CN209784277U - Derivative device and chromatograph with same - Google Patents
Derivative device and chromatograph with same Download PDFInfo
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- CN209784277U CN209784277U CN201920244794.4U CN201920244794U CN209784277U CN 209784277 U CN209784277 U CN 209784277U CN 201920244794 U CN201920244794 U CN 201920244794U CN 209784277 U CN209784277 U CN 209784277U
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Abstract
The utility model provides a derivatization device and a chromatograph with the derivatization device, wherein the derivatization device comprises a reactor, the reactor is provided with a derivatization pipeline and a heating unit coupled with the derivatization pipeline, and the heating unit can heat a substance to be detected in the derivatization pipeline; the cooling pipeline is communicated with the derivative pipeline; the derivative device also comprises a radiator, wherein the radiator is arranged on the outer side of the cooling pipeline and can cool the substance to be detected in the cooling pipeline. Through add in the cooling pipeline outside and to wait that the material carries out refrigerated radiator to detecting in the cooling pipeline, the utility model provides a device derives can improve the cooling pipeline's of unit length radiating efficiency effectively, when guaranteeing the effective cooling of the mobile phase after heating in the high temperature system of deriving, can reduce the length of cooling pipeline, has alleviated the problem of widening of the chromatographic peak because of the diffusion causes effectively.
Description
Technical Field
The present invention relates to a chromatography, and more particularly, to a derivatization device for derivatizing a substance to be detected, and a chromatograph having the derivatization device.
background
Derivatization is the use of chemical transformations to convert compounds into substances of similar chemical structure. In general, a compound of a particular function participates in a derivatization reaction, and a deviation in solubility, boiling point, melting point, aggregation state, or chemical composition occurs. The derivatization of the sample mainly serves to convert substances which are difficult to analyze into substances which are similar to the chemical structure of the sample but easy to analyze, and facilitates quantification and separation. When the detection substance is not readily detectable, e.g., no UV absorption, it can be treated, e.g., with a chromophore, to produce a detectable substance. Therefore, derivatization is widely used in instrumental analysis.
In a chromatograph, a derivatization reaction is generally performed on a mobile phase that has been separated by a chromatographic column using a post-column derivatization device. In order to increase the rate of the derivatization reaction or to meet the reaction temperature requirement, the substance to be detected is generally heated, and therefore, the post-column derivatization device is generally equipped with a heating unit. Meanwhile, for a high-temperature derivatization system, the temperature of the heated mobile phase is high, and the mobile phase with the excessively high temperature can cause adverse effects on the detection accuracy and the reliability of the instrument, so that the post-column derivatization device is correspondingly provided with a cooling pipeline for cooling the heated mobile phase at the upstream of the detector.
however, the chromatographic instrument using the post-column derivatization device in the prior art has serious broadening of the chromatographic peak and lower resolution.
SUMMERY OF THE UTILITY MODEL
the inventor finds that the chromatographic peak is seriously widened and the resolution is lower due to at least part of the reasons that the chromatographic peak is seriously widened and the resolution is lower through the intensive research of a post-column derivative device in the prior art: in long cooling lines, the diffusion of the substance to be detected in the mobile phase is severe.
Fig. 1 is a schematic diagram of diffusion of a substance to be detected in a cooling pipeline, and referring to fig. 1, when a mobile phase flows in the cooling pipeline, the flow resistance f1 of the mobile phase near the inner wall portion of the pipeline is larger, the flow resistance f2 of the central portion is smaller, after flowing for a certain distance, the substance to be detected in the mobile phase will relatively diffuse and spread along the conveying direction, and the diffusion degree of the central portion is larger than that of the mobile phase near the inner wall portion of the pipeline, so as to form a distribution of the substance to be detected as shown in the right side of fig. 1, and the substance to be detected which is unevenly distributed will be successively introduced into a detector for analysis in a longer duration, so that the chromatographic peak thereof is widened, and the resolution of a chromatograph is reduced. The problem of broadening of the chromatographic peak caused by the diffusion becomes more serious as the length of the cooling pipeline increases. However, simply shortening the cooling line may affect the accuracy of detection and the reliability of the instrument due to insufficient cooling of the mobile phase.
In view of the above technical problems in the prior art, the utility model provides a derivatization device, which comprises a reactor, wherein the reactor is provided with a derivatization pipeline and a heating unit coupled with the derivatization pipeline, and the heating unit can heat a substance to be detected in the derivatization pipeline; the cooling pipeline is communicated with the derivative pipeline; the derivative device also comprises a radiator, wherein the radiator is arranged on the outer side of the cooling pipeline and can cool the substance to be detected in the cooling pipeline.
Through add in the cooling pipeline outside and to wait that the material carries out refrigerated radiator to detecting in the cooling pipeline, the utility model provides a device derives can improve the cooling pipeline's of unit length radiating efficiency effectively, when guaranteeing the effective cooling of the mobile phase after heating in the high temperature system of deriving, can reduce the length of cooling pipeline, has alleviated the problem of widening of the chromatographic peak because of the diffusion causes effectively.
The utility model discloses an among the preferred technical scheme, the radiator is attached the heat dissipation piece that the cooling line surface set up. The heat dissipation part attached to the surface of the cooling pipeline can effectively conduct the heat on the surface of the cooling pipeline, and the heat dissipation effect is improved.
The utility model discloses an among the preferred technical scheme, the radiator is for providing the air cooling device of flowing gas to the cooling line surface.
The utility model discloses an among the preferred technical scheme, the radiator is the liquid cooling device with cooling line surface coupling. Adopt the liquid cooling device to cool off the cooling pipeline surface, can provide better cooling effect on the one hand, on the one hand the liquid cooling device noise, shake all less, are favorable to improving detection device measuring stability.
The utility model discloses an among the preferred technical scheme, the material of cooling line is: one or more of stainless steel, copper, aluminum, polyether-ether-ketone, high-density polyethylene and nylon. The cooling pipeline can be made of the doped or undoped, coated or uncoated material, so that the corrosion resistance of the material is ensured, and the heat conduction performance of the cooling pipeline is effectively improved.
The utility model discloses an among the preferred technical scheme, the inside of cooling tube still possesses porous structure. The cooling pipeline with the porous structure can increase the contact area between the substance to be detected and the pipeline in the pipeline, and improve the heat dissipation effect of the cooling pipeline.
The utility model discloses an among the preferred technical scheme, cooling line one end is direct to be linked together with the pipeline that derives, and the other end can be direct to be linked together with the introduction port of chromatograph detector. Through above connected mode, the length of cooling tube can be further reduced, avoids using the pipeline of unnecessary length to dispel the heat.
The utility model discloses an among the preferred technical scheme, the radiating piece still includes a plurality of radiating fin, slope or perpendicular to cooling pipeline setting. The arrangement of the radiating fins can further increase the contact area of the radiating piece and the external environment, and the radiating effect is improved.
The utility model discloses an among the preferred technical scheme, the radiating piece deviates from one side of cooling line and the attached setting of casing of derived device. The shell of the derivative device can help the heat dissipation plate to dissipate heat conducted from the cooling pipeline in time, and therefore the heat dissipation effect is improved.
In a preferred embodiment of the present invention, the derivatization device is a post-column derivatization device for chromatographic analysis.
The utility model also provides a chromatograph with derivative device.
Drawings
FIG. 1 is a schematic view of diffusion of a substance to be detected in a cooling circuit;
Fig. 2 is a schematic structural diagram of a derivative device according to a first embodiment of the present invention;
3 FIG. 3 3 3 is 3 a 3 cross 3- 3 sectional 3 view 3 of 3 the 3 cooling 3 circuit 3 portion 3 of 3 the 3 derivative 3 device 3 of 3 FIG. 3 2 3 taken 3 along 3 the 3 line 3 A 3- 3 A 3; 3
Fig. 4 is a schematic structural view of a derivatization device according to a second embodiment of the present invention;
Fig. 5 is a schematic structural diagram of a derivatization device in a third embodiment of the present invention;
Fig. 6 is a schematic structural diagram of a derivatization device according to a fourth embodiment of the present invention.
reference numerals: 1-a mobile phase mixing line; 11-a first conduit; 12-a second conduit; 2-a reactor; 20-a derivative line; 21-a heating unit; 3-a cooling pipeline; 31-a porous structure; 4-a radiator; 41-a heat sink; 42-heat dissipation fins; 5-a detector; 50-sample inlet.
Detailed Description
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only for explaining the technical principle of the present invention, and are not intended to limit the scope of the present invention. And can be modified as needed by those skilled in the art to suit particular applications.
It should be noted that in the description of the preferred embodiments of the present invention, the terms of direction or positional relationship indicated by the terms "upper", "lower", "left", "right", "front", "rear", "vertical", "horizontal", "inner", "outer", etc., are based on the directions or positional relationships shown in the drawings, which are for convenience of description only, and do not indicate or imply that the devices or components must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
Implementation mode one
As shown in fig. 2, the present embodiment provides a post-column derivatization device for a high performance liquid chromatograph, which is used for performing a derivatization reaction on a substance to be detected in a mobile phase separated by a chromatographic column. The post-column derivatization device sequentially comprises the following components in the conveying direction of a mobile phase: mobile phase mixing line 1, reactor 2 and cooling line 3.
The mobile phase mixing pipeline 1 comprises a first pipeline 11 used for conveying a mobile phase which is separated by a liquid chromatographic column and contains a substance to be detected, and a second pipeline 12 used for conveying a derivative reaction liquid, wherein the first pipeline 11 and the second pipeline 12 are communicated with each other, and the mobile phase containing the substance to be detected is mixed with the derivative reaction liquid and then is introduced into the reactor 2.
In the present embodiment, the reactor 2 includes a derivation line 20 communicating with the mobile phase mixing line 1, and a derivatization reaction occurs in the derivation line 20. In order to increase the reaction rate of the derivatization reaction or meet the reaction temperature requirement, the reactor 2 in this embodiment is configured with a heating unit 21 coupled to the derivatization pipeline 20, the heating unit 21 can adopt a heating mode with programmed temperature control, and the temperature of the derivatization pipeline 20 can be stably controlled within the range from room temperature to 160 ℃. Under high temperature conditions, the substance to be detected inside the derivation pipeline 20 will undergo a chemical reaction, and a substance which is easily detected by the detector 5 is obtained from the substance which is originally not easily detected by the detector 5. In this embodiment, the derivative conduit 20 is a long conduit or other suitable type of flow path.
After the derivatization reaction is completed or basically completed, the high-temperature mobile phase with the substance to be detected is introduced into the cooling pipeline 3, so that the mobile phase is cooled to a temperature range which can be accepted by the detector 5, and the influence on the detection accuracy and the reliability of the instrument is prevented.
in order to sufficiently cool the high-temperature mobile phase by the cooling line 3 which is as short as possible, the cooling line 3 is made of a stainless material in the present embodiment. The cooling pipeline 3 made of the stainless steel material can give consideration to both the corrosion resistance and the heat conduction performance of the material. In other embodiments of the present invention, the cooling pipeline 3 may also be made of doped or undoped, coated or uncoated copper, aluminum, polyetheretherketone, high density polyethylene, nylon, or other materials. The heat-conducting property of the material can be improved by doping particles such as metal, ceramic and the like, and the corrosion resistance of the cooling pipeline 3 can be effectively improved by plating metal or a high-molecular film. Fig. 3 is a schematic cross-sectional structure diagram of a portion of the cooling pipeline 3 in fig. 2, and as can be seen from fig. 3, the cooling pipeline 3 is internally provided with a porous structure 31, and the porous structure 31 can increase the contact area between the mobile phase and the cooling pipeline 3, on one hand, and improve the heat transfer performance between the mobile phase and the cooling pipeline 3; on the other hand, the problem of chromatographic peak broadening caused by uneven distribution of the substances to be detected close to and far from the inner wall of the pipeline can be relieved.
Further, a radiator 4 capable of cooling the substance to be detected in the cooling line 3 is provided outside the cooling line 3. In the present embodiment, the heat sink 4 is a heat sink attached to the outer wall surface of the cooling line 3, and includes a heat dissipation plate 41 having a shape matching the outer wall shape of the cooling line 3, and the heat dissipation plate 41 is closely attached to the outer wall surface of the cooling line 3. In the present embodiment, the heat radiation plate 41 is a copper plate, has excellent heat conductivity, and can effectively conduct the heat accumulated in the cooling line 3 to the external environment, thereby improving the heat radiation effect of the heat sink 4.
In this embodiment, the heat sink 4 further includes a plurality of heat dissipation fins 42 fixedly disposed on the surface of the heat dissipation plate 41, and the heat dissipation fins 42 are perpendicular to the surface of the heat dissipation plate 41 and extend toward the same side of the heat dissipation plate 41. The heat radiation fins 42 can effectively increase the contact area between the heat sink 4 and the external environment, and further improve the heat radiation effect of the heat sink 4. In other embodiments of the present invention, the heat dissipating fins 42 may be disposed on the surface of the cooling pipeline 3, and directly contact with the cooling pipeline 3 to be used as the heat sink 4. The angle of installation of the heat dissipating fins 42 is not limited to the vertical installation in the present embodiment, and may be inclined at a certain angle to the surface of the cooling line 3.
In some embodiments of the present invention, in order to further increase the heat dissipation efficiency of the cooling pipeline 3 per unit length, a side surface of the heat dissipation plate 41 away from the cooling pipeline 3 can be further configured to be disposed against a housing (not shown in the figure) of the derivative device, so as to conduct the heat generated by the cooling pipeline 3 to the housing with a relatively large contact area between the derivative device and the external environment, and rapidly dissipate the heat.
In this way, the cooling pipeline 3 of the derivative device provided by the embodiment has high cooling efficiency, and the mobile phase in the derivative device can be cooled to a temperature range acceptable by the detector 5 through the shorter cooling pipeline 3; meanwhile, the problem of chromatographic peak broadening caused by diffusion can be relieved by the shorter cooling pipeline 3, so that a chromatograph can obtain an analysis spectrogram with higher resolution.
In addition, in the present embodiment, one end of the cooling pipeline 3 is communicated with the end of the derivative pipeline 20, and the other end can be directly communicated with the sample inlet 50 of the detector 5 or other suitable components, and the connection manner can avoid using a long cooling pipeline 3 to ensure the cooling effect, thereby alleviating the problem of chromatographic peak broadening caused by diffusion.
The utility model also provides an use the high performance liquid chromatograph of above-mentioned device of deriving, during the installation device of deriving, only need to be connected the first pipeline 11 of device of deriving with high performance liquid chromatograph's chromatographic column, and communicate cooling line 3's directness and chromatograph detector 5's introduction port 50, can accomplish the antithetical couplet of device of deriving and chromatograph, the installation is simple and convenient.
Second embodiment
The second embodiment of the present invention provides a derivative device, which is slightly changed based on the first embodiment, and the parts not specifically illustrated include the same reference numerals and text descriptions as the first embodiment, and are not repeated herein.
the main change of the second embodiment over the first embodiment is that in the second embodiment, the radiator 4 for cooling the substance to be detected in the cooling duct 3 by the derivative device is a liquid cooling device disposed outside the cooling duct 3. The liquid cooling device comprises a radiating pipe sleeved on the outer side of the cooling pipeline 3, cooling liquid is filled in the radiating pipe, and the liquid cooling device can utilize a pump to enable the cooling liquid in the radiating pipe to circulate and continuously absorb heat on the surface of the cooling pipeline 3, so that a substance to be detected in the cooling pipeline 3 is helped to dissipate heat.
In this embodiment, the liquid cooling device adopts forced circulation mode help cooling tube 3 heat dissipation the utility model discloses an among the other embodiments, the liquid cooling device also can be configured into natural circulation's radiating mode, utilizes the density difference formation natural circulation's liquid stream after the liquid is heated in the radiator pipe, with the heat transfer on 3 surfaces of cooling tube to easily radiating position, improves the radiating effect.
In some embodiments, the heat dissipation pipe and the cooling pipeline 3 can also be indirectly contacted through the liquid cooling jacket, and the liquid cooling jacket can be processed according to the shapes of the heat dissipation pipe and the cooling pipeline 3, so that the heat dissipation pipe and the cooling pipeline 3 can be conveniently attached and fixed, and the heat transfer performance is improved.
Through the way, the derivative device provided by the embodiment adopts the liquid cooling device to cool the surface of the cooling pipeline 3, the cooling performance is excellent, the heat dissipation performance of the cooling pipeline 3 in unit length can be effectively improved, the chromatographic peak broadening is reduced, and the spectrogram resolution is improved. In addition, the noise and the jitter of the liquid cooling device are small, and when the liquid cooling device is used in combination with a chromatograph, the stability of measurement of the detector 5 coupled with the liquid cooling device can be effectively improved.
Third embodiment
The third embodiment of the present invention provides a derivation apparatus, which is slightly changed based on the first embodiment, and the parts not specifically illustrated include the same reference numerals and text descriptions as the first embodiment, and are not repeated herein.
The main variation of the third embodiment with respect to the first embodiment is that in the third embodiment, the heat sink 4 for cooling the substance to be detected in the cooling duct 3 is an air cooling device disposed outside the cooling duct 3. This air cooling device can blow the surface of cooling duct 3 continuously including setting up the fan in the cooling duct 3 outside, provides stable cooling air current to cooling duct 3 surface, constantly takes away the heat from cooling duct 3 surface, and the inside material that detects of help cooling duct 3 cools off.
The utility model discloses an in some embodiments, the air cooling device also can use with the radiating piece cooperation among the embodiment one, and the radiating fin of radiating piece has higher specific surface area, uses the air cooling device to blow to the radiating piece that has radiating fin, can reduce the surface temperature of radiating piece rapidly, improves cooling tube 3's heat dispersion effectively.
Embodiment IV
The fourth embodiment of the present invention provides a derivation apparatus, which is slightly changed based on the first embodiment, and the parts not specifically illustrated include the same reference numerals and text descriptions as the first embodiment, and are not repeated herein.
Fourth embodiment a main change of the first embodiment is that, in the fourth embodiment, the heat sink 4 for cooling the substance to be detected in the cooling pipeline 3 by the derivative device is a high-emissivity coating coated on the surface of the cooling pipeline 3, and the high-emissivity coating enhances the heat dissipation performance of the cooling pipeline by improving the infrared radiation efficiency of the surface of the cooling pipeline.
The heat dissipation performance of the cooling pipeline 3 is improved in a coating mode, the implementation is simple and convenient, and the cost is low. In addition, in the present embodiment, the cooling duct 3 is disposed inside the housing of the derivative device, and the absorption of the high-radiation coating with high blackness to the external radiation can be reduced, thereby further improving the heat dissipation effect of the cooling duct 3.
So far, the technical solution of the present invention has been described with reference to the accompanying drawings, but it is easily understood by those skilled in the art that the scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, a person skilled in the art can make equivalent changes or substitutions to the related technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.
Claims (10)
1. A derivative device, comprising:
The device comprises a reactor and a control unit, wherein the reactor is provided with a derivative pipeline and a heating unit coupled with the derivative pipeline, and the heating unit can heat a substance to be detected in the derivative pipeline;
A cooling pipeline which is communicated with the derived pipeline and is used for the substance to be detected in the derived pipeline to flow in,
Characterized in that the derivation device also comprises
The radiator is arranged on the outer side of the cooling pipeline and can cool the substance to be detected in the cooling pipeline.
2. The derivative device of claim 1, wherein said heat sink is a heat sink attached to a surface of said cooling circuit.
3. The derivative device of claim 1, wherein said heat sink is an air-cooled device capable of providing an air flow to said cooling circuit surface.
4. The derivative device of claim 1 wherein said heat sink is a liquid cooling device coupled to a surface of said cooling conduit.
5. The derivative device according to any one of claims 1 to 4, wherein said cooling circuit is made of: one or more of stainless steel, copper, aluminum, polyether-ether-ketone, high-density polyethylene and nylon.
6. The derivatization device according to any one of claims 1 to 4, wherein the cooling line further comprises a porous structure inside the cooling line.
7. The derivative device of claim 2, wherein said heat sink further comprises a plurality of heat dissipating fins disposed obliquely or perpendicularly to said cooling circuit.
8. Derivative as claimed in claim 2, characterized in that a side of the heat sink facing away from the cooling circuit is arranged in attachment with a housing of the derivative.
9. the derivatization device of any one of claims 1-4, 7, and 8, wherein the derivatization device is a post-column derivatization device for chromatography.
10. A chromatograph having a derivative device according to any of claims 1-9.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201920244794.4U CN209784277U (en) | 2019-02-26 | 2019-02-26 | Derivative device and chromatograph with same |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201920244794.4U CN209784277U (en) | 2019-02-26 | 2019-02-26 | Derivative device and chromatograph with same |
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| CN209784277U true CN209784277U (en) | 2019-12-13 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115112813A (en) * | 2021-08-13 | 2022-09-27 | 深圳德谱仪器有限公司 | Nozzle for chromatograph |
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2019
- 2019-02-26 CN CN201920244794.4U patent/CN209784277U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115112813A (en) * | 2021-08-13 | 2022-09-27 | 深圳德谱仪器有限公司 | Nozzle for chromatograph |
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