CN110632233A - Constant temperature chromatographic device - Google Patents
Constant temperature chromatographic device Download PDFInfo
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- CN110632233A CN110632233A CN201911018325.1A CN201911018325A CN110632233A CN 110632233 A CN110632233 A CN 110632233A CN 201911018325 A CN201911018325 A CN 201911018325A CN 110632233 A CN110632233 A CN 110632233A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/30—Control of physical parameters of the fluid carrier of temperature
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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Abstract
The invention provides a constant temperature chromatographic device, which comprises a temperature control device, a flow control device, a gas interface and a capillary gas chromatographic column, wherein the temperature control device is connected with the flow control device; the gas interface is a hollow tubular structure with a through hole, the capillary gas chromatographic columns are arranged in a surrounding way by taking the gas interface as a shaft, the input end of each capillary gas chromatographic column is connected with the flow control device, and the output end of each capillary gas chromatographic column penetrates through the through hole from one end of the gas interface; the temperature control device is respectively connected with the gas interface and the capillary gas chromatographic column and supplies a required temperature field for the gas interface and the capillary gas chromatographic column. According to the constant-temperature chromatographic device provided by the invention, the capillary gas chromatographic column and the gas interface are coaxially arranged, so that the volume of the whole device is greatly reduced, and the power consumption of the whole device is effectively controlled.
Description
Technical Field
The invention relates to the technical field of gas chromatography instruments, in particular to a constant-temperature chromatography device, and particularly relates to a simple constant-temperature chromatography device.
Background
Gas Chromatography Mass Spectrometer (Gas Chromatography Mass Spectrometer) is widely applied to the fields of environmental protection industry, electronic industry, textile industry, petrochemical industry, essence and flavor industry, pharmaceutical industry, agriculture, food safety and the like; analyzing organic pollutants in the environment (analyzing air, water quality and pollution in soil); analyzing pesticide residues, animal residues and medicine residues; analyzing aroma components of the essence and the spice; detection of harmful substances in the textile industry. Wherein the gas chromatography separates the components of the sample, which plays a role in sample preparation; the interface sends each component flowing out of the gas chromatography into a mass spectrometer for detection; the mass spectrometer analyzes each component introduced by the interface to become a detector of the gas chromatograph. The computer system controls the chromatograph, the interface and the mass spectrometer to acquire and process data.
Because the chromatographic column and the gas interface need to maintain a certain temperature or heat according to a certain program mode, and in a common chromatographic apparatus, the chromatographic column and the gas interface are separated, 2 sets of independent peripheral auxiliary heating and temperature control devices are needed to construct and maintain the temperature field required by the chromatographic column or the gas interface, which is relatively large in volume and power consumption. Another study is to integrate the chromatographic column and the gas interface into a flat plate, so that the volume of the flat plate is reduced greatly, but because the flat plate has a large surface area and is serious in heat dissipation, a heat preservation oven box built around the flat plate is still large to maintain a stable temperature field well, and meanwhile, the loss in the aspect of power consumption is relatively large. One important indicator is the uniformity of the temperature distribution of the column. Only the chromatographic column with uniform temperature distribution can ensure that the analysis result has high repeatability and precision every time, otherwise, retention time drift can be caused, and the phenomena of supercooling condensation and overheating decomposition of a sample at the local position of the chromatographic column can occur when the temperature distribution is serious.
Chinese patent publication No. CN103760284A discloses a chromatographic column heating device, which includes a chromatographic column, a heating module, a circulation fan, and a heat insulation box for accommodating the chromatographic column, the heating module, and the circulation fan, wherein the circulation fan is located between the chromatographic column and the heating module. The chromatographic column heating device provided by the technical scheme has large invalid power and large power consumption. In addition, the device is required to be insulated, and the whole device is large in size and is not suitable for portable instruments. When the device is used for programmed temperature rise operation, the temperature reduction is slow.
Disclosure of Invention
In view of the defects in the prior art, the invention aims to provide a constant temperature chromatographic device.
The constant temperature chromatographic device provided by the invention comprises a temperature control device, a flow control device, a gas interface and a capillary gas chromatographic column;
the gas interface is a hollow tubular structure with a through hole, the capillary gas chromatographic columns are arranged in a surrounding way by taking the gas interface as a shaft, the input ends of the capillary gas chromatographic columns are connected with the flow control device, and the output ends of the capillary gas chromatographic columns penetrate through the through hole from one end of the gas interface;
the temperature control device is respectively connected with the gas interface and the capillary gas chromatographic column and supplies a required temperature field for the gas interface and the capillary gas chromatographic column.
Preferably, the mass spectrometer further comprises a mass spectrometer, the other end of the gas interface is connected with the mass spectrometer, and the output end of the capillary gas chromatographic column penetrates through the through hole from one end of the gas interface and then enters the mass spectrometer.
Preferably, the other end of the gas interface is provided with a connecting nut, the gas interface is connected with the mass spectrometer through the connecting nut, and the interface is sealed through a graphite clamping sleeve;
the joint of the capillary gas chromatographic column and the gas interface is sealed by a graphite cutting sleeve.
Preferably, the capillary gas chromatographic column is provided with an insulating heating wire and a platinum wire temperature measuring device, the insulating heating wire is arranged along the length direction of the capillary gas chromatographic column or wound around the capillary gas chromatographic column as a shaft, and the insulating heating wire is connected with the temperature control device through a lead and provides a required temperature field for the capillary gas chromatographic column under the control of the temperature control device.
Preferably, the gas interface is a hollow stainless steel metal pipe, is connected with the temperature control device through a lead and keeps constant temperature under the control of the temperature control device; and a platinum wire temperature measuring device is arranged on the gas interface.
Preferably, the capillary gas chromatographic column is isolated from the gas interface through a heat-insulating layer, and the heat-insulating layer can ensure that the temperature fields of the capillary gas chromatographic column and the gas interface are independent and have no interference.
Preferably, the outer side of the capillary gas chromatographic column is wrapped with a heat preservation layer, and the heat preservation layer can insulate heat and ensure that the temperature field of the capillary gas chromatographic column is uniform.
Preferably, the heat-insulating layer is any one or more of quartz wool, heat-insulating foam, heat-insulating plastic, aerogel and an aluminized polyester film.
Preferably, the flow control device comprises a sample inlet and a quantitative ring;
the output of ration ring is connected with the input of capillary gas chromatographic column, and the input of ration ring is connected with the introduction port, is provided with cold brush head and hot brush head on the ration ring, and the ration ring can change self temperature through switching cold brush head and hot brush head.
Preferably, the flow control means is disposed on the axis of the gas mass interface.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the constant temperature chromatographic device provided by the invention, the gas mass interface and the capillary gas chromatographic column are coaxially arranged, so that the volume of the device is greatly reduced, and the whole device has a simple structure and is particularly suitable for portable instruments.
2. According to the constant-temperature chromatographic device provided by the invention, the temperature fields of the gas mass interface and the capillary gas chromatographic column are provided by a set of power supply and control unit, so that the control is flexible, and the power consumption is saved.
3. The constant-temperature chromatographic device provided by the invention adopts the heat-insulating layer such as the heat-insulating quartz wool to completely cover the gas interface and the capillary gas chromatographic column, has reliable temperature field and uniform distribution, and is favorable for ensuring the accuracy and the reproducibility of chromatographic separation.
4. The constant temperature chromatographic device provided by the invention has a compact structure, the temperature control device directly heats the capillary gas chromatographic column, the power consumption is low, the heating speed is high, when the temperature needs to be reduced, the power is directly cut off, and the capillary gas chromatographic column is only contacted with the environment through the heat insulation layer, so the temperature reduction speed is high.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic diagram of a simple structure of a conventional gas chromatograph-mass spectrometer.
Fig. 2 is a schematic structural diagram of the present invention.
FIG. 3 is a schematic cross-sectional view of a gas chromatography column of the present invention wound uniformly with the gas interface as the axis.
FIG. 4 is a graph comparing the actual power consumption of the present invention with the power consumption of a conventional chromatographic apparatus at different temperatures.
The figures show that:
201-mass spectrometer 205-quantitative ring 208-sample inlet
203-temperature control device 206-gas interface 209-insulating layer
204-flow control device 207-capillary gas chromatography column 210-through-hole
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
In the description of the present application, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience in describing the present application and simplifying the description, but do not indicate or imply that the referred device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present application.
The constant temperature chromatography device provided by the invention, as shown in fig. 2 to 3, comprises a temperature control device 203, a flow control device 204, a gas interface 206 and a capillary gas chromatography column 207; the gas interface 206 is a hollow tubular structure with a through hole 210, the capillary gas chromatography columns 207 are arranged around the gas interface 206 as a ring, the input ends of the capillary gas chromatography columns 207 are connected with the flow control device 204, and the output ends of the capillary gas chromatography columns pass through the through hole 210 from one end of the gas interface 206; the temperature control device 203 is respectively connected with the gas interface 206 and the capillary gas chromatography column 207 and supplies the required temperature fields for the gas interface 206 and the capillary gas chromatography column 207. The gas interface 206 and the capillary gas chromatographic column 207 are coaxially arranged, so that the volume of the device is greatly reduced, and the whole device has a simple structure and is particularly suitable for portable instruments. Preferably, the gas interface 206 is a hollow stainless steel metal tube. Preferably, the temperature control device 203 is a simple temperature control device.
The mass spectrometer 201 is further included, the other end of the gas mass interface 206 is connected with the mass spectrometer 201, and the output end of the capillary gas chromatography column 207 passes through the through hole 210 from one end of the gas mass interface 206 and then enters the mass spectrometer 201. The other end of the gas interface 206 is provided with a connecting nut, the gas interface 206 is connected with the mass spectrometer 201 through the connecting nut, and the interface is sealed through a graphite clamping sleeve; the connection between the capillary gas chromatography column 207 and the gas interface 206 is sealed by a graphite ferrule to ensure that the inside of the mass spectrometer 201 is in a vacuum environment.
The capillary gas chromatographic column 207 is provided with an insulating heating wire and a platinum wire temperature measuring device, the insulating heating wire is arranged along the length direction of the capillary gas chromatographic column 207 or is arranged around the capillary gas chromatographic column 207 by taking the capillary gas chromatographic column 207 as a shaft, and the insulating heating wire is connected with the temperature control device 203 through a lead and provides a required temperature field for the capillary gas chromatographic column 207 under the control of the temperature control device 203. The gas interface 206 is a hollow stainless steel metal pipe, and the gas interface 206 is connected with the temperature control device 203 through a lead and keeps constant temperature under the control of the temperature control device 203; and a platinum wire temperature measuring device is arranged on the gas interface 206. The capillary gas chromatographic column 207 and the gas interface 206 are isolated by an insulating layer 209, and the insulating layer can ensure that the temperature fields of the capillary gas chromatographic column 207 and the gas interface 206 are independent and have no interference. The outer side of the capillary gas chromatographic column 207 is wrapped with an insulating layer 209, and the insulating layer 209 can insulate heat and ensure that the temperature field of the capillary gas chromatographic column 207 is uniform. The heat-insulating layer 209 is any one or more of quartz wool, heat-insulating foam, heat-insulating plastic, aerogel and an aluminum-plated polyester film. Preferably, the diameter of the opening of the hollow stainless steel metal tube is 0.5-0.8 mm. The temperature fields of the gas interface 206 and the capillary gas chromatographic column 207 are provided by a set of power supply and control unit (namely the temperature control device 203), so that the control is flexible, and the power consumption is saved. The gas interface 206 and the capillary gas chromatographic column 207 are completely covered by the heat-insulating layer 209 such as heat-insulating quartz wool, and the temperature fields of the gas interface 206 and the capillary gas chromatographic column 207 are reliable and are uniformly distributed, so that the accuracy and the reproducibility of chromatographic separation can be ensured. Preferably, the thickness of the insulating layer 209 wrapped outside the gas interface 206 is about 3mm, and the thickness of the insulating layer wrapped outside the capillary gas chromatography column 207 is about 5 mm.
The flow control device 204 comprises a sample inlet 208 and a quantitative ring 205; the output end of the quantitative ring 205 is connected with the input end of the capillary gas chromatography column 207, the input end of the quantitative ring 205 is connected with the sample inlet 208, the quantitative ring 205 is provided with a cold brush head and a hot brush head, and the quantitative ring 205 can change the temperature thereof by switching the cold brush head and the hot brush head. The flow control device 204 is disposed on the axis of the gas-mass interface 206. The cold brush head is a cold electric brush, and the hot brush head is a hot electric brush.
Example (b):
as shown in fig. 2, the temperature control device 203 is connected to the gas interface 206 and the capillary gas chromatography column 207 of the constant temperature chromatography device through 2 wires, respectively, so as to precisely control the temperature thereof. The gas interface 206 and capillary gas chromatography column 207 are wound and distributed as shown in fig. 3, wherein an insulating layer 209 (e.g., quartz wool) plays a role in heat insulation. The gas phase portion of the sample inlet 208 is used to introduce a gas or liquid sample. In practice, the quantitative ring 205 is first switched to a cold brush head, the temperature of the cold brush head is controlled at-20 ℃, a gas sample is injected from the sample inlet 208 by an injector, and the sample is quenched, namely is completely stored in the quantitative ring 205, and the process lasts for a moment and plays a role in sample enrichment. For samples with lower concentration, the sensitivity of analysis can be effectively improved. After the enrichment process is completed, the sample injection is stopped and the dosing ring 205 is switched to the hot brush head. At this time, the gas sample enriched in the quantitative ring 205 rapidly expands upon heating and rapidly enters the capillary gas chromatography column 207. On the other hand, the temperature control device 203 controls the capillary gas chromatography column 207 to 50 ℃ in the initial low temperature state, and all the components are effectively adsorbed on the capillary gas chromatography column 207. Then the temperature of the capillary gas chromatographic column 207 is controlled to be raised by the temperature control device 203, and due to different boiling points of different components, when the boiling points of the different components are close to each other, the sample components are desorbed from the capillary gas chromatographic column 207 to realize component separation, and then enter the mass spectrometer 201 ion source through the through hole 210 of the gas mass interface 206 to perform subsequent mass spectrometry. In the separation and sample introduction process, the temperature control device 203 controls the gas interface 206 to always keep a higher constant temperature state.
Controlling the temperature of the gas interface 206 to be 200 ℃ and the initial low-temperature state of the capillary gas chromatographic column 207 to be 50 ℃, changing the temperature maintained by the high temperature of the capillary gas chromatographic column 207, and respectively measuring the power consumption comparison of the traditional chromatographic device and the device of the invention under different high-temperature working conditions, as shown in fig. 4, it can be seen that when the high temperature is low, the power consumption of the invention is only 10% of that of the traditional chromatographic device; the relative proportion of the high temperature section increases with increasing temperature, and the power consumption of the invention is 20% of that of the traditional chromatographic device when the temperature reaches 200 ℃. Therefore, the invention can greatly reduce the energy consumption of the whole chromatographic device.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.
Claims (10)
1. A constant temperature chromatography device, which is characterized by comprising a temperature control device (203), a flow control device (204), a gas interface (206) and a capillary gas chromatography column (207);
the gas interface (206) is a hollow tubular structure with a through hole (210), the capillary gas chromatographic columns (207) are arranged in a surrounding way by taking the gas interface (206) as a ring, the input ends of the capillary gas chromatographic columns (207) are connected with the flow control device (204), and the output ends of the capillary gas chromatographic columns penetrate through the through hole (210) from one end of the gas interface (206);
the temperature control device (203) is respectively connected with the gas interface (206) and the capillary gas chromatographic column (207) and supplies required temperature fields for the gas interface (206) and the capillary gas chromatographic column (207).
2. The constant-temperature chromatography device according to claim 1, further comprising a mass spectrometer (201), wherein the other end of the gas mass interface (206) is connected with the mass spectrometer (201), and the output end of the capillary gas chromatography column (207) passes through the through hole (210) from one end of the gas mass interface (206) and enters the mass spectrometer (201).
3. The constant-temperature chromatography device according to claim 2, wherein a connecting nut is arranged at the other end of the gas interface (206), the gas interface (206) is connected with the mass spectrometer (201) through the connecting nut, and the interface is sealed through a graphite ferrule;
the joint of the capillary gas chromatographic column (207) and the gas interface (206) is sealed by a graphite cutting sleeve.
4. The constant temperature chromatography device according to claim 1, wherein an insulating heating wire and a platinum wire temperature measuring device are arranged on the capillary gas chromatography column (207), the insulating heating wire is arranged along the length direction of the capillary gas chromatography column (207) or is wound around the capillary gas chromatography column (207), and the insulating heating wire is connected with the temperature control device (203) through a lead and provides a required temperature field for the capillary gas chromatography column (207) under the control of the temperature control device (203).
5. The isothermal chromatography device according to claim 1, wherein the gas interface (206) is a hollow stainless steel metal tube, and the gas interface (206) is connected with the temperature control device (203) through a lead and is kept at a constant temperature under the control of the temperature control device (203); and a platinum wire temperature measuring device is arranged on the gas interface (206).
6. The constant-temperature chromatography device according to claim 1, wherein the capillary gas chromatography column (207) is isolated from the gas interface (206) by an insulating layer (209), and the insulating layer can ensure that the temperature fields of the capillary gas chromatography column (207) and the gas interface (206) are independent and have no interference.
7. The constant-temperature chromatography device according to claim 1, wherein an insulating layer (209) is wrapped outside the capillary gas chromatography column (207), and the insulating layer (209) can insulate heat and ensure that the temperature field of the capillary gas chromatography column (207) is uniform.
8. The constant temperature chromatography device according to claim 6 or 7, wherein the heat-insulating layer (209) is any one or more of quartz wool, heat-insulating foam, heat-insulating plastic, aerogel and aluminized polyester film.
9. The stationary temperature chromatography device according to claim 1, wherein the flow control device (204) comprises a sample inlet (208), a quantification ring (205);
the output end of the quantitative ring (205) is connected with the input end of the capillary gas chromatographic column (207), the input end of the quantitative ring (205) is connected with the sample inlet (208), the quantitative ring (205) is provided with a cold brush head and a hot brush head, and the quantitative ring (205) can change the temperature of the quantitative ring through switching the cold brush head and the hot brush head.
10. The stationary temperature chromatography device according to claim 1, wherein the flow control device (204) is arranged on an axis on which the gas mass interface (206) is located.
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| CN201911018325.1A CN110632233A (en) | 2019-10-24 | 2019-10-24 | Constant temperature chromatographic device |
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| CN201911018325.1A CN110632233A (en) | 2019-10-24 | 2019-10-24 | Constant temperature chromatographic device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113804809A (en) * | 2021-09-26 | 2021-12-17 | 上海裕达实业有限公司 | Portable gas chromatography-mass spectrometer rapid temperature control device |
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Application publication date: 20191231 |