阅读说明：本技术 一种用于气相色谱分析法分析氢同位素的低温控制装置 (Low-temperature control device for analyzing hydrogen isotopes by gas chromatography ) 是由 任英 武超 胡石林 吕卫星 李乐斌 刘丽飞 刘艳 于 2020-12-30 设计创作，主要内容包括：本发明涉及一种用于气相色谱法分析氢同位素的低温控制装置,包括制冷机构、冷头套件、色谱柱和色谱仪；所述色谱仪与所述色谱柱连接；所述制冷机构的冷头与所述色谱柱连接以提供冷源；所述色谱柱进行气体组分分离；所述色谱柱安装在所述冷头套件中。本发明的有益效果如下：本发明的气相色谱法分析氢同位素的低温控制装置采用脉管式制冷机的冷头、色谱柱、连接管的结构,通过脉管式制冷机提供冷源、在真空下维持较低漏热的方式,通过控制器可将色谱柱温度设置为40K-室温范围内,无需补充液氮,为排灰气分析过程的自动化控制提供了可能性。同时在40K-室温范围内进行温度调节,为氢同位素分析的色谱条件优化提供可能性。(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, and the possibility is provided for the optimization of chromatographic conditions of hydrogen isotope analysis.)

1. A low-temperature control device for analyzing hydrogen isotopes by gas chromatography is characterized by comprising 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.

2. The cryogenic control device for gas chromatography of hydrogen isotopes as claimed in claim 1, further comprising 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.

3. The cryogenic control device for gas chromatography of hydrogen isotopes as claimed in claim 2, wherein the vacuum pump is connected to the vacuum chamber by a bellows.

4. The cryogenic control device for gas chromatography of hydrogen isotopes as claimed in claim 2, wherein an isolation valve is provided on a pipe between the vacuum chamber and the vacuum pump.

5. The cryogenic control device for gas chromatography of hydrogen isotopes as claimed in claim 2, wherein a purge valve is provided on the vacuum chamber.

6. The cryogenic control device for gas chromatography of hydrogen isotopes as claimed in claim 2, wherein the chromatographic column is connected to a chromatograph by a connecting tube; the two connecting pipes are respectively connected with a sample introduction system and a detector of the chromatograph.

7. The cryogenic control device for gas chromatography of hydrogen isotopes as claimed in claim 6, wherein the connecting tube is made of stainless steel tubing and has the same column diameter as the chromatographic column.

8. The cryogenic control device for gas chromatography of hydrogen isotopes as claimed in claim 6, wherein the chromatographic column and the connecting tube are connected by a metal joint.

9. The cryogenic control device for gas chromatography of hydrogen isotopes as claimed in any one of claims 1 to 8, wherein the coldhead kit is a sleeve of oxygen-free copper material.

10. A cryogenic control device for gas chromatography of hydrogen isotopes as claimed in any one of claims 1 to 8, wherein the refrigeration mechanism comprises a water chiller and a refrigerator; the water chiller is connected with the refrigerator through a pipeline.

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 ite ash gas measurement processes. 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 isotope by the 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 analyzing hydrogen isotopes by gas chromatography, an isolation valve is disposed on a pipeline between the vacuum chamber and the vacuum pump.

Further, in the low-temperature control device for analyzing hydrogen isotopes by gas chromatography, the vacuum chamber is provided with a gas release valve.

Further, in the above cryogenic control device for gas chromatography of hydrogen isotopes, 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.

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 gas component separation; 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. Still be provided with the bleed valve on the vacuum chamber 3, be convenient for relieve the vacuum state of 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 cold head external member 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 low 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, and 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, and pumping the vacuum degree in the vacuum chamber 3 to a set value and keeping 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) starting 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 the 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.