Capillary column oven

Abstract

The application provides a capillary column oven, comprising: a temperature control module and a transduction chamber, the temperature control module being connected to the transduction chamber; a cavity being arranged in the transduction chamber; a flow path module being arranged in the cavity; the flow path module being provided with an inlet pipe end and an outlet pipe end; a capillary being arranged in the flow path module, the capillary entering from the inlet pipe end and extending from the outlet pipe end; the temperature control module being configured to heat or cool the transduction chamber, so that the temperature in the cavity is maintained within a set temperature range; wherein the temperature of the liquid in the capillary at the outlet pipe end is within the set temperature range, so as to solve the problems that it is difficult to install a capillary in a capillary column oven at present, the capillary is prone to breakage, the Nano chromatographic resolution is low, and the peak time of the separated substance is unstable.

Description

Technical Field

[0001] This application relates to the field of Nano liquid chromatography column oven technology, and more particularly to a capillary column oven. Background Technology

[0002] Nano LC (Nano Liquid Chromatography) capillary column temperature control systems are precise temperature control devices designed for microscale chromatographic columns. The core function of these systems is to stabilize the column temperature through a capillary oven, thereby improving separation efficiency and experimental repeatability. The key value of these systems lies in addressing the temperature sensitivity of microscale chromatographic columns.

[0003] Capillary column ovens are extremely small, and fluctuations in ambient temperature directly affect the viscosity of the mobile phase and the solute partition coefficient, thus impacting retention time. A temperature control system can keep column temperature fluctuations within ±0.1°C, ensuring reproducible experimental results. By precisely controlling the column temperature (typically ranging from room temperature to 80°C), the distribution balance of the solute in the stationary and mobile phases can be adjusted, reducing peak broadening and improving the resolution of complex samples (such as proteins and peptides). Capillary column ovens generally use a metal block for heating, leveraging the uniform thermal conductivity of metal, making them suitable for applications requiring extremely high temperature uniformity.

[0004] However, the above-mentioned capillary column oven has many shortcomings in practical applications. Currently, the capillary is installed by first manufacturing the capillary column oven and then inserting the capillary tube into it. However, in order to increase the length of the capillary tube inside the capillary column oven, it is generally installed by bending. However, bending the capillary tube inside the capillary column oven can cause damage to the capillary tube. Utility Model Content

[0005] This application provides a capillary column oven to solve the technical problems of difficulty in installing capillary tubes in capillary column ovens, easy capillary tube breakage, low Nanochromatographic resolution, and unstable peak times of substances to be separated.

[0006] This application provides a capillary column oven, comprising: A temperature control module and a transducer chamber, wherein the temperature control module is connected to the transducer chamber; The transducer chamber is provided with a cavity; the cavity is provided with a flow path module; the flow path module is provided with an inlet end and an outlet end; a capillary tube is provided in the flow path module, the capillary tube enters from the inlet end and extends from the outlet end; The temperature control module is configured to heat or cool the transducer chamber to maintain the temperature inside the chamber within a set temperature range. The liquid temperature inside the capillary tube at the outlet end is within the set temperature range.

[0007] In some embodiments, the temperature control module includes: A semiconductor cooler is connected to the transducer chamber; the semiconductor cooler is used to heat or cool the transducer chamber to maintain the temperature inside the chamber within a set temperature range. An external transducer is disposed on the side of the thermoelectric cooler away from the transducer chamber; the external transducer is used to reduce the operating temperature of the thermoelectric cooler.

[0008] In some embodiments, the transducer chamber includes: A transducer block is connected to the semiconductor cooler, and a temperature sensor is installed inside the transducer block to obtain the temperature inside the cavity. A cover plate, which is connected to the transducer block; The cover plate, when connected to the transducer block, forms the chamber for accommodating the flow path module.

[0009] In some embodiments, the flow path module includes: Bottom cover; Upper cover, which is connected to the lower cover; The upper cover and the lower cover are connected to form a receiving space for accommodating the capillary; and the capillary has an inlet end that enters the receiving space and an outlet end that extends out of the receiving space; the inlet end and the outlet end are provided with connectors, and the capillary is sleeved in the connectors.

[0010] In some embodiments, the top cover is provided with a plurality of connection holes; The lower cover is provided with several snap-fit ​​posts; The lower cover is connected to the upper cover by engaging the connecting hole with the snap-fit ​​post.

[0011] In some embodiments, a snap-fit ​​bracket is provided on the outer side of the upper cover; The outer side of the lower cover is provided with a snap-fit ​​groove; The lower cover is connected to the upper cover by snapping the clip into the clip groove.

[0012] In some embodiments, the inlet end and the outlet end are located on the same side or opposite side of the flow path module.

[0013] In some embodiments, the capillary tube is provided with a plurality of inflection points within the flow path module.

[0014] In some embodiments, the thermoelectric cooler is provided with a cooling mode and a heating mode; the thermoelectric cooler is communicatively connected to the temperature sensor; The semiconductor cooler is also used to turn on or off according to the temperature inside the cavity; If the temperature inside the chamber is higher than the set temperature, the semiconductor cooler is turned on and operates in the cooling mode. If the temperature inside the chamber is equal to the set temperature, then the semiconductor cooler is turned off; If the temperature inside the chamber is lower than the set temperature, the semiconductor cooler is turned on and operates in the heating mode.

[0015] This application provides a capillary column oven, comprising: a temperature control module and a transducer chamber, wherein the temperature control module is connected to the transducer chamber; a cavity is provided within the transducer chamber; a flow path module is provided within the cavity; the flow path module is provided with an inlet end and an outlet end; a capillary tube is provided within the flow path module, the capillary tube entering from the inlet end and extending from the outlet end; the temperature control module is configured to heat or cool the transducer chamber to maintain the temperature within the cavity within a set temperature range; wherein the liquid temperature within the capillary tube located at the outlet end is within the set temperature range, thereby reducing the difficulty of installing the capillary tube within the capillary column oven by pre-installing the capillary tube within the flow path module and then placing the flow path module within the cavity of the capillary column oven, thus avoiding the problem of capillary tube breakage, and improving the Nanochromatographic separation degree and the peak time stability of the substances to be separated by the setting of the flow path module. Attached Figure Description

[0016] To more clearly illustrate the technical solution of this application, the drawings used in the embodiments will be briefly introduced below. Obviously, for those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0017] Figure 1 This is a schematic diagram of the capillary column oven in this application at one angle. Figure 2 This is a schematic diagram of the capillary column oven in this application from another angle. Figure 3 This is a schematic diagram of the capillary column oven in this application from another angle. Figure 4 This is a schematic diagram of the flow path module in one embodiment of this application; Figure 5 This is a schematic diagram of the flow path module in another embodiment of this application; Figure 6 This is a schematic diagram of the flow path module in another embodiment of this application; Figure 7 This is a schematic diagram of the first structure of the capillary in this application; Figure 8 This is a schematic diagram of the second structure of the capillary in this application; Figure 9 This is a schematic diagram of the third structure of the capillary in this application; Figure 10 This is a schematic diagram of the fourth structure of the capillary in this application; Figure 11 This is a schematic diagram of the fifth structure of the capillary in this application; Figure 12 This is a schematic diagram of the sixth structure of the capillary in this application; Figure 13 This is a schematic diagram of the seventh structure of the capillary in this application; Figure 14 The chromatograms of each substance under capillary column oven conditions described in this application were not used. Figure 15 The chromatograms of each substance obtained under capillary column temperature oven conditions as described in this application are used.

[0018] Explanation of reference numerals in the attached figures: 1-Temperature control module; 11-Semiconductor cooler; 12-External transducer; 2-Transducer chamber; 21-Cavity; 22-Transducer block; 23-Temperature sensor; 24-Cover plate; 3-Flow path module; 31-Inlet pipe end; 32-Outlet pipe end; 33-Capillary tube; 34-Lower cover; 341-Snap-fit ​​post; 342-Snap-fit ​​groove; 343-Intermediate snap-fit ​​groove; 35-Upper cover; 351-Connecting hole; 352-Snap-fit ​​bracket; 36-Connector. Detailed Implementation

[0019] To enable those skilled in the art to better understand the technical solutions in this application, the technical solutions in the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, and not all embodiments. Based on the embodiments in this application, all other embodiments obtained by those skilled in the art without creative effort should fall within the scope of protection of this application.

[0020] Because installing capillary tubes in capillary column ovens is difficult and prone to damage in some techniques, and because Nano chromatography results in low resolution and unstable peak times for the substances to be separated, this application provides a capillary column oven to address these technical problems. The structure of each part of the capillary column oven is described below: like Figures 1 to 3 The diagram shown is a structural schematic of the capillary column oven in this application.

[0021] This application provides a capillary column oven, comprising: Temperature control module 1 and transducer chamber 2, wherein temperature control module 1 is connected to transducer chamber 2; temperature control module 1 is used to heat transducer chamber 2 so that the temperature inside transducer chamber 2 reaches a set temperature.

[0022] The transducer chamber 2 is provided with a cavity 21; the cavity 21 is provided with a flow path module 3; the flow path module 3 is provided with an inlet end 31 and an outlet end 32; the flow path module 3 is provided with a capillary tube 33, which enters through the inlet end 31 and extends through the outlet end 32; the temperature control module 1 is configured to heat or cool the transducer chamber 2, so that the temperature in the cavity 21 is maintained within a set temperature range; wherein, the liquid temperature in the capillary tube 33 located at the outlet end 32 is within the set temperature range. The flow rate of the fluid in the capillary tube 33 is 0.01 ml / min to 5 ml / min, and the diameter of the capillary tube 33 is small, with an outer diameter of less than 1 mm and an inner diameter of less than 0.5 mm, making it suitable for use in nano-liquid chromatography and analytical chromatography environments. The chamber 21 is heated to a set temperature by the temperature control module 1, and the flow rate of the fluid in the capillary 33 is relatively slow, sufficient to heat or cool the fluid in the capillary 33 to the set temperature. The capillary 33 is used to transport the fluid to be heated or cooled.

[0023] For example, the capillary column oven provided in this application can also be used in nano liquid chromatography to control the temperature of the capillary column, thereby improving the resolution of nano chromatography and the stability of the peak time of the substances to be separated. It can also be used in analytical chromatography to heat the front end of the column, reducing the temperature difference between the liquid in the capillary and the column, resulting in a more stable instrument baseline. The capillary 33 in the capillary column oven provided in this application has an outer diameter of less than 1 mm and an inner diameter of less than 0.5 mm, which is suitable for experimental environments with low flow rates. Furthermore, the temperature control module 1 can maintain the liquid temperature inside the capillary 33 at the experimental temperature, i.e., the set temperature.

[0024] This application provides a capillary column oven. Because the temperature control module 1 is in direct contact with the transducer chamber 2, the heat exchange efficiency of the transducer chamber 2 is high, ensuring that the temperature inside the transducer chamber 2 is always maintained within the set temperature range, thus achieving temperature stability. Furthermore, the flow path module 3 is independently disposed within the chamber 21 inside the transducer chamber 2, ensuring the integrity of the capillary tube 33 wall and enabling the capillary tube 33 to withstand higher pressures. Simultaneously, different capillary tubes (such as PEEK capillary tubes, quartz, titanium, stainless steel, PTFE, etc.) can be replaced according to different application requirements, allowing the capillary column oven to be applied to multiple fields such as chromatography, capillary electrophoresis, and microfluidics, making it more flexible in use. It features a simple structure, convenient miniaturization, and low cost.

[0025] This application provides a capillary column temperature chamber. By setting a flow path module 3 to pre-install the capillary tube 33 in the flow path module 3, and then setting the flow path module 3 in the chamber 21 of the capillary column temperature chamber, the installation difficulty of the capillary tube 33 in the capillary column temperature chamber is reduced, thereby avoiding the problem of capillary tube 33 being damaged.

[0026] In this embodiment, the temperature control module 1 includes: A semiconductor cooler 11 is connected to the transducer chamber 2; the semiconductor cooler 11 is used to heat or cool the transducer chamber 2 so that the temperature inside the chamber 21 is maintained within a set temperature range; the semiconductor cooler 11 is provided with conditional positive and negative electrodes, through which a cooling mode or a heating mode can be selected.

[0027] The transducer chamber 2 includes: A transducer 22 is connected to the semiconductor cooler 11. A temperature sensor 23 is provided inside the transducer 22 to obtain the temperature inside the chamber 21. A cover plate 24 is connected to the transducer 22. The cover plate 24 and the transducer 22 form the chamber 21 for accommodating the flow path module 3.

[0028] Specifically, the semiconductor cooler 11 is provided with a cooling mode and a heating mode; the semiconductor cooler 11 is communicatively connected to the temperature sensor 23; the semiconductor cooler 11 is also used to turn on or off according to the temperature inside the chamber 21.

[0029] The conditions and mechanisms for turning the semiconductor cooler 11 on and off, as well as selecting the cooling and heating modes, are as follows: When the temperature inside the chamber 21 is greater than the set temperature, the semiconductor cooler 11 and the external transducer 12 are turned on and operated in the cooling mode to lower the temperature inside the chamber 21; when the temperature inside the chamber 21 is equal to the set temperature, the semiconductor cooler 11 and the external transducer 12 are turned off; when the temperature inside the chamber 21 is less than the set temperature, the semiconductor cooler 11 and the external transducer 12 are turned on and operated in the heating mode to raise the temperature inside the chamber 21.

[0030] For example, the operating power of the thermoelectric cooler 11 is determined according to the temperature difference between the temperature inside the chamber 21 and the set temperature. If the temperature difference between the temperature inside the chamber 21 and the set temperature is large, the thermoelectric cooler 11 operates at a higher operating power; if the temperature difference between the temperature inside the chamber 21 and the set temperature is small, the thermoelectric cooler 11 operates at a lower operating power.

[0031] An external transducer 12 is disposed on the side of the thermoelectric cooler 11 away from the transducer chamber 2. The external transducer 12 is used to reduce the operating temperature of the thermoelectric cooler 11. The external transducer 12 is used to dissipate heat from the thermoelectric cooler 11 and exchange heat with the outside air to ensure the stable operation of the thermoelectric cooler 11 and prevent damage caused by excessively high operating temperature. The heat exchange method, such as fan cooling or water cooling, is not limited here.

[0032] In this embodiment, the flow path module 3 includes: A lower cover 34 and an upper cover 35 are connected to the lower cover 34. The upper cover 35, when connected to the lower cover 34, forms a receiving space for accommodating the capillary tube 33. The capillary tube 33 has an inlet end 31 that enters the receiving space and an outlet end 32 that extends out of the receiving space. The inlet end 31 and the outlet end 32 are provided with connectors 36, and the capillary tube 33 is fitted into the connectors 36. The connectors 36 prevent the capillary tube 33 from bending at the inlet end 31 and the outlet end 32, thereby avoiding damage to the capillary tube 33.

[0033] In this embodiment, by pre-positioning the capillary tube 33 between the lower cover 34 and the upper cover 35 (which can be pre-bent around the snap-fit ​​post 341), and by stamping the lower cover 34 and the upper cover 35 into a single unit, the capillary tube 33 can be completely positioned between the two covers. Compared to the current method of inserting the capillary tube 33 into the capillary column oven, this method prevents damage to the capillary tube 33. Furthermore, by appropriately setting the size of the capillary tube 33 and its length within the capillary column oven, the sample to be separated within the capillary tube 33 is heated more uniformly, resulting in higher separation of substances in the sample entering the capillary column oven and more stable peak times.

[0034] In this embodiment, the upper cover 35 is provided with a plurality of connecting holes 351, such as Figure 4 and Figure 5 As shown, the lower cover 34 is provided with a plurality of snap-fit ​​posts 341; wherein, the snap-fit ​​posts 341 snap into the connecting holes 351, so that the lower cover 34 is connected to the upper cover 35. The connection holes 351 and the snap-fit ​​posts 341 allow the upper cover 35 to snap into the lower cover 34, so that the user can open the flow path module 3 to replace different capillary tubes 33 according to different application requirements.

[0035] In this embodiment, a snap-fit ​​bracket 352 is provided on the outer side of the upper cover 35, such as... Figure 6 As shown, a snap-fit ​​groove 342 is provided on the outer side of the lower cover 34; wherein, the snap-fit ​​bracket 352 snaps into the snap-fit ​​groove 342, so that the lower cover 34 is connected to the upper cover 35. Compared with the snap-fit ​​post 341, the snap-fit ​​bracket 352 and the snap-fit ​​groove 342 do not occupy the internal space of the flow path module 3, so the length of the capillary tube 33 set in the flow path module 3 can be longer, thereby improving the heat exchange effect of the fluid in the capillary tube 33.

[0036] In this embodiment, the inlet end 31 and the outlet end 32 are located on the same side or opposite sides of the flow path module 3, such as... Figure 4 or Figure 5 As shown. Users can freely choose according to their needs.

[0037] In this embodiment, the capillary 33 is located within the flow path module 3 and has several inflection points, such as... Figures 7 to 13As shown. By bending the capillary tube 33, typically with more than five bends, the length of the capillary tube 33 within the flow path module 3 is increased, thereby increasing the heat exchange area and improving heat exchange efficiency. Different bending methods can be designed according to different application scenarios. The capillary tube 33 can be bent according to the position of the clamping post 341. The bent capillary tubes 33 have gaps between them, preventing contact and thus avoiding interference between contacting capillary tubes 33 and affecting the fluid heat exchange effect within the capillary tube 33.

[0038] For example, the capillary column oven provided in this application can be applied to a capillary column oven temperature control system. The temperature control system includes a micro-flow pump, a sample injection system, a capillary column oven, and a detector connected in sequence. The sample injection system is used to draw the sample to be separated into a capillary tube 33, which is disposed in the capillary column oven. The micro-flow pump is used to draw the mobile phase to separate the sample in the capillary tube. Figure 14 and Figure 15 It is evident that, after using the capillary column oven provided in this application, the separation degree of each substance in the sample entering the capillary column oven is higher and the peak elution time is more stable, resulting in better reproducibility.

[0039] The above detailed embodiments further illustrate the purpose, technical solution, and beneficial effects of the embodiments of this application. It should be understood that the above are merely specific embodiments of the embodiments of this application and are not intended to limit the protection scope of the embodiments of this application. Any modifications, equivalent substitutions, improvements, etc., made on the basis of the technical solutions of the embodiments of this application should be included within the protection scope of the embodiments of this application.

Claims

1. A capillary column temperature chamber, characterized in that, include: Temperature control module (1) and transducer chamber (2), wherein the temperature control module (1) is connected to the transducer chamber (2); The transducer chamber (2) is provided with a chamber (21); the chamber (21) is provided with a flow path module (3); the flow path module (3) is provided with an inlet end (31) and an outlet end (32); the flow path module (3) is provided with a capillary tube (33), which enters from the inlet end (31) and extends from the outlet end (32); The temperature control module (1) is configured to heat or cool the transducer chamber (2) so that the temperature inside the chamber (21) is maintained within a set temperature range; The liquid temperature in the capillary (33) located at the outlet end (32) is within the set temperature range.

2. The capillary column temperature chamber according to claim 1, characterized in that, The temperature control module (1) includes: A semiconductor cooler (11) is connected to the transducer chamber (2); the semiconductor cooler (11) is used to heat or cool the transducer chamber (2) so that the temperature inside the chamber (21) is maintained within a set temperature range. An external transducer (12) is disposed on the side of the semiconductor cooler (11) away from the transducer chamber (2); the external transducer (12) is used to reduce the operating temperature of the semiconductor cooler (11).

3. A capillary column temperature chamber according to claim 2, characterized in that, The transducer chamber (2) includes: A transducer (22) is connected to the semiconductor cooler (11). A temperature sensor (23) is provided inside the transducer (22) and is used to obtain the temperature inside the chamber (21). Cover plate (24), the cover plate (24) is connected to the transducer block (22); The cover plate (24) is connected to the transducer block (22) to form the chamber (21) for accommodating the flow path module (3).

4. A capillary column temperature chamber according to claim 1, characterized in that, The flow path module (3) includes: Lower cover (34); Upper cover (35), the upper cover (35) being connected to the lower cover (34); The upper cover (35) and the lower cover (34) are connected to form a receiving space for accommodating the capillary tube (33); and the capillary tube (33) enters the receiving space at the inlet end (31) and the capillary tube (33) extends out of the receiving space at the outlet end (32); the inlet end (31) and the outlet end (32) are provided with connectors (36), and the capillary tube (33) is sleeved in the connectors (36).

5. A capillary column temperature chamber according to claim 4, characterized in that, The upper cover (35) is provided with a plurality of connection holes (351); The lower cover (34) is provided with a plurality of snap-fit ​​posts (341). The lower cover (34) is connected to the upper cover (35) by means of the snap-fit ​​post (341) snapping into the connection hole (351).

6. A capillary column temperature chamber according to claim 4, characterized in that, A snap-fit ​​bracket (352) is provided on the outer side of the upper cover (35); The lower cover (34) has a snap-fit ​​groove (342) on its outer side; The lower cover (34) is connected to the upper cover (35) by the snap-fit ​​bracket (352) snapping into the snap-fit ​​groove (342).

7. A capillary column temperature chamber according to claim 1, characterized in that, The inlet end (31) and the outlet end (32) are located on the same side or opposite side of the flow path module (3).

8. A capillary column temperature chamber according to claim 1, characterized in that, The capillary (33) is located within the flow path module (3) and has several inflection points.

9. A capillary column temperature chamber according to claim 3, characterized in that, The semiconductor cooler (11) is provided with a cooling mode and a heating mode; the semiconductor cooler (11) is communicatively connected to the temperature sensor (23). The semiconductor cooler (11) is also used to turn on or off according to the temperature inside the chamber (21); If the temperature inside the chamber (21) is greater than the set temperature, the semiconductor cooler (11) is turned on and operates in the cooling mode. If the temperature inside the chamber (21) is equal to the set temperature, then the semiconductor cooler (11) is turned off. If the temperature inside the chamber (21) is lower than the set temperature, the semiconductor cooler (11) is turned on and operates in the heating mode.

Images