Gas chromatographic analysis system for trace impurities in high-purity krypton

By designing a gas chromatography analysis system in high-purity krypton gas and using switching valves to alternately use the intake pipe unit, the problem of too long detection time is solved, and fast and efficient trace impurity detection is achieved to meet industrial production needs.

CN222212696UActive Publication Date: 2024-12-20HENAN JUNDE GAS CO LTD
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Patent Information

Application Number
CN202420265135.X
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-02-02
Publication Date
2024-12-20
Estimated Expiration
2034-02-02

AI Technical Summary

Technical Problem

The detection time of trace impurities in high-purity krypton gas in the prior art is too long to meet the rapid detection needs of industrial production.

Method used

Design a gas chromatography analysis system for trace impurities in high-purity krypton. It adopts two sets of intake pipe units and switching valve VⅢ. It is connected to the DID detector through the switching valve, so as to realize the alternating use of the intake pipe units, saving gas phase sampling and division and push time to improve detection efficiency.

Benefits of technology

It realizes that when using the same DID detector, it shortens the detection time, improves the detection efficiency, and meets the rapid detection needs of industrial production. It has the characteristics of simplicity in operation, high accuracy and short analysis time.

✦ Generated by Eureka AI based on patent content.

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Abstract

The utility model relates to a gas chromatographic analysis system for trace impurities in high-purity krypton. Comprising two sets of air inlet pipeline units which are respectively connected with an analysis and detection pipeline unit; the analysis and detection pipeline unit comprises a switching valve VIII; the switching valve VIII is respectively connected with the two sets of gas inlet pipeline units and a DID detector for detecting trace impurities in high-purity krypton; the method has the characteristics that the operation is simple and convenient, the accuracy rate is high, the analysis time is short, multiple continuous sample injection can be realized, and trace impurities in the high-purity krypton gas can be rapidly detected so as to meet the industrial production requirements.
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Description

Technical Field

[0001] The utility model relates to the technical field of detecting trace impurities in high-purity krypton gas, in particular to a gas chromatography analysis system for detecting trace impurities in high-purity krypton. Background Art

[0002] High-purity gases play an important role in modern industry, among which high-purity krypton (Kr) is one of the most widely used high-purity gases, which can be widely used in special light sources, building energy conservation, medical treatment, electronics, aerospace, scientific research and national defense. Krypton can form clathrate inclusion compounds, such as using discharge, electron radiation, ultraviolet radiation and other methods; it is widely used in lighting, and can be used as a filling gas in advanced electron tubes or lamps. Krypton lamps also have the characteristics of energy saving, long service life and high luminous efficiency. Krypton gas is used in products such as off-road vehicle illumination lights, aircraft runway lights, high-pressure mercury lamps, sodium lamps, zirconium point light sources, flash lamps, stroboscopic observers, voltage tubes, counting discharge tubes and gas relays; it is also widely used in scientific research, medical treatment and other fields. Krypton gas can be used to fill ionization (ionization) chambers to measure high-energy rays (cosmic rays), and can also be used as a light-shielding material when X-rays are working. It can be used in gas lasers and plasma streams; liquid krypton can be used in the bubble chambers of particle detectors; radioactive isotopes of krypton can be used as tracers in medical applications; krypton can also be used to produce specialty flat glass for the solar, automotive and construction industries. Krypton is used in the glass coating process to create unique properties.

[0003] The detection of trace impurities in high-purity gases is mainly based on gas chromatography; the discharge helium ionization detector (DID detector for short) is a highly sensitive general-purpose detector. The use of pulsed discharge helium ionization chromatography to detect trace impurities in high-purity gases is a new method that has just been developed in recent years. It has the advantages of high sensitivity and low detection limit; but when there are many components to be detected, the analysis time is often more than half an hour. Due to the long analysis time, it cannot meet the needs of rapid detection in industrial production. Utility Model Content

[0004] The utility model aims to solve the defects in the prior art and provide a gas chromatography analysis system for trace impurities in high-purity krypton.

[0005] In order to achieve the above purpose, the utility model provides the following technical solutions:

[0006] A gas chromatography analysis system for trace impurities in high-purity krypton, comprising two sets of air intake pipeline units, which are respectively connected to analysis and detection pipeline units; the analysis and detection pipeline units comprise switching valves VIII, which are respectively connected to the two sets of air intake pipeline units and a DID detector for detecting trace impurities in high-purity krypton.

[0007] The beneficial effects of the utility model are as follows: the utility model uses a switching valve VⅢ so that one end of the switching valve is connected to two sets of air intake pipe units, and the other end is connected to a DID detector for detecting trace impurities in high-purity krypton; one set of air intake pipe units in the above arrangement cooperates with the DID detector to realize analysis and detection of the gas phase in the air intake pipe unit, and the other set of air intake pipe units divides the gas phase for standby; when the analysis and detection of the gas phase in the aforementioned set of air intake pipe units is completed, the switching valve VⅢ is used for conversion, so that the divided and standby gas phase in the other set of air intake pipe units is sent to the DID detector for analysis and detection through the switching valve VⅢ; in the above process, the time for gas phase sampling, division and pushing can be saved, so as to achieve the purpose of improving the detection efficiency under the premise of using the same DID detector.

[0008] Preferably, the switching valve VⅢ is a six-way purge pneumatic switching valve, interface No. ① in the switching valve VⅢ is connected to the first set of air intake pipeline units, interface No. ② in the switching valve VⅢ is connected to the first needle valve, interface No. ③ in the switching valve VⅢ is connected to the second set of air intake pipeline units, interface No. ④ in the switching valve VⅢ is connected to interface No. ⑥ in the switching valve VⅢ, and interface No. 5 in the switching valve VⅢ is connected to the DID detector.

[0009] Preferably, the first set of air inlet pipeline units includes a switching valve VI for taking sample gas, realizing sample gas pushing and pre-segmentation, and a switching valve VII for realizing sample gas pushing and sample gas segmentation. The switching valve VII is connected to the No. ① interface of the switching valve VIII through a second 5A molecular sieve chromatographic column.

[0010] Preferably, the switching valve VI is a ten-way purge pneumatic switching valve, interface No. ① in the switching valve VI is connected to the first sample gas inlet pipeline, interface No. ② in the switching valve VI is connected to the first sample gas outlet pipeline, a first quantitative loop is arranged between interface No. ③ in the switching valve VI and interface No. ⑩ in the switching valve VI, interface No. ④ in the switching valve VI is connected to the first carrier gas pipeline, a CILICA GEL column is arranged between interface No. ⑤ in the switching valve VI and interface No. ⑨ in the switching valve VI, interface No. ⑥ in the switching valve VI is connected to interface No. ① in the switching valve VI via a first 5A molecular sieve chromatographic column, interface No. ⑦ in the switching valve VI is connected to the second carrier gas pipeline, and interface No. ⑧ in the switching valve VI is connected to the second needle valve.

[0011] Preferably, the switching valve VⅡ is a six-way purge pneumatic switching valve, interface No. ② in the switching valve VⅡ is connected to interface No. ① in VⅢ through a second 5A molecular sieve chromatographic column, interface No. ③ in the switching valve VⅡ is connected to the third carrier gas pipeline, interface No. ④ in the switching valve VⅡ is connected to interface No. ⑥ in the switching valve VⅡ, and interface No. 5 in the switching valve VⅡ is connected to the third needle valve.

[0012] Preferably, the second set of air intake pipeline units includes a switching valve VIV for taking sample gas and pushing sample gas, and a switching valve VV for pushing sample gas and splitting sample gas. The switching valve VV is connected to the No. ③ interface of the switching valve VIII through the second Hayesep D column.

[0013] Preferably, the switching valve VIV is a six-way purge pneumatic switching valve, interface No. ⑥ in the switching valve VIV is connected to the second sample gas inlet pipeline, interface No. ① in the switching valve VIV is connected to the second sample gas outlet pipeline, a second quantitative loop is provided between interface No. ⑤ in the switching valve VIV and interface No. ② in the switching valve VIV, interface No. ④ in the switching valve VIV is connected to the fourth carrier gas pipeline, and interface No. ③ in the switching valve VIV is connected to interface No. ① in the switching valve VV through the first Hayesep D column.

[0014] Preferably, interface No. ② in the switching valve VⅤ is connected to interface No. ③ in the switching valve VⅢ through the second Hayesep D column, interface No. ③ in the switching valve VⅤ is connected to the fifth carrier gas pipeline, interface No. ④ in the switching valve VⅤ is connected to interface No. ⑥ in the switching valve VⅤ, and interface No. ⑤ in the switching valve VⅤ is connected to the fourth needle valve.

[0015] Preferably, the sample gas inlet pipeline is provided with an inlet quick-change joint, and the sample gas outlet pipeline is provided with an outlet quick-change joint; the sample gas outlet pipeline is also provided with a vacuum generator.

[0016] According to the above technical scheme, a gas chromatography analysis system for trace impurities in high-purity krypton is manufactured. By setting a switching valve VⅢ with a DID detector connected to two sets of air intake pipeline units, one of the two sets of air intake pipeline units cooperates with the DID detector to perform gas phase detection, and the other set is used for sampling, pushing and cutting the gas phase for standby, thereby achieving the characteristic of saving detection time under the premise of using the same DID detector; the utility model sets a first set of air intake pipeline units, which includes a switching valve VI for sampling gas, and The sample gas push and pre-segmentation are realized, and the switching valve VⅡ further pushes the sample gas and splits the sample gas, so as to facilitate the detection by the DID detector in the subsequent process; by setting a second set of air intake pipeline units, the second set of air intake pipeline units includes a switching valve VⅣ for taking sample gas and realizing sample gas push, and a switching valve VⅤ for realizing sample gas push and sample gas segmentation; it has the characteristics of simple operation, high accuracy, short analysis time, and the ability to realize multiple continuous sampling and quickly detect trace impurities in high-purity krypton gas to meet the needs of industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 It is a structural schematic diagram of the utility model.

[0018] Figure 2 This is a gas path diagram of the utility model switching valve VI taking samples to the first 5A molecular sieve chromatographic column, the second 5A molecular sieve chromatographic column and the SILICA GEL silica gel column and then to the detector.

[0019] Figure 3 This is the gas path diagram of the switching valve VⅡ of the utility model for venting the first main component Kr.

[0020] Figure 4 Gas path diagram for the utility model switching valve VIV to sample to the Hayesep D column and cut Xe, CF4, CO2, N2O, C2F6 to the detector.

[0021] Figure 5 This is a gas path diagram of the utility model in which the switching valves VⅣ and VⅤ are used to vent the main component in the second path.

[0022] In the figure:

[0023] 1. Switching valve VI; 2. Switching valve VII; 3. Switching valve VIII; 4. Switching valve VIV; 5. Switching valve VV; 6. First sample gas inlet pipeline; 7. First sample gas outlet pipeline; 8. First quantitative ring;

[0024] 9. The first carrier gas pipeline; 10. CILICA GEL column; 11. The first 5A molecular sieve chromatographic column; 12. The second carrier gas pipeline; 13. The second needle valve; 14. The second 5A molecular sieve chromatographic column; 15. The third carrier gas pipeline; 16. The third needle valve; 17. The second Hayesep D column; 18. The second sample gas inlet pipeline; 19. The second sample gas outlet pipeline; 20. The second quantitative loop; 21. The fourth carrier gas pipeline; 22. The first Hayesep D column; 23. The fifth carrier gas pipeline; 24. The fourth needle valve; 25. The inlet quick-change joint; 26. The outlet quick-change joint; 27. The vacuum generator; 28. The DID detector; 29. ​​The first needle valve. DETAILED DESCRIPTION

[0025] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments.

[0026] In the description of the present invention, it should be understood that the terms "upper", "lower", "front", "back", "left", "right", "top", "bottom", "inside", "outside", etc., indicating directions or positional relationships, are based on the directions or positional relationships shown in the accompanying drawings, and are only for the convenience of describing the present invention and simplifying the description, rather than indicating or implying that the device or element referred to must have a specific direction, be constructed and operated in a specific direction, and therefore should not be understood as a limitation on the present invention.

[0027] Reference Figure 1-5 The utility model is a gas chromatography analysis system for trace impurities in high-purity krypton, which includes two sets of air intake pipeline units, which are respectively connected to the analysis and detection pipeline units; the analysis and detection pipeline units include switching valves VⅢ3, which are respectively connected to the two sets of air intake pipeline units and the DID detector 28 for detecting trace impurities in high-purity krypton. The utility model sets two sets of air intake pipeline units to realize that one set of air intake pipeline units enters the DID detector 28 through the switching valve VⅢ3 for detection, and the other set of air intake pipeline units samples the sample gas, pushes and splits the sample gas, and places it outside the switching valve VⅢ3 for standby; when the above-mentioned air intake pipeline unit is detected, it is switched through the switching valve VⅢ3, so that the standby gas in the other set of air intake pipeline unit enters the DID detector 28 for detection. In the above process, the two sets of air intake pipeline units are alternately detected and standby, and the standby air intake pipeline unit is used to sample, push and cut the gas. The above process can save the above time and thus achieve the characteristic of saving detection time.

[0028] Further, the switching valve VⅢ3 is a six-way purge pneumatic switching valve, the No. ① interface of the switching valve VⅢ3 is connected to the first set of intake pipeline units, the No. ② interface of the switching valve VⅢ3 is connected to the first needle valve 29, the No. ③ interface of the switching valve VⅢ3 is connected to the second set of intake pipeline units, the No. ④ interface of the switching valve VⅢ3 is connected to the No. ⑥ interface of the switching valve VⅢ3, and the No. ⑤ interface of the switching valve VⅢ3 is connected to the DID detector 28. The utility model achieves the characteristic of detecting the gas phase by setting the switching valve VⅢ3 to be connected to the DID detector 28, and at the same time, the switching valve VⅢ3 is connected to two sets of intake pipeline units to switch the intake pipeline units, thereby realizing the purpose of saving detection time.

[0029] Furthermore, the first set of air inlet pipeline units includes a switching valve VⅠ1 for taking sample gas, realizing sample gas pushing and pre-segmentation, and a switching valve VⅡ2 for realizing sample gas pushing and sample gas segmentation. The switching valve VⅡ2 is connected to the interface No. ① in the switching valve VⅢ3 through the second 5A molecular sieve chromatographic column 14. The switching valve VⅠ1 is a ten-way purge pneumatic switching valve, wherein interface No. ① in the switching valve VⅠ1 is connected to the first sample gas inlet pipeline 6, interface No. ② in the switching valve VⅠ1 is connected to the first sample gas outlet pipeline 7, a first quantitative ring 8 is arranged between interface No. ③ in the switching valve VⅠ1 and interface No. ⑩ in the switching valve VⅠ1, interface No. ④ in the switching valve VⅠ1 is connected to the first carrier gas pipeline 9, a CILICA GEL column 10 is arranged between interface No. ⑤ in the switching valve VⅠ1 and interface No. ⑨ in the switching valve VⅠ1, interface No. ⑥ in the switching valve VⅠ1 is connected to interface No. ① in the switching valve VⅡ2 through a first 5A molecular sieve chromatographic column 11, interface No. ⑦ in the switching valve VⅠ1 is connected to the second carrier gas pipeline 12, and interface No. ⑧ in the switching valve VⅠ1 is connected to the second needle valve 13. The switching valve VⅡ2 is a six-way purge pneumatic switching valve, the interface No. ② in the switching valve VⅡ2 is connected to the interface No. ① in VⅢ3 through the second 5A molecular sieve chromatographic column 14, the interface No. ③ in the switching valve VⅡ2 is connected to the third carrier gas pipeline 15, the interface No. ④ in the switching valve VⅡ2 is connected to the interface No. ⑥ in the switching valve VⅡ2, and the interface No. ⑤ in the switching valve VⅡ2 is connected to the third needle valve 16. The first quantitative ring 8 can be provided to retain the injected gas, so as to achieve the purpose of chromatographic analysis of the gas phase of trace impurities in high-purity krypton gas by one injection; further, the utility model controls the gas flow rate through the carrier gas in the first carrier gas pipeline 9 and the second carrier gas pipeline 12, so as to drive the corresponding sample gas into the relevant chromatographic column and the switching valve. The sample gas injection and sampling are realized by setting the switching valve VI1, and the switching valve VI2 is used for cutting the sample gas and switching the carrier gas, etc. The utility model can be controlled manually or automatically, preferably automatically, that is, all the above actions are completed by the system reverse control chromatography workstation, each valve corresponds to an external event to control, and the order of its action is also executed by the event compilation program, the overall analysis process is automatically controlled, and the repeatability and accuracy of the system data are guaranteed by the stable flow gas path and accurate valve switching; the utility model uses a ten-way purge pneumatic switching valve and a six-way purge pneumatic switching valve, which have a short gas path stroke in the valve body compared to the four-way valve, and adopts a central cutting system to vent the main components to ensure a stable baseline; at the same time, the ten-way valve positive blowing method is adopted to make the gas path flow of the system change less after the valve body is switched; the needle valve in the utility model adopts a stainless steel regulating needle valve to control the venting flow; CILICA The GEL column 10, the first 5A molecular sieve chromatographic column 11 and the second 5A molecular sieve chromatographic column 14 all use independent column boxes, so that different chromatographic columns have the function of independent temperature control.

[0030] Furthermore, the second set of air inlet pipeline units includes a switching valve VIV4 for taking sample gas and pushing sample gas, and a switching valve VV5 for pushing sample gas and splitting sample gas. The switching valve VV5 is connected to the No. ③ interface of the switching valve VIII3 through the second Hayesep D column 17. The switching valve VIV4 is a six-way purge pneumatic switching valve. The No. ⑥ interface of the switching valve VIV4 is connected to the second sample gas inlet pipeline 18, the No. ① interface of the switching valve VIV4 is connected to the second sample gas outlet pipeline 19, a second quantitative ring 20 is provided between the No. ⑤ interface of the switching valve VIV4 and the No. ② interface of the switching valve VIV4, the No. ④ interface of the switching valve VIV4 is connected to the fourth carrier gas pipeline 21, and the No. ③ interface of the switching valve VIV4 is connected to the No. ① interface of the switching valve VV5 through the first Hayesep D column 22. The interface No. ② in the switching valve VⅤ5 is connected to the interface No. ③ in the switching valve VⅢ3 through the second Hayesep D column 17, the interface No. ③ in the switching valve VⅤ5 is connected to the fifth carrier gas pipeline 23, the interface No. ④ in the switching valve VⅤ5 is connected to the interface No. ⑥ in the switching valve VⅤ5, and the interface No. ⑤ in the switching valve VⅤ5 is connected to the fourth needle valve 24. The second quantitative ring 20 can be provided to retain the second gas phase injection gas, so as to achieve the purpose of chromatographic analysis of the gas phase of trace impurities in the high-purity krypton gas by one injection; further, the utility model controls the gas flow rate through the carrier gas in the fourth carrier gas pipeline 21 and the fifth carrier gas pipeline 23, so as to drive the corresponding sample gas into the relevant chromatographic column and the switching valve. The switching valve VⅣ4 is provided to realize the sample gas injection and sampling, and the switching valve VⅤ5 is used for cutting the sample gas and switching the carrier gas, etc. The utility model can be controlled manually or automatically, preferably automatically, that is, all the above actions are completed by the system reverse control chromatography workstation, each valve corresponds to an external event to control, and the order of its action is also executed by the event compilation program, the overall analysis process is automatically controlled, and the repeatability and accuracy of the system data are guaranteed by the stable flow gas path and accurate valve switching; the intake pipeline unit uses a six-way purge pneumatic switching valve, which has a short gas path stroke in the valve body compared to the four-way valve, and adopts a central cutting system to vent the main components to ensure a stable baseline; the needle valve in the utility model adopts a stainless steel regulating needle valve to control the venting flow; the first Hayesep D column 22 and the second Hayesep D column 17 both use independent column boxes, so that different chromatographic columns have the function of independent temperature control.In the utility model, a passage is formed by the first sample gas inlet pipeline 6, the first sample gas outlet pipeline 7, the second sample gas inlet pipeline 18 and the second sample gas outlet pipeline 19 to realize sampling of the sample gas, and the main gas and part of the trace impurities in the high-purity krypton gas are effectively separated by the first 5A molecular sieve chromatographic column 11, the second 5A molecular sieve chromatographic column 14, the CILICA GEL column 10 and the corresponding switching valve, and part of the trace impurities are sent to the DID detector 19 for detection by the corresponding carrier gas while the main gas is sent out, so as to avoid the main gas affecting the first 5A molecular sieve chromatographic column 11 and the CILICA GEL column 10 and causing the defect of a long time interval between two analyses; the main gas and another part of the trace impurities in the high-purity krypton gas are separated by the first Hayesep D column 22, the second Hayesep D column 17 and the corresponding switching valve, so as to realize the detection of the other part of the trace impurities.

[0031] Furthermore, the sample gas inlet pipeline is provided with an inlet quick-change joint 25, and the sample gas outlet pipeline is provided with an outlet quick-change joint 26; the sample gas outlet pipeline is also provided with a vacuum generator 27. The inlet quick-change joint 25 and the outlet quick-change joint 26 can facilitate the rapid connection of production equipment and / or storage equipment, so as to achieve the purpose of rapid and industrialized effective detection of trace impurity gas phase in high-purity krypton; the vacuum generator 27 can achieve rapid emptying of the sample gas after analysis, so that the baseline can be quickly restored to a stable state, and the analysis time can be reduced.

[0032] The working principle of the utility model is as follows: the utility model detects the trace impurity gas phase in high-purity krypton in a double-injection method of sample gas. First, the sample gas is collected through the switching valve VI1. Figure 1 As shown, the sample gas production equipment and / or storage equipment is connected to the first sample gas inlet pipeline 6 in the switching valve VI1, and the sample gas in the sample gas production equipment and / or storage equipment passes through the No. ① interface in the switching valve VI1, the No. ③ interface in the switching valve VI1, the first quantitative loop 8, the No. ⑩ interface in the switching valve VI1 and the first sample gas outlet pipeline 7 to form a passage, so that the product exists in the first quantitative loop 8; when the above sampling is completed, the sampling starts, as shown in FIG. Figure 2As shown, during one injection process, the main component is pre-cut and separated into H2, O2+Ar, N2, CH4, CO, and Kr components when entering the CILICA GEL column 10 in the switching valve VI1, and the gas is cut when passing through the first 5A molecular sieve chromatographic column 11 and the second 5A molecular sieve chromatographic column 14, and H2, O2+Ar, N2, CH4, and CO are switched to the DID detector 28 through the switching valve VIII3 to respond to the peak; the specific steps are as follows: the switching valve VI1 is connected to the pipeline in a forward injection mode, and the carrier gas in the first carrier gas pipeline 9 transports the sample gas in the first quantitative loop 8 to the CILICA GEL column 10, and the sample gas is pre-cut. When the sample gas passes through the CILICA GEL column 10, Kr is The peaks on the GEL column 10 emerge slowly, and H2, O2+Ar, N2, and CH4 enter the first 5A molecular sieve chromatographic column 11 first; further, the gas is cut by the switching valve VⅡ2, and the main krypton gas after cutting is vented through the first needle valve 16 (most of the main peak is vented), and at the same time, the carrier gas in the third carrier gas pipeline 15 drives the impurity components through the second 5A molecular sieve chromatographic column 14 and is sent to the DID detector 28 connected to the switching valve VⅢ3 for detection; in the above process, the carrier gas in the first carrier gas pipeline 9 and the carrier gas in the third carrier gas pipeline 15 have the same flow rate, keeping the baseline stable, and the impurity components emerge on the baseline, thereby improving the sensitivity of component detection; the order of the impurity components when passing through the second 5A molecular sieve chromatographic column 14 is H2, O2+Ar, N2, CH4, CO; the intake process of the second set of intake pipeline units is: Figure 1 As shown, the sample gas production equipment and / or storage equipment is connected to the second sample gas inlet pipeline 18, and the sample gas in the sample gas production equipment and / or storage equipment forms a passage through the No. ⑥ interface in the switching valve VⅣ4, the No. ⑤ interface in the switching valve VⅣ4, the second quantitative loop 20, the No. ② interface in the switching valve VⅣ4 and the second sample gas outlet pipeline 19, so that the product exists in the second quantitative loop 20; when the above sampling is completed, the injection is started, and the main component of the second injection process enters the first Hayesep D column 22 in the switching valve VⅣ4, and the main component is released through the third needle valve 18 through the switching valve VⅤ5, and the separated CO2, N2O, C2F6, and Xe are carried by the carrier gas in the fifth carrier gas pipeline 23 through the second Hayesep D column 17 into the switching valve 3, and are switched into the DID detector 28 to respond to the peak; the specific steps are: as shown in FIG. Figure 4 As shown, the carrier gas in the fourth carrier gas pipeline 21 transports the sample gas in the second quantitative loop 26 to the first Hayesep D column 22 for separation, as shown in FIG. Figure 5As shown, the main component in the sample gas first enters the first Hayesep D column 22 and is discharged through the fourth needle valve 24 connected to the interface ⑤ in the switching valve VⅤ5; the switching valve VⅤ5 serves as the central cutter of the secondary injection, switching the CO2 and other components to the DID detector 28 for response peak. It should be noted that, Figure 1-4 As shown, after the gas detection passes through the corresponding pipeline, the corresponding carrier gas purges the corresponding pipeline to prevent the filler in the corresponding column from being deactivated and to evacuate the corresponding gas phase in the pipeline to facilitate subsequent detection.

[0033] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes within the technical scope disclosed by the present invention according to the technical scheme and the utility model concept of the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A gas chromatography analysis system for trace impurities in high-purity krypton, characterized in that: The gas chromatography analysis system comprises two sets of air intake pipeline units, which are respectively connected to the analysis and detection pipeline units; The analysis and detection pipeline unit comprises a switching valve VIII (3), and the switching valve VIII (3) is respectively connected to two sets of air intake pipeline units and a DID detector (28) for detecting trace impurities in high-purity krypton.

2. A gas chromatography analysis system for trace impurities in high-purity krypton according to claim 1, characterized in that: The switching valve VIII (3) is a six-way purge pneumatic switching valve. Interface No. 1 in the switching valve VⅢ (3) is connected to the first set of intake pipe units, interface No. 2 in the switching valve VⅢ (3) is connected to the first needle valve (29), interface No. 3 in the switching valve VⅢ (3) is connected to the second set of intake pipe units, interface No. 4 in the switching valve VⅢ (3) is connected to interface No. 6 in the switching valve VⅢ (3), and interface No. 5 in the switching valve VⅢ (3) is connected to the DID detector (28).

3. A gas chromatography analysis system for trace impurities in high-purity krypton according to claim 2, characterized in that: The first set of air inlet pipeline units comprises a switching valve VI (1) for taking sample gas, pushing sample gas and pre-segmenting the sample gas, and a switching valve VII (2) for pushing sample gas and splitting the sample gas. The switching valve VII (2) is connected to the interface No. ① in the switching valve VIII (3) via a second 5A molecular sieve chromatographic column (14).

4. A gas chromatography analysis system for trace impurities in high-purity krypton according to claim 3, characterized in that: The switching valve VI (1) is a ten-way purge pneumatic switching valve. Interface No. ① in the switching valve VI (1) is connected to a first sample gas inlet pipeline (6), interface No. ② in the switching valve VI (1) is connected to a first sample gas outlet pipeline (7), a first quantitative loop (8) is arranged between interface No. ③ in the switching valve VI (1) and interface No. ⑩ in the switching valve VI (1), interface No. ④ in the switching valve VI (1) is connected to a first carrier gas pipeline (9), a CILICA GEL column (10) is arranged between interface No. ⑤ in the switching valve VI (1) and interface No. ⑨ in the switching valve VI (1), interface No. ⑥ in the switching valve VI (1) is connected to interface No. ① in the switching valve VI (2) via a first 5A molecular sieve chromatography column (11), interface No. ⑦ in the switching valve VI (1) is connected to a second carrier gas pipeline (12), and interface No. ⑧ in the switching valve VI (1) is connected to a second needle valve (13).

5. A gas chromatography analysis system for trace impurities in high-purity krypton according to claim 4, characterized in that: The switching valve VⅡ(2) is a six-way purge pneumatic switching valve. Interface No. ② in the switching valve VⅡ (2) is connected to interface No. ① in VⅢ (3) via a second 5A molecular sieve chromatographic column (14), interface No. ③ in the switching valve VⅡ (2) is connected to a third carrier gas pipeline (15), interface No. ④ in the switching valve VⅡ (2) is connected to interface No. ⑥ in the switching valve VⅡ (2), and interface No. ⑤ in the switching valve VⅡ (2) is connected to a third needle valve (16).

6. A gas chromatography analysis system for trace impurities in high-purity krypton according to claim 2, characterized in that: The second set of air inlet pipeline units includes a switching valve VIV (4) for taking sample gas and pushing the sample gas, and a switching valve VV (5) for pushing the sample gas and splitting the sample gas. The switching valve VV (5) is connected to the interface No. ③ in the switching valve VIII (3) through the second Hayesep D column (17).

7. A gas chromatography analysis system for trace impurities in high-purity krypton according to claim 6, characterized in that: The switching valve VIV (4) is a six-way purge pneumatic switching valve. Interface No. ⑥ in the switching valve VIV (4) is connected to the second sample gas inlet pipeline (18), interface No. ① in the switching valve VIV (4) is connected to the second sample gas outlet pipeline (19), a second quantitative loop (20) is provided between interface No. ⑤ in the switching valve VIV (4) and interface No. ② in the switching valve VIV (4), interface No. ④ in the switching valve VIV (4) is connected to the fourth carrier gas pipeline (21), and interface No. ③ in the switching valve VIV (4) is connected to interface No. ① in the switching valve VV (5) via a first Hayesep D column (22).

8. A gas chromatography analysis system for trace impurities in high-purity krypton according to claim 7, characterized in that: Interface No. ② in the switching valve VⅤ (5) is connected to interface No. ③ in the switching valve VⅢ (3) via the second Hayesep D column (17), interface No. ③ in the switching valve VⅤ (5) is connected to the fifth carrier gas pipeline (23), interface No. ④ in the switching valve VⅤ (5) is connected to interface No. ⑥ in the switching valve VⅤ (5), and interface No. ⑤ in the switching valve VⅤ (5) is connected to the fourth needle valve (24).

9. A gas chromatography analysis system for trace impurities in high-purity krypton according to claim 4 or 7, characterized in that: The sample gas inlet pipeline is provided with an inlet quick-change joint (25), and the sample gas outlet pipeline is provided with an outlet quick-change joint (26); A vacuum generator (27) is also provided on the sample gas outlet pipeline.