CN112834668B - Low-temperature control device for analyzing hydrogen isotopes by gas chromatography - Google Patents
Low-temperature control device for analyzing hydrogen isotopes by gas chromatography Download PDFInfo
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- CN112834668B CN112834668B CN202011620744.5A CN202011620744A CN112834668B CN 112834668 B CN112834668 B CN 112834668B CN 202011620744 A CN202011620744 A CN 202011620744A CN 112834668 B CN112834668 B CN 112834668B
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- chromatographic column
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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
- G01N30/50—Conditioning of the sorbent material or stationary liquid
- G01N30/52—Physical parameters
- G01N30/54—Temperature
Abstract
The invention relates to a low-temperature control device for analyzing hydrogen isotopes by gas chromatography, which comprises a refrigeration mechanism, a cold head kit, a chromatographic column and a chromatograph; the chromatograph is connected with the chromatographic column; the cold head of the refrigerating mechanism is connected with the chromatographic column to provide a cold source; the chromatographic column is used for separating gas components; the chromatography column is mounted in the cold head kit. The invention has the following beneficial effects: the low-temperature control device for analyzing the hydrogen isotope by the gas chromatography adopts the structure of the cold head, the chromatographic column and the connecting pipe of the pulse tube type refrigerator, the pulse tube type refrigerator provides a cold source, and a low heat leakage mode is maintained under vacuum, the temperature of the chromatographic column can be set to be within a range of 40K-room temperature through the controller, liquid nitrogen does not need to be supplemented, and the possibility is provided for automatic control of the ash gas analysis process. Meanwhile, the temperature is adjusted within the range of 40K-room temperature, so that the possibility is provided for the optimization of chromatographic conditions of hydrogen isotope analysis.
Description
Technical Field
The invention belongs to the field of hydrogen isotope analysis, and particularly relates to a low-temperature control device for analyzing hydrogen isotopes by gas chromatography.
Background
Analysis of hydrogen isotopes by gas chromatography is widely used in the ash emission measurement of ITER. One key factor in chromatographic quantitation is the column temperature.
Whereas the hydrogen isotope component needs to be separated at a low temperature. At present, the technical scheme that the column temperature is increased by adopting a column temperature box to keep the column temperature stable in the prior art cannot meet the low-temperature requirement of hydrogen isotope component separation. For this reason, the art generally adopts a method of placing a chromatographic column in a self-made liquid nitrogen container, and providing a low temperature environment and separation by soaking the chromatographic column with liquid nitrogen.
However, in the analysis process, the liquid level of the liquid nitrogen changes due to factors such as volatilization of the liquid nitrogen, heat transfer of air flow and the like, and the liquid level change can cause column temperature change of a chromatographic column, so that the reproducibility of a quantitative result is poor, the reproducibility is usually maintained by a method of manual liquid level monitoring and timely replenishment, the operation is complicated, and program control is not easy to realize; and the separation temperature is limited to the liquid nitrogen temperature and cannot be adjusted, so that the optimization of the column temperature condition is limited.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the low-temperature control device for analyzing the hydrogen isotope by the gas chromatography.
The technical scheme of the invention is as follows:
a low-temperature control device for analyzing hydrogen isotopes by gas chromatography comprises a refrigeration mechanism, a cold head kit, a chromatographic column and a chromatograph; the chromatograph is connected with the chromatographic column; the cold head of the refrigerating mechanism is connected with the chromatographic column to provide a cold source; the chromatographic column is used for separating gas components; the chromatography column is mounted in the cold head kit.
Further, the low-temperature control device for analyzing the hydrogen isotopes by gas chromatography also comprises a vacuum structure; the vacuum structure comprises a vacuum chamber and a vacuum pump; the chromatography column and cold head kit are disposed in the vacuum chamber to provide reduced heat leakage.
Further, in the above-mentioned low-temperature control apparatus for gas chromatography of hydrogen isotopes, the vacuum pump is connected to the vacuum chamber through a bellows.
Further, in the above low temperature control device for gas chromatography analysis of hydrogen isotopes, an isolation valve is disposed on a pipeline between the vacuum chamber and the vacuum pump.
Further, in the above low temperature control device for gas chromatography analysis of hydrogen isotopes, the vacuum chamber is provided with a purge valve.
Further, in the above cryogenic control device for gas chromatography of hydrogen isotopes, the chromatographic column is connected to the chromatograph through a connecting pipe; the two connecting pipes are respectively connected with a sample introduction system and a detector of the chromatograph.
Further, in the low temperature control apparatus for gas chromatography of hydrogen isotopes, the connecting pipe is made of stainless steel pipe material, and the diameter of the connecting pipe is the same as that of the chromatographic column.
Further, in the above cryogenic control device for gas chromatography analysis of hydrogen isotopes, the chromatographic column and the connecting pipe are connected by a metal joint.
Further, in the low-temperature control device for analyzing the hydrogen isotope by the gas chromatography, the cold head sleeve is a sleeve made of an oxygen-free copper material.
Further, the above mentioned low temperature control device for gas chromatography analysis of hydrogen isotopes, the refrigeration mechanism comprises a water chiller and a refrigerator; the water chiller is connected with the refrigerator through a pipeline.
The invention has the following beneficial effects:
the low-temperature control device for analyzing the hydrogen isotope by the gas chromatography adopts the structure of the cold head, the chromatographic column and the connecting pipe of the pulse tube type refrigerator, the pulse tube type refrigerator provides a cold source, and a low heat leakage mode is maintained under vacuum, the temperature of the chromatographic column can be set to be within a range of 40K-room temperature through the controller, liquid nitrogen does not need to be supplemented, and the possibility is provided for automatic control of the ash gas analysis process. Meanwhile, the temperature is adjusted within the range of 40K-room temperature, and the possibility is provided for the optimization of chromatographic conditions of hydrogen isotope analysis.
Drawings
Fig. 1 is a schematic structural view of a low-temperature control apparatus for analyzing hydrogen isotopes by gas chromatography according to the present invention.
In the above drawings, 1, a vacuum pump; 2. an isolation valve; 3. a vacuum chamber; 4. a refrigerator; 5. a cold head kit; 6. a chromatographic column; 7. a chromatograph; 8. a connecting pipe; 9. a water cooling machine.
Detailed Description
The invention is described in detail below with reference to the figures and examples.
As shown in fig. 1, the present invention provides a low temperature control apparatus for analyzing hydrogen isotopes by gas chromatography, comprising a refrigeration mechanism, a cold head kit 5, a chromatographic column 6 and a chromatograph 7; the chromatograph 7 is connected with the chromatographic column 6; the cold head of the refrigerating mechanism is connected with the chromatographic column 6 to provide a cold source; the chromatographic column 6 is used for separating gas components; the chromatography column 6 is mounted in the coldhead kit 5.
The invention also includes a vacuum structure; the vacuum structure comprises a vacuum chamber 3 and a vacuum pump 1; the chromatography column 6 and cold head kit 5 are arranged in the vacuum chamber 3 to provide reduced heat leakage. The vacuum pump 1 is connected to a vacuum chamber 3 through a bellows. An isolating valve 2 is arranged on a pipeline between the vacuum chamber 3 and the vacuum pump 1. The vacuum chamber 3 is also provided with a deflation valve, which is convenient for relieving the vacuum state of the vacuum chamber 3.
The chromatographic column 6 is connected with a chromatograph 7 through a connecting pipe 8; the two connecting pipes 8 are respectively connected with the sample introduction system and the detector of the chromatograph 7. The connecting pipe 8 is made of stainless steel pipe material, and the column diameter is the same as that of the chromatographic column 6. The chromatographic column 6 and the connecting pipe 8 are connected through a metal joint. The cold head external member 5 is a sleeve made of an oxygen-free copper material, and the size of the sleeve is determined according to the diameter of the chromatographic column 6. The refrigerating mechanism comprises a water chiller 9 and a refrigerator 4 (a pulse tube refrigerator in the embodiment); the water chiller 9 is connected with the refrigerator 4 through a pipeline.
The invention provides a cold source through the pulse tube type refrigerator and provides vacuum through the vacuum pump 1, so that the vacuum chamber 3 and the chromatographic column 6 can maintain lower heat leakage; the cold head kit 5 made of the oxygen-free copper material has fast heat conduction, the size is designed according to the ring diameter requirement of the chromatographic column 6, and the sleeve structure ensures that the chromatographic column 6 is wholly in a low-temperature constant-temperature state. The vacuum chamber 3 can be designed and processed according to the sizes of the chromatographic column 6 and the cold head kit 5, and is easy to weld and process by adopting stainless steel materials, and the vacuum degree is ensured.
The low-temperature control device for analyzing the hydrogen isotopes by the gas chromatography adopts the structure of the cold head, the chromatographic column 6 and the connecting pipe 8 of the pulse tube type refrigerator, the pulse tube type refrigerator provides a cold source and maintains a low heat leakage mode under vacuum, the temperature of the chromatographic column 6 can be set to be within a 40K-room temperature range by the controller, liquid nitrogen does not need to be supplemented, and the possibility is provided for automatic control of the ash discharge gas analysis process. Meanwhile, the temperature is adjusted within the range of 40K-room temperature, so that the possibility is provided for the optimization of chromatographic conditions of hydrogen isotope analysis.
The temperature control device of the embodiment of the invention is adopted to measure a certain hydrogen isotope sample, and the main measuring process is as follows:
the (first) chromatographic column 6 is installed. The chromatography column 6 is wound onto the cold head, the two end joints are connected with the connecting pipe 8, the cold head kit 5 is installed, and then the vacuum chamber 3 is installed. The other end of the connecting pipe 8 is connected with a sample introduction system and a detector of the gas chromatograph.
(II) vacuumizing: starting the vacuum pump 1 and opening a gas valve of the vacuum system to pump the vacuum degree in the vacuum chamber 3 to a set value and keep the vacuum degree constant.
(III) boiling water cooler: and (4) opening the water cooling machine to ensure that the water circulation system of the refrigerating machine 4 works normally.
(IV) turning on a refrigerator: the controller of the refrigerator 4 is turned on, the temperature control value is set, and the refrigerator 4 is started.
(V) chromatographic measurement: and starting a gas chromatograph to measure the hydrogen isotope sample.
The application result shows that: the temperature control device has the advantages of high temperature control precision, stable temperature, wide controllable temperature range, simple structure, convenient use, no need of supplementing liquid nitrogen and the like, and has wide application prospect in hydrogen isotope chromatographic analysis and other occasions requiring precise temperature control.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is intended to include such modifications and variations.
Claims (7)
1. A low-temperature control device for analyzing hydrogen isotopes by gas chromatography is characterized by comprising a refrigerating mechanism, a cold head kit, a chromatographic column and a chromatograph; the chromatograph is connected with the chromatographic column; the cold head of the refrigerating mechanism is connected with the chromatographic column to provide a cold source; the chromatographic column is used for separating gas components; the chromatography column is mounted in the cold head kit;
the refrigerating mechanism comprises a water chiller and a refrigerator, and the water chiller is connected with the refrigerator through a pipeline;
further comprising a vacuum structure comprising a vacuum chamber and a vacuum pump, the chromatography column and coldhead kit being disposed in the vacuum chamber to provide reduced heat leakage;
the refrigerator is a pulse tube type refrigerator, and the cold head sleeve is a sleeve made of an oxygen-free copper material.
2. The cryogenic control device for analyzing hydrogen isotopes by gas chromatography as claimed in claim 1, wherein the vacuum pump is connected to the vacuum chamber through a bellows.
3. The cryogenic control device for analyzing hydrogen isotopes by gas chromatography as claimed in claim 1, wherein an isolation valve is provided on a pipe between the vacuum chamber and the vacuum pump.
4. The cryogenic control device for analyzing hydrogen isotopes by gas chromatography as claimed in claim 1, wherein a purge valve is provided on the vacuum chamber.
5. The cryogenic control device for analyzing hydrogen isotopes by gas chromatography as claimed in claim 1, wherein the chromatographic column is connected to a chromatograph through a connecting tube; the two connecting pipes are respectively connected with a sample introduction system and a detector of the chromatograph.
6. The cryogenic control device for analyzing hydrogen isotopes by gas chromatography as claimed in claim 5, wherein the connecting tube is made of stainless steel tubing and has the same column diameter as the chromatographic column.
7. The cryogenic control device for analyzing hydrogen isotopes by gas chromatography as claimed in claim 5, wherein the chromatographic column and the connecting pipe are connected by a metal joint.
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| CN202011620744.5A CN112834668B (en) | 2020-12-30 | 2020-12-30 | Low-temperature control device for analyzing hydrogen isotopes by gas chromatography |
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