is supplied, the mobile phase temperature adjustment device for a supercritical fluid device including: a rod-shaped cartridge heater; a flow path section wound around the cartridge heater and guiding the mobile phase to the separation column; and a first temperature sensor that is attached to the flow path section and detects the temperature of the flow path section.

[ Effect of the invention ]

According to the present invention, the occurrence of a temperature gradient in the mobile phase in the separation column can be suppressed.

Drawings

Fig. 1 is a diagram showing a structure of a supercritical fluid apparatus according to an embodiment of the present invention.

Fig. 2 is a diagram showing the structure of the mobile phase temperature control device of fig. 1.

Fig. 3 is a sectional view taken along line a-a of the mobile phase temperature adjusting device of fig. 2.

Fig. 4 is a block diagram showing a configuration of the control unit of fig. 1.

Detailed Description

(1) Structure of supercritical fluid device

Hereinafter, a mobile phase temperature control device for a supercritical fluid device (hereinafter, simply referred to as a mobile phase temperature control device) and a supercritical fluid device according to an embodiment of the present invention will be described in detail with reference to the drawings. Fig. 1 is a diagram showing a structure of a supercritical fluid apparatus according to an embodiment of the present invention. As shown in fig. 1, the supercritical fluid apparatus 100 is a Supercritical Fluid Chromatograph (SFC) including: a mobile phase temperature control device 10, a mobile phase supply unit 20, a sample supply unit 30, a separation column 40, a detector 50, a back pressure valve 60, and a control unit 70. In the following description, the direction in which the mobile phase flows is defined as the downstream direction, and the opposite direction is defined as the upstream direction.

The mobile phase supply section 20 includes: two bottles 21, 22, two supply parts 23, a supply part 24, and a mixing part 25. In bottle 21, liquefied carbon dioxide, cooled, for example, to about 5 ℃, is stored as a mobile phase. In the bottle 22, a modifier (modifier) such as an organic solvent is stored as a mobile phase. The supply units 23 and 24 are, for example, liquid-feeding pumps, and pressure-feed the mobile phases stored in the bottles 21 and 22, respectively. The supply unit 23 and the supply unit 24 are examples of a first supply unit and a second supply unit, respectively. The mixing section 25 is, for example, a gradient mixer (gradient mixer), and supplies the mobile phase pumped by the supply section 23 and the supply section 24 while mixing the mobile phase at a predetermined ratio.

The mobile phase temperature control device 10 is provided in the flow path of the liquefied carbon dioxide upstream of the separation column 40. In the present embodiment, the mobile phase temperature control device 10 is provided between the supply unit 23 and the mixing unit 25. The mobile phase temperature control apparatus 10 preheats the liquefied carbon dioxide pumped by the supply unit 23 to a temperature equal to or higher than the critical temperature (about 40 ℃ in this example) so that the liquefied carbon dioxide in the mobile phase supplied by the mobile phase supply unit 20 is in a supercritical state at least in the separation column 40. The details of the mobile phase temperature control apparatus 10 will be described later.

The sample supply unit 30 is, for example, an ejector (injector), and introduces a sample to be analyzed and the mobile phase supplied from the mobile phase supply unit 20 into the separation column 40. The separation column 40 is housed in a column thermostat, not shown, and is heated to a predetermined temperature (about 40 ℃ in the present example) so that the liquefied carbon dioxide in the introduced mobile phase is in a supercritical state. The separation column 40 separates the introduced sample into components according to the difference in chemical properties or composition.

The detector 50 is, for example, an absorbance detector, and detects components of the sample separated by the separation column 40. The detection result obtained by the detector 50 is used to generate, for example, a supercritical fluid chromatogram showing the relationship between the retention time and the detection intensity of each component. The back pressure valve 60 maintains the pressure in the flow path of the mobile phase at a pressure equal to or higher than the critical pressure of carbon dioxide (for example, 8MPa) so that the liquefied carbon dioxide in the mobile phase is in a supercritical state at least in the separation column 40.

The control Unit 70 includes a Central Processing Unit (CPU), a memory, a microcomputer, and the like, and controls the operations of the mobile phase temperature control device 10, the mobile phase supply Unit 20, the sample supply Unit 30, the separation column 40 (column thermostat), the detector 50, and the back pressure valve 60. In the case where a separation device such as a fraction collector (fraction collector) is provided downstream of the back pressure valve 60, the control unit 70 controls the operation of the separation device based on the detection result obtained by the detector 50. The control unit 70 may be provided in the back pressure valve 60.

(2) Structure of mobile phase temperature adjusting device

Fig. 2 is a diagram showing the structure of the mobile phase temperature control device 10 in fig. 1. Fig. 3 is a sectional view taken along line a-a of the mobile phase temperature conditioning device 10 of fig. 2. In the following description, the horizontal direction of the paper surface in fig. 2 and 3 is referred to as the width direction, the vertical direction of the paper surface in fig. 2 is referred to as the longitudinal direction, and the vertical direction of the paper surface in fig. 3 is referred to as the height direction. The width direction, the length direction and the height direction are orthogonal to each other.

As shown in fig. 2 and 3, the mobile phase temperature control device 10 includes: the cartridge heater includes a plurality of cartridge heaters 1, a flow path section 2, a metal plate 3, a metal plate 4, a fixing member 5, a first temperature sensor 6, a second temperature sensor 7, and a plurality of third temperature sensors 8. The mobile phase temperature control device 10 further includes a drive unit 9 (see fig. 9 described later) for driving the plurality of cartridge heaters 1. The driving unit 9 is, for example, a 24V power supply.

Each cartridge heater 1 has a structure in which a coil-shaped heating element is covered with a cylindrical metal body. Therefore, each cartridge heater 1 has a rod shape (in this example, a cylindrical shape having an outer diameter of 10mm and a length of 45 mm) extending in one direction. In this example, four cartridge heaters 1 generating heat of 100W are connected in series. Therefore, the heat generation amount of the entire four cartridge heaters 1 is 400W. The four cartridge heaters 1 are arranged to extend in the longitudinal direction and to be arranged at substantially equal intervals in the width direction.

The flow path section 2 is, for example, a pipe, and is provided so as to connect between the supply section 23 and the mixing section 25 in fig. 1 and wind around the four cartridge heaters 1. Specifically, the flow path section 2 is formed in a coil shape having an inner diameter (for example, 9.5mm) slightly smaller than the outer diameter of each cartridge heater 1 at four portions. The four cartridge heaters 1 are respectively fitted into the four coil-shaped portions of the flow path portion 2, and the flow path portion 2 is wound around the four cartridge heaters 1.

The state in which the liquefied carbon dioxide flows through the flow path unit 2 is referred to as a liquid passing state, and the state in which the liquefied carbon dioxide does not flow through the flow path unit 2 is referred to as a liquid non-passing state. According to the method of mounting the flow path portion 2, since the inner peripheral surface of the flow path portion 2 and the cylindrical outer peripheral surfaces of the plurality of cartridge heaters 1 are brought into close contact with each other, the thermal contact resistance (heat loss) between the flow path portion 2 and the plurality of cartridge heaters 1 is reduced. Therefore, in the liquid passing state, the liquefied carbon dioxide pressure-fed from the supply unit 23 is preheated with high responsiveness and high efficiency by the four cartridge heaters 1, and is guided to the mixing unit 25.

The metal plate 3 has a flat plate shape. The metal plate 4 has a cross-sectional concave shape (see fig. 3). The metal plate 3 and the metal plate 4 are fixed by a plurality of (five in this example) screw members 11 in a state of sandwiching the four cartridge heaters 1 around which the flow path section 2 is wound. Specifically, five screw members 11 are inserted into five openings of the metal plate 3 between two adjacent cartridge heaters 1 in the width direction and at both ends in the width direction. In this state, the front ends of the five screw members 11 are screwed to the five screw holes of the metal plate 4, respectively. Thereby, the four cartridge heaters 1 are integrated.

The fixing member 5 has a cross-sectional concave shape (see fig. 3). One end surface and the other end surface of the metal plate 4 in the width direction are attached to one end surface and the other end surface of the fixing member 5 in the width direction, respectively, by two screw members 12, for example. Thus, the mobile phase temperature control device 10 can be made into a relatively small heater module. In this example, the dimensions of the mobile phase temperature adjustment device 10 in the width direction, the length direction, and the height direction are about 130mm, about 100mm, and about 60mm, respectively. The integrated four cartridge heaters 1 can be fixed to a desired portion of the supercritical fluid apparatus 100 by mounting the fixing member 5 to the portion.

The first temperature sensor 6 and the second temperature sensor 7 each include, for example, a thermistor (thermistor). The first temperature sensor 6 is attached to a downstream portion of the flow path section 2, and detects the temperature of the downstream portion of the flow path section. The second temperature sensor 7 is attached to an upstream portion of the flow path section 2, and detects a temperature of the upstream portion of the flow path section.

In this example, the first temperature sensor 6 is attached to a portion of the flow path section 2 drawn from the cartridge heater 1 disposed furthest downstream among the four cartridge heaters 1. The second temperature sensor 7 is attached to a portion of the flow path section 2 wound around the cartridge heater 1 arranged at the most upstream of the four cartridge heaters 1. In fig. 2, a part of the metal plate 3 is shown in a state of being virtually notched in order to facilitate the visibility of the second temperature sensor 7.

Since the first temperature sensor 6 and the second temperature sensor 7 are directly attached to the surface of the flow path unit 2, respectively, the temperature of the liquefied carbon dioxide flowing through the flow path unit 2 can be accurately detected as the temperature of the flow path unit 2. The first temperature sensor 6 and the second temperature sensor 7 can be fixed to the flow path portion 2 by an electrically conductive tape or an electrically conductive adhesive having high thermal conductivity. In this case, the temperature of the flow path section 2 can be detected with higher accuracy.

The plurality of third temperature sensors 8 each include, for example, a tag terminal thermistor. In this example, five third temperature sensors 8 are fixed to the metal plate 3 by the five screw members 11 so that the temperatures of the four cartridge heaters 1 can be detected through the metal plate 3. Therefore, the four cartridge heaters 1 are located between each two third temperature sensors 8 adjacent in the width direction. Since each of the third temperature sensors 8 detects the temperature of one of the cartridge heaters 1 via the metal plate 3, the metal plate 3 is preferably formed of a member having high thermal conductivity (for example, a metal containing aluminum).

(3) Structure of control part

Fig. 4 is a block diagram showing the configuration of the control unit 70 of fig. 1. As shown in fig. 4, the control unit 70 includes: a first temperature acquisition unit 71, a second temperature acquisition unit 72, a third temperature acquisition unit 73, a liquid passage determination unit 74, an abnormality determination unit 75, a first operation control unit 76, a second operation control unit 77, and an output unit 78. The CPU of the control unit 70 implements a functional unit of the control unit 70 by executing a predetermined application program (application program) stored in the memory. A part or all of the functional units of the control unit 70 may be realized by hardware such as an electronic circuit.

The first temperature acquisition unit 71 acquires the temperature of the downstream portion of the flow path unit 2 detected by the first temperature sensor 6. The second temperature acquisition unit 72 acquires the temperature of the upstream portion of the flow path unit 2 detected by the second temperature sensor 7. The third temperature acquisition unit 73 acquires the temperatures of the plurality of portions of the flow path unit 2 detected by the plurality of third temperature sensors 8.

The liquid passage determination unit 74 is an example of a determination unit that determines whether or not the flow path unit 2 is in the liquid passage state based on the temperatures acquired by the first temperature acquisition unit 71 and the second temperature acquisition unit 72. Specifically, in the liquid passing state, the temperature of the downstream portion of the flow path section 2 is equal to or higher than the temperature of the upstream portion. In the non-liquid passing state, the temperature of the downstream portion of the flow path section 2 is lower than that of the upstream portion. Therefore, when the temperature detected by the first temperature acquisition unit 71 is equal to or higher than the temperature detected by the second temperature acquisition unit 72, it is determined that the flow path unit 2 is in the liquid-passing state. When the temperature detected by the first temperature acquisition unit 71 is lower than the temperature detected by the second temperature acquisition unit 72, it is determined that the flow path unit 2 is in the non-liquid-passing state.

The abnormality determination unit 75 determines whether or not the plurality of cartridge heaters 1 are operating normally based on the temperatures at the plurality of locations acquired by the third temperature acquisition unit 73. When the temperatures at the plurality of locations acquired by the third temperature acquiring unit 73 are substantially the same, it is determined that the plurality of cartridge heaters 1 are operating normally. When some of the temperatures acquired by the third temperature acquiring unit 73 are extremely different from the other temperatures, it is determined that the operation of one of the cartridge heaters 1 is abnormal, without determining that the plurality of cartridge heaters 1 are operating normally.

When the liquid passage determination unit 74 determines that the flow path unit 2 is in the liquid passage state, the first operation control unit 76 controls the operation of the drive unit 9 so that the temperature acquired by the first temperature acquisition unit 71 becomes a predetermined value (for example, about 40 ℃). In this case, the operation of the driving unit 9 is precisely controlled, and the driving unit 9 supplies an appropriate driving voltage to the plurality of cartridge heaters 1 so that the temperature of the liquefied carbon dioxide flowing through the flow path unit 2 becomes a predetermined value.

When the liquid passage determination unit 74 determines that the flow path unit 2 is in the emergency liquid passage state, the second operation control unit 77 controls the operation of the drive unit 9 so as to regularly repeat the on and off states of the plurality of cartridge heaters 1. In this case, the temperature of the flow path section 2 during standby can be maintained within a predetermined range by simple control.

When the abnormality determination unit 75 determines that a certain cartridge heater 1 is operating abnormally, the output unit 78 controls the drive unit 9 to stop the supply of voltage to the plurality of cartridge heaters 1. Alternatively, the output unit 78 may output an alarm indicating an abnormal operation of a certain cartridge heater 1 together with the control of the drive unit 9 or in place of the control of the drive unit 9. As the output of the alarm, for example, an alarm sound may be generated by an alarm or the like, or an alarm may be displayed by a lamp or the like.

(4) Effect

In the mobile phase temperature control device 10 of the present embodiment, since the flow path portion 2 is wound around the rod-shaped cartridge heater 1, heat is exchanged between the cartridge heater 1 and the flow path portion 2 with high responsiveness while contact thermal resistance is reduced. Here, since the first temperature sensor 6 is attached to the downstream portion of the flow path unit 2, the temperature of the flow path unit 2 can be accurately detected as the temperature of the liquefied carbon dioxide flowing through the flow path unit 2. Therefore, the temperature of the liquefied carbon dioxide flowing through the flow path section 2 can be adjusted by the cartridge heater 1 based on the detected temperature.

Further, since the flow path section 2 is wound, the mobile phase temperature control device 10 is maintained compact even when a sufficiently long flow path section 2 is used. Therefore, by using the sufficiently long flow path section 2, the temperature of the liquefied carbon dioxide can be efficiently adjusted to a predetermined temperature even when the temperature of the liquefied carbon dioxide is low and the capacity of the liquefied carbon dioxide is large. As a result, it is possible to suppress the occurrence of a temperature gradient in the liquefied carbon dioxide in the separation column 40.

(5) Other embodiments

(a) In the above embodiment, the mobile phase temperature control device 10 includes four cartridge heaters 1, but the embodiment is not limited thereto. The mobile phase temperature conditioning device 10 may also include more than five cartridge heaters 1, and may also include three, two, or one cartridge heater 1. In the case where the mobile phase temperature adjusting device 10 includes one cartridge heater 1, the first temperature sensor 6 may be installed at a position closer to the downstream end portion than the upstream end portion of the flow path portion 2 that is in contact with the cartridge heater 1.

(b) In the above embodiment, the cartridge heater 1 has a cylindrical shape, but the embodiment is not limited thereto. The cartridge heater 1 may have an elliptic cylindrical shape, and may have other rod shapes such as other angular cylindrical shapes.

(c) In the above embodiment, the cartridge heater 1 includes the second temperature sensor 7 and the plurality of third temperature sensors 8, but the embodiment is not limited thereto. The cartridge heater 1 may also not comprise part or all of the second temperature sensor 7 and the plurality of third temperature sensors 8.

(d) In the above embodiment, the supercritical fluid apparatus 100 is configured to be able to supply liquefied carbon dioxide and the modifying agent together, but the embodiment is not limited thereto. The supercritical fluid apparatus 100 may not be configured to be able to supply the modifying agent.

(e) In the above embodiment, the mobile phase temperature control device 10 is provided to adjust the temperature of the liquefied carbon dioxide, but the embodiment is not limited thereto. The mobile phase temperature control device 10 may be provided to control the temperature of the modifier instead of the liquefied carbon dioxide, or may be provided to control the temperature of the liquefied carbon dioxide and the modifier after mixing. Alternatively, two mobile phase temperature control devices 10 may be provided to control the respective temperatures of the liquefied carbon dioxide and the modifier.

(f) In the above embodiment, the supercritical fluid apparatus 100 is configured as an SFC, but the embodiment is not limited thereto. Supercritical fluid apparatus 100 may also be configured as a supercritical fluid extraction apparatus (SFE). Alternatively, the supercritical fluid apparatus 100 may be configured to include a Mass Spectrometer (MS) instead of the SFC-MS of the detector 50.

(6) Form of the composition

The mobile phase temperature control device for supercritical fluid device according to (item 1)

The supercritical fluid device is used in a supercritical fluid device including a separation column supplied with a mobile phase in a supercritical state, and the mobile phase temperature adjustment device for the supercritical fluid device includes:

a rod-shaped cartridge heater;

a flow path section wound around the cartridge heater and guiding the mobile phase to the separation column; and

and a first temperature sensor that is attached to the flow path section and detects the temperature of the flow path section.

In the mobile phase temperature control device for a supercritical fluid device, the flow path section is wound around a rod-shaped cartridge heater, and the mobile phase is guided to the separation column of the supercritical fluid device by the flow path section. The mobile phase becomes supercritical at least in the separation column. The first temperature sensor is attached to the flow path section, and detects the temperature of the flow path section by the first temperature sensor.

According to the above configuration, since the flow path portion is wound around the rod-shaped cartridge heater, heat is exchanged between the cartridge heater and the flow path portion with high responsiveness while reducing contact thermal resistance (heat loss). Here, since the first temperature sensor is attached to the flow path portion, the temperature of the flow path portion can be accurately detected as the temperature of the mobile phase flowing through the flow path portion. Therefore, the temperature of the mobile phase flowing through the flow path portion can be adjusted by the cartridge heater based on the detected temperature.

Further, since the flow path section is wound, the mobile phase temperature control device for a supercritical fluid device can be maintained compactly even when a sufficiently long flow path section is used. Therefore, by using a sufficiently long flow path portion, the temperature of the mobile phase can be efficiently adjusted to a predetermined temperature even when the temperature of the mobile phase is low and the capacity of the mobile phase is large. As a result, the occurrence of a temperature gradient in the mobile phase in the separation column can be suppressed.

(item 2) the mobile phase temperature regulating device for supercritical fluid apparatus according to item 1, wherein the cartridge heater has a cylindrical shape.

In this case, the cartridge heater can be more easily brought into close contact with the flow path portion. This further improves the efficiency of heat exchange between the cartridge heater and the flow path portion. As a result, the occurrence of a temperature gradient in the mobile phase in the separation column can be suppressed more efficiently.

(item 3) the mobile phase temperature control device for supercritical fluid device according to item 1 or 2, which may be

The flow path portion includes an upstream end portion and a downstream end portion which are in contact with the cartridge heater, and

the first temperature sensor is attached to the flow path portion at a position closer to the downstream end portion than the upstream end portion.

In this case, the temperature of the mobile phase adjusted by the cartridge heater can be detected more accurately.

(item 4) the mobile phase temperature adjusting device for supercritical fluid device according to item 1 or 2, which may be

The cartridge heater is provided in a plurality of numbers,

a plurality of cartridge heaters are arranged in parallel,

the flow path portion is wound around the plurality of cartridge heaters.

According to the above configuration, since the flow path section is wound around the plurality of cartridge heaters arranged in parallel, the mobile phase temperature control device for a supercritical fluid device can be prevented from becoming large even when the flow path section is extremely long.

(item 5) the mobile phase temperature regulating device for supercritical fluid apparatus according to item 4, wherein the plurality of cartridge heaters are electrically connected in series.

In this case, the temperature of the mobile phase can be adjusted more sufficiently by using a plurality of cartridge heaters.

(item 6) the mobile phase temperature control device for supercritical fluid device according to item 4, which may be

The first temperature sensor is mounted at a position closer to the cartridge heater disposed furthest downstream than the cartridge heater disposed furthest upstream among the plurality of cartridge heaters.

In this case, the temperatures of the mobile phase adjusted by the plurality of cartridge heaters can be detected more accurately.

(item 7) the mobile phase temperature adjusting device for supercritical fluid device according to item 1 or 2, which may be

The temperature sensor further includes a second temperature sensor that is attached to the flow path portion and detects a temperature of the flow path portion, upstream of the first temperature sensor.

In this case, the cartridge heater can be operated more precisely based on the temperatures of the portions of the flow path section detected by the first temperature sensor and the second temperature sensor, respectively.

The supercritical fluid apparatus according to another aspect (item 8) may include:

a separation column;

a first supply unit configured to supply a first mobile phase that is in a supercritical state at least in the separation column;

a second supply unit for supplying a second mobile phase used as a modifier;

a mixing section that mixes the first mobile phase supplied from the first supply section with the second mobile phase supplied from the second supply section and guides the mixed phase to the separation column; and

the mobile phase temperature adjustment device for a supercritical fluid device according to claim 1 or 2, which is configured to adjust a temperature of at least one of the first mobile phase and the second mobile phase.

According to the above configuration, since the temperature of at least one of the first mobile phase and the second mobile phase is adjusted by the mobile phase temperature adjusting device for a supercritical fluid apparatus, the temperature of the mobile phase after mixing can be efficiently adjusted to a predetermined temperature. This can suppress the occurrence of a temperature gradient in the mobile phase in the separation column.

In another aspect (item 9), a supercritical fluid apparatus includes:

a separation column;

a mobile phase supply unit for supplying a mobile phase;

the mobile phase temperature control device for a supercritical fluid device according to claim 7, wherein the temperature of the mobile phase supplied from the mobile phase supply unit is controlled and guided to the separation column; and

a control unit for controlling the operation of the mobile phase temperature adjusting device for the supercritical fluid device,

the control section includes:

a determination unit that determines whether or not the mobile phase flows through the flow path unit based on detection results obtained by the first temperature sensor and the second temperature sensor of the mobile phase temperature adjustment device for a supercritical fluid device;

a first operation control unit that controls operation of the cartridge heater so that a temperature of the mobile phase becomes a preset temperature when the determination unit determines that the mobile phase flows through the flow path unit; and

and a second operation control unit that controls operation of the cartridge heater so that on/off of the cartridge heater is regularly repeated when the determination unit determines that the mobile phase does not flow in the flow path unit.

According to the above configuration, when the mobile phase flows through the flow path portion, the temperature of the mobile phase is adjusted to a predetermined temperature, whereby occurrence of a temperature gradient in the mobile phase in the separation column can be suppressed. On the other hand, when the mobile phase does not flow through the flow path portion, the temperature of the flow path portion can be maintained within a predetermined range by simple control by regularly repeating the on/off operation of the cartridge heater.