Device for controlling temperature of chromatographic column and method for manufacturing the same

Abstract

The present invention provides a device for controlling the temperature of a chromatographic column and a manufacturing method thereof, wherein the device for controlling the temperature of a chromatographic column comprises a chromatographic column, a bottom plate, a cavity and a top plate; further comprising: a heat conduction unit having heat dissipation teeth and arranged on the inner side of the bottom plate; a refrigeration unit arranged on the outer side of the bottom plate and in contact with the heat conduction unit; a circuit board arranged on the outer side of the cavity; a heating module winding around the chromatographic column, and a spiral chromatographic column arranged on the upper side of the heat conduction unit; a wire connecting the heating module connecting the circuit board; a temperature sensor arranged in the cavity, and a wire connecting the temperature sensor connecting the circuit board; a heating seat having an opening and arranged on the outer side of the cavity; a joint arranged in the heating seat and connected to the opening; two ends of the chromatographic column respectively pass through the through holes of the cavity and are connected to the joint; a heater and a temperature measuring element are respectively arranged in the heating seat. The present invention has the advantages of small size and low energy consumption.

Description

Technical Field

[0001] The invention relates to the field of chromatographic analysis, and in particular to a device for controlling the temperature of a chromatographic column and a manufacturing method thereof. Background Art

[0002] At present, the temperature control technology of column oven mostly adopts gas bath heating scheme, specifically, heating wire gas bath heating realizes programmed temperature rise of chromatographic column. The power required for heating is relatively high (about 2000W), and the temperature control range is usually around room temperature + 10℃ ~ 400℃. Some low-boiling point substances can only be effectively separated at lower temperatures, and ordinary column ovens cannot achieve effective separation of low-boiling point substances.

[0003] In order to solve the problem of high power of column oven, some companies have launched miniaturized column oven, but the chromatographic column is still heated by gas bath heating. The disadvantage of this method is that it cannot solve the problem of heat loss in gas bath heating.

[0004] In order to solve the problem of low-temperature separation, the existing technology uses liquid nitrogen or liquid CO2 to provide a lower initial temperature for the column box. The disadvantage of this method is that it cannot achieve precise control of the low temperature. Summary of the invention

[0005] In order to solve the deficiencies in the above-mentioned prior art solutions, the present invention provides a device for controlling the temperature of a chromatographic column.

[0006] The objective of the present invention is achieved through the following technical solutions:

[0007] A device for controlling the temperature of a chromatographic column, the device comprising a chromatographic column, a bottom plate, a cavity and a top plate, wherein the bottom plate, the cavity and the top plate enclose a closed space, and the chromatographic column is arranged in the closed space; the device further comprising:

[0008] A heat conduction unit, the heat conduction unit having heat dissipation teeth and arranged on the inner side of the bottom plate;

[0009] A refrigeration unit, which is arranged on the outside of the bottom plate and in contact with the heat conduction unit;

[0010] A circuit board, wherein the circuit board is arranged outside the cavity;

[0011] A heating module, wherein the heating module is wound around the chromatographic column, and the spiral chromatographic column is arranged on the upper side of the heat conducting unit; and an electric wire connecting the heating module is connected to the circuit board;

[0012] A temperature sensor, wherein the temperature sensor is disposed in the cavity, and a wire connected to the temperature sensor is connected to the circuit board;

[0013] A heating seat and a joint, wherein the heating seat has an opening and is arranged outside the cavity; the joint is arranged inside the heating seat and communicates with the opening; two ends of the chromatographic column respectively pass through the through holes of the cavity and are connected to the joint;

[0014] The heater and the temperature measuring element are respectively arranged in the heating seat.

[0015] The object of the present invention is also to provide a method for manufacturing a device for controlling the temperature of a chromatographic column according to the present invention, and the object of the invention is achieved by the following technical solutions:

[0016] A method for manufacturing a device for controlling the temperature of a chromatographic column, the method comprising the following steps:

[0017] (A1) fixing a heat conduction unit on the inner side of the bottom plate, wherein the heat conduction unit has heat dissipation teeth;

[0018] (A2) fixing a spiral chromatographic column on the upper side of the heat conducting unit, with a heating module wrapped around the outer side of the chromatographic column; and a temperature sensor being arranged on the upper side of the bottom plate;

[0019] (A3) installing a cavity, placing the cavity on the upper side of the bottom plate, placing a first connector at a through hole of the cavity, and sealing the through hole;

[0020] The heating seat is fixed on the outside of the cavity, the heating seat has an opening, and the cylindrical part on the lower side of the heating seat passes through the through hole of the cavity; the joint is arranged in the heating seat and communicated with the opening; the two ends of the chromatographic column pass through the cylindrical part respectively and are connected to the joint;

[0021] (A4) Line connection: The wires of the heating module and the temperature sensor are respectively plugged into the part of the first connector located inside the cavity;

[0022] The heater and the temperature measuring element are respectively arranged in the heating seat;

[0023] (A5) fixing a top plate on the upper side of the cavity;

[0024] (A6) a circuit board is plugged into a portion of the first connector that is outside the cavity;

[0025] (A7) Wrapping the heat-insulating material around the outside of the cavity, the bottom plate and the top plate;

[0026] (A8) A protective shell is provided on the outside of the heat-insulating material, and the second connector on the circuit board is exposed.

[0027] Compared with the prior art, the present invention has the following beneficial effects:

[0028] 1. High temperature control efficiency;

[0029] The chromatographic column is directly heated by the heating module wrapped around the chromatographic column, while the heating of the chromatographic column (the part entering and exiting the cavity) not wrapped by the heating module is realized by the outer body and the cylindrical part of the chromatographic column, thereby realizing the rapid heating of the entire chromatographic column;

[0030] The refrigeration unit arranged outside the cavity is connected to the heat transfer unit, which quickly reduces the temperature inside the cavity; the setting of the fan further reduces the cooling time;

[0031] By using various seals and insulation materials, the space where the chromatographic column is located is sealed, and the heat exchange with the outside world (non-refrigeration unit) is reduced, further improving the temperature control efficiency;

[0032] 2. High temperature control accuracy;

[0033] The temperature sensor is set in a closed space, and the real-time temperature is used to accurately control the heating module and the refrigeration unit, thereby improving the temperature control accuracy of the chromatographic column part in the cavity;

[0034] The temperature sensor suspended between the heat dissipation teeth accurately obtains the real temperature and improves the subsequent temperature control accuracy;

[0035] The heating of the chromatographic column that is not wrapped with the heating module is realized by the heater and the temperature measuring element alone, so that the temperature control accuracy of the chromatographic column part entering and leaving the cavity is achieved;

[0036] 3. Low power consumption;

[0037] In view of the direct heating solution and the use of protective materials for insulation, as well as the closed space formed, the power consumption of heating is reduced, and the overall heating power is less than 100W, which is significantly lower than 2000W in the prior art. BRIEF DESCRIPTION OF THE DRAWINGS

[0038] The disclosure of the present invention will become easier to understand with reference to the accompanying drawings. It is easy for those skilled in the art to understand that these drawings are only used to illustrate the technical solution of the present invention and are not intended to limit the scope of protection of the present invention. In the drawings:

[0039] Figure 1 It is a schematic flow chart of a method for manufacturing a device for controlling the temperature of a chromatographic column according to an embodiment of the present invention. DETAILED DESCRIPTION

[0040] Figure 1The following description describes the optional embodiments of the present invention to teach those skilled in the art how to implement and reproduce the present invention. In order to explain the technical solution of the present invention, some conventional aspects have been simplified or omitted. Those skilled in the art will understand that variations or replacements derived from these embodiments will be within the scope of the present invention. Those skilled in the art will understand that the following features can be combined in various ways to form multiple variations of the present invention. Thus, the present invention is not limited to the following optional embodiments, but is only limited by the claims and their equivalents.

[0041] Embodiment 1:

[0042] The device for controlling the temperature of a chromatographic column according to an embodiment of the present invention comprises:

[0043] A chromatographic column, a bottom plate, a cavity and a top plate, wherein the bottom plate, the cavity and the top plate enclose a closed space, and the chromatographic column is arranged in the closed space;

[0044] A heat conduction unit, the heat conduction unit having heat dissipation teeth and arranged on the inner side of the bottom plate;

[0045] A cooling unit, such as a TEC, is disposed on the outside of the base plate and in contact with the heat transfer unit;

[0046] A circuit board, wherein the circuit board is arranged outside the cavity;

[0047] A heating module, such as an insulated heating wire, is wound around the chromatographic column, and the spiral chromatographic column is arranged on the upper side of the heat conducting unit; the wires connected to the heating module are connected to the circuit board, such as the wires pass through the through holes of the cavity to connect to the circuit board, or are connected by a connector arranged at the through holes of the cavity;

[0048] A temperature sensor, wherein the temperature sensor is disposed in the cavity, and a wire connected to the temperature sensor is connected to the circuit board, such as the wire passes through a through hole in the cavity to connect to the circuit board, or is connected by a connector disposed at the through hole in the cavity;

[0049] A heating seat and a connector, wherein the heating seat has an opening and is arranged outside the cavity; the connector is arranged inside the heating seat and communicates with the opening; both ends of the chromatographic column respectively pass through the through holes of the cavity and are connected to the connector; that is, the heating of the portion of the chromatographic column that is not wound by the heating module (that is, the portion entering and exiting the cavity) is achieved;

[0050] The heater and the temperature measuring element are respectively arranged in the heating seat.

[0051] In order to utilize the heating seat outside the cavity to heat the chromatographic column entering and exiting the cavity, the heating seat further comprises:

[0052] A body, the body having the opening and arranged outside the cavity, a first sealing member being arranged between the body and the outer wall of the cavity; the heater and the temperature measuring element being arranged inside the body;

[0053] A cylindrical component, one end of which is fixed to the bottom side of the body, and the other end of which passes through the through hole of the cavity and enters the cavity; the chromatographic column passes through the cylindrical component and is connected to the joint.

[0054] In order to prevent accidental contact with the heating seat with high temperature and form a closed space, the heating seat further includes:

[0055] A protective cover, the two ends of the protective cover are open and arranged outside the body; a second sealing member is arranged between the bottom end of the protective cover and the body, and a third sealing member is arranged between the outer wall of the body on the upper side of the joint and the protective cover;

[0056] The screw passes through the through hole surrounding the opening at the top of the protective cover and is fixed in the screw hole at the top of the body; the second sealing member and the third sealing member are respectively squeezed between the protective cover and the body, and the opening of the body is exposed.

[0057] In order to stably fix the chromatographic column, further, a support column is arranged on the inner wall of the bottom plate, the support column is arranged around the heat conduction unit, the chromatographic column is fixed on the support column, and a gap is provided between the heat conduction unit and the chromatographic column.

[0058] In order to increase the cooling speed, further, the device for controlling the temperature of the chromatographic column also includes:

[0059] A fan is arranged on the upper side of the heat conduction unit and is located in the area surrounded by the chromatographic column; an electric wire connected to the fan passes through the cavity and is connected to the circuit board.

[0060] In order to form a closed space to improve the efficiency of temperature control, further, the device for controlling the temperature of the chromatographic column also includes:

[0061] A first connector is arranged at the through hole of the cavity and closes the through hole; the wires of the heating module, the temperature sensor and the fan are respectively plugged into the part of the first connector located inside the cavity, and the circuit board is plugged into the part of the first connector located outside the cavity.

[0062] In order to improve the temperature efficiency and protection effect of the chromatographic column, further, the device for controlling the temperature of the chromatographic column also includes:

[0063] A shell, the shell being arranged outside the cavity, the bottom plate and the top plate;

[0064] The heat-insulating material is arranged in the space between the shell and the cavity, and the second connector on the circuit board is exposed.

[0065] In order to accurately obtain the temperature of the chromatographic column, further, the temperature sensor is suspended between the heat dissipation teeth.

[0066] Figure 1 A flow chart of a method for manufacturing a device for controlling the temperature of a chromatographic column according to an embodiment of the present invention is schematically provided. Figure 1 As shown, the manufacturing method comprises the following steps:

[0067] (A1) fixing a heat conduction unit on the inner side of the bottom plate, such as by screws, wherein the heat conduction unit has heat dissipation teeth;

[0068] (A2) fixing a spiral chromatographic column on the upper side of the heat conducting unit, with a heating module wrapped around the outer side of the chromatographic column; and a temperature sensor being arranged on the upper side of the bottom plate;

[0069] (A3) installing a cavity, placing the cavity on the upper side of the bottom plate, placing a first connector at a through hole of the cavity, and sealing the through hole;

[0070] The heating seat is fixed on the outside of the cavity, the heating seat has an opening, and the cylindrical part on the lower side of the heating seat passes through the through hole of the cavity; the joint is arranged in the heating seat and communicated with the opening; the two ends of the chromatographic column pass through the cylindrical part respectively and are connected to the joint;

[0071] (A4) Line connection: The wires of the heating module and the temperature sensor are respectively plugged into the part of the first connector located inside the cavity;

[0072] The heater and the temperature measuring element are respectively arranged in the heating seat;

[0073] (A5) fixing a top plate on the upper side of the cavity;

[0074] (A6) a circuit board is plugged into a portion of the first connector that is outside the cavity;

[0075] (A7) Wrapping the heat-insulating material around the outside of the cavity, the bottom plate and the top plate;

[0076] (A8) A protective shell is provided on the outside of the heat-insulating material, and the second connector on the circuit board is exposed.

[0077] In order to prevent accidental contact with the high-temperature heating seat and form a closed space, further, in step (A3), a protective cover is put on the outer side of the heating seat, and the opening of the heating seat is exposed;

[0078] The screw passes through the through hole surrounding the opening at the top of the protective cover and is fixed in the screw hole at the top of the heating seat; the second sealing member between the bottom end of the protective cover and the heating seat is squeezed, and the third sealing member provided between the outer wall of the heating seat on the upper side of the joint and the protective cover is squeezed;

[0079] The first seal between the heating seat and the cavity is compressed.

[0080] Embodiment 2:

[0081] An application example of the device for controlling a chromatographic column and the method for manufacturing the same according to Example 1 of the present invention.

[0082] In this application example, the inner wall of the rectangular bottom plate has a sixth annular groove, a sixth O-ring is arranged inside, a rectangular through hole is provided in the enclosed area of ​​the sixth annular groove, and a mounting hole is provided between the rectangular through hole and the sixth annular groove;

[0083] The side of the heat conduction unit facing the rectangular through hole is a plane, and the other side facing away from the rectangular through hole has heat dissipation teeth distributed in an array. The screws pass through the heat conduction unit and are fixed on the mounting hole, so that the heat conduction unit is fixed on the inner side of the rectangular through hole, that is, the inner side of the bottom plate; a plurality of support columns are fixed on the inner side of the bottom plate and surround the heat conduction unit; the cooling unit arranged on the outer side of the bottom plate adopts TEC, and the cold end passes through the rectangular through hole and contacts with the plane of the heat conduction unit;

[0084] The heating module uses a heating wire, which is directly wound on the chromatographic column. The chromatographic column is spiral-shaped, and the inlet and outlet ends are linear. A heat-conducting film is wound around the spiral part of the chromatographic column, and this part of the chromatographic column is fixed on the support column, and there is a gap between the chromatographic column and the heat dissipation teeth (no contact).

[0085] The temperature sensor is suspended between the heat dissipation teeth, and the fan is arranged on the upper side of the heat dissipation teeth and is located in the area surrounded by the spiral chromatographic column;

[0086] The cavity is rectangular, and the hollow part is cylindrical; the upper side of the cavity has a first through hole and a second through hole, and the lower side has a third through hole; the outer wall of the cavity has a fifth annular groove surrounding the third through hole, and a fifth O-ring is arranged in the groove; the first connector is fixed at the third through hole and squeezes the fifth O-ring, thereby closing the third through hole; the outer side of the cavity has a first annular groove surrounding the first through hole, and a fourth annular groove surrounding the second through hole, the first O-ring is arranged in the first annular groove, and the fourth O-ring is arranged in the fourth annular groove;

[0087] The first heating seat and the second heating seat adopt the same structure, the first joint and the second joint are the same, the first heating seat includes a body and a cylindrical part made of metal material, the top end of the body has an opening connected to the first joint, and a hole surrounding the opening, the body is fixed on the outside of the first through hole and squeezes the first O-ring, the cylindrical part is fixed on the lower side of the body, passes through the first through hole, surrounds the linear chromatographic column, the first joint is between the bodies, and is connected to the chromatographic column passing through the cylindrical part; the outer wall of the body on the upper side of the first joint has a third annular groove, and the third O-ring is arranged in the third annular groove; the first protective cover is the same as the second protective cover, both of which are open at two ends; the bottom end of the first protective cover has a second annular groove, the second O-ring is arranged in the second annular groove, and the top end has a plurality of through holes surrounding the opening; the screw passes through the through hole at the top end of the first protective cover and is fixed in the hole at the top end of the body, and the second O-ring and the third O-ring are squeezed; the installation method between the second protective cover and the second heating seat is the same as the first protective cover;

[0088] The circuit board is arranged outside the cavity and plugged into the part of the first connector outside the cavity, and the second connector is fixed on the circuit board; the wires of the heating module, the fan and the temperature sensor are plugged into the part of the first connector inside the cavity;

[0089] The heat-insulating material is arranged on the outside of the cavity, the bottom plate and the top plate, the shell is arranged on the outside of the heat-insulating material, and the second connector on the circuit board is exposed to facilitate connection with external electrical components.

[0090] like Figure 1 As shown, the manufacturing method of the device for controlling the chromatographic column of this embodiment comprises the following steps:

[0091] (A1) fixing the heat conducting unit on the inner side of the bottom plate, that is, the inner side of the rectangular through hole, wherein the heat conducting unit has heat dissipation teeth on the side facing away from the rectangular through hole and a flat surface on the side facing the rectangular through hole;

[0092] (A2) fixing a spiral chromatographic column on the upper side of the heat-conducting unit, and winding a heating module and a heat-conducting film around the outer side of the chromatographic column in sequence; a temperature sensor is arranged on the upper side of the bottom plate, suspended between the heat-dissipating teeth;

[0093] (A3) installing the cavity, setting the cavity on the upper side of the bottom plate, with a sixth O-ring between the cavity and the bottom plate; setting the first connector at the third through hole of the cavity, and squeezing the fifth O-ring to close the third through hole;

[0094] The straight portion of the chromatographic column passes through the first through hole and the second through hole respectively;

[0095] The screw passes through the bottom plate and connects to the cavity, and the sixth O-ring is squeezed;

[0096] The body of the first heating seat is fixed at the first through hole on the outside of the cavity, the body squeezes the first O-ring, the cylindrical component passes through the first through hole into the cavity, the linear chromatographic column passes through the cylindrical component and is connected to the first joint, and the first joint is connected to the opening of the body;

[0097] The first protective cover is arranged on the outer side of the body, the screw passes through the through hole at the top of the first protective cover and is fixed in the hole at the top of the body, and the second O-ring and the third O-ring are squeezed;

[0098] Similarly, install the second heating seat and the second protective cover;

[0099] (A4) Line connection: The wires of the heating module, the fan and the temperature sensor are respectively plugged into the part of the first connector located inside the cavity;

[0100] The heater and the temperature measuring element are respectively arranged in the first heating seat and the second heating seat;

[0101] (A5) fixing the top plate on the upper side of the cavity, the lower side of the top plate having a seventh annular groove, and a seventh O-ring disposed inside the groove;

[0102] The screw passes through the top plate and connects to the chamber, and the seventh O-ring is squeezed;

[0103] (A6) a circuit board is plugged into a portion of the first connector that is outside the cavity;

[0104] (A7) Wrapping the heat-insulating material around the outside of the cavity, the bottom plate and the top plate;

[0105] (A8) A protective shell is provided on the outside of the heat-insulating material, and the second connector on the circuit board is exposed.

Claims

1. A method for manufacturing a device for controlling the temperature of a chromatographic column, the device comprising a chromatographic column, a bottom plate, a cavity and a top plate, wherein the bottom plate, the cavity and the top plate enclose a closed space, and the chromatographic column is arranged in the closed space; The device for controlling the temperature of the chromatographic column also includes: A heat conduction unit, the heat conduction unit having heat dissipation teeth and arranged on the inner side of the bottom plate; A refrigeration unit, which is arranged on the outside of the bottom plate and in contact with the heat conduction unit; A circuit board, wherein the circuit board is arranged outside the cavity; A heating module, wherein the heating module is wound around the chromatographic column, and the spiral chromatographic column is arranged on the upper side of the heat conducting unit; and an electric wire connecting the heating module is connected to the circuit board; A temperature sensor, wherein the temperature sensor is suspended between the heat dissipation teeth, and a wire connected to the temperature sensor is connected to the circuit board; A heating seat and a joint, wherein the heating seat comprises a body and a cylindrical component, the top end of the body has an opening, the body is arranged outside the cavity, and a sealing member is arranged between the body and the outer wall of the cavity; one end of the cylindrical component is fixed to the bottom side of the body, and the other end passes through the through hole of the cavity and enters the cavity; the joint is between the bodies and communicated with the opening; the two ends of the chromatographic column respectively pass through the cylindrical component and are connected to the joint; A heater and a temperature measuring element, wherein the heater and the temperature measuring element are respectively arranged in the body; The manufacturing method comprises the following steps: (A1) fixing a heat conduction unit on the inner side of the bottom plate, wherein the heat conduction unit has heat dissipation teeth; (A2) fixing a spiral chromatographic column on the upper side of the heat conducting unit, with a heating module wrapped around the outer side of the chromatographic column; and a temperature sensor being arranged on the upper side of the bottom plate; (A3) installing the cavity, placing the cavity on the upper side of the bottom plate, placing the first connector at the through hole of the cavity, and sealing the through hole; The heating seat is fixed on the outside of the cavity, the heating seat has an opening, and the cylindrical component on the lower side of the heating seat passes through the through hole of the cavity and enters the cavity; the joint is arranged in the heating seat and communicated with the opening; the two ends of the chromatographic column pass through the cylindrical component respectively and are connected to the joint; (A4) Line connection: The wires of the heating module and the temperature sensor are respectively plugged into the part of the first connector located inside the cavity; The heater and the temperature measuring element are respectively arranged in the heating seat; (A5) fixing the top plate on the upper side of the cavity, the bottom plate, the cavity and the top plate enclose a closed space, and the chromatographic column is arranged in the closed space; (A6) The circuit board is plugged into the portion of the first connector that is outside the cavity; (A7) Wrapping the insulation material around the outside of the cavity, the bottom plate and the top plate; (A8) A protective shell is provided on the outer side of the heat-insulating material, and the second connector on the circuit board is exposed.

2. The manufacturing method according to claim 1, characterized in that: In step (A3), the protective cover is put on the outer side of the heating seat, and the opening of the heating seat is exposed; The screw passes through the through hole surrounding the opening at the top of the protective cover and is fixed in the screw hole at the top of the heating seat; the second sealing member between the bottom end of the protective cover and the heating seat is squeezed, and the third sealing member provided between the outer wall of the heating seat on the upper side of the joint and the protective cover is squeezed; The first seal between the heating seat and the cavity is compressed.

3. The manufacturing method according to claim 1, characterized in that: The heating seat also includes: A protective cover, the two ends of the protective cover are open and arranged outside the body; a second sealing member is arranged between the bottom end of the protective cover and the body, and a third sealing member is arranged between the outer wall of the body on the upper side of the joint and the protective cover; The screw passes through the through hole surrounding the opening at the top of the protective cover and is fixed in the screw hole at the top of the body; the second sealing member and the third sealing member are respectively squeezed between the protective cover and the body, and the opening of the body is exposed.

4. The manufacturing method according to claim 1, characterized in that: A support column is arranged on the inner wall of the bottom plate, the support column is arranged around the heat conduction unit, the chromatographic column is fixed on the support column, and a gap is provided between the heat conduction unit and the chromatographic column.

5. The manufacturing method according to claim 1, characterized in that: The device for controlling the temperature of the chromatographic column also includes: A fan is arranged on the upper side of the heat conduction unit and is located in the area surrounded by the chromatographic column; an electric wire connected to the fan passes through the cavity and is connected to the circuit board.

6. The manufacturing method according to claim 5, characterized in that: The device for controlling the temperature of the chromatographic column also includes: A first connector is arranged at the through hole of the cavity and closes the through hole; the wires of the heating module, the temperature sensor and the fan are respectively plugged into the part of the first connector located inside the cavity, and the circuit board is plugged into the part of the first connector located outside the cavity.

7. The manufacturing method according to claim 1, characterized in that: The device for controlling the temperature of the chromatographic column also includes: A shell, the shell being arranged outside the cavity, the bottom plate and the top plate; The heat-insulating material is arranged in the space between the shell and the cavity, and the second connector on the circuit board is exposed.

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