Gas chromatography system for high-purity chlorine trifluoride

Abstract

A gas chromatography system for high-purity chlorine trifluoride, comprising a sample pretreatment unit (1), a negative pressure sampling unit (3), a carrier gas unit (4), and a test unit (5). The negative pressure sampling unit (3) can effectively implement a sampling operation of a chlorine trifluoride sample by means of a negative pressure sampling / sample introduction mode, so as to ensure that when leaking, a chlorine trifluoride pipeline will not leak a chlorine trifluoride gas to ensure the safety of analysts and the environment, and can effectively keep the purity of the chlorine trifluoride sample under test, so as to ensure the precision of a subsequent test result. The whole test process of the test unit (5) can be continuously carried out and, during the test process, tested samples can all enter a second adsorption tank (7) to be decontaminated and then discharged, thereby obviously reducing mutual effects among three tests so as to improve test precision and greatly improve the test efficiency of the samples.

Description

A gas chromatography analysis system for high-purity chlorine trifluoride Technical Field

[0001] The invention relates to a gas chromatography analysis system for high-purity chlorine trifluoride, which can realize the automation of qualitative and quantitative analysis of impurities in high-purity chlorine trifluoride, realize the automation of chlorine trifluoride sample sampling and injection, and improve the safety during the analysis process. Background Art

[0002] Chlorine trifluoride is a chemically active, highly corrosive, and toxic compound composed of elements in the fluorine and chlorine family. Its leakage into the air poses a significant risk. Currently, only methods for analyzing chlorine trifluoride impurities have been reported, both domestically and internationally. However, a safe and reliable automated analysis system for chlorine trifluoride has yet to be developed, hindering efficient and accurate intelligent analysis of chlorine trifluoride.

[0003] Therefore, the research purpose of the present invention is to develop and design a high-purity chlorine trifluoride gas chromatography analysis system that can achieve efficient qualitative and quantitative analysis of chlorine trifluoride and improve the safety of the analysis process, thereby providing a basic guarantee for the chlorine trifluoride process and application.

[0004] Summary of the Invention

[0005] In response to the technical problems existing in the above-mentioned prior art, the present invention is a gas chromatography analysis system for high-purity chlorine trifluoride, which can effectively solve the technical problems existing in the above-mentioned prior art.

[0006] The technical solution of the present invention is:

[0007] A gas chromatography analysis system for high-purity chlorine trifluoride, comprising

[0008] The sample pretreatment unit includes a particle filter device, wherein the air inlet end of the particle filter device is connected to an external sample source through a corresponding filter air inlet valve, and the air outlet end of the particle filter device is externally connected to a corresponding sample injection tube, on which an electric regulating valve and at least one injection switch valve are fixed in sequence;

[0009] A negative pressure sampling unit comprises a six-way valve provided with valve ports 1, 2, 3, 4, 5, and 6 in sequence, wherein valve port 1 of the six-way valve is connected to the sample injection tube via a sample injection branch pipe equipped with at least one sampling injection valve, a corresponding gas quantitative loop is connected between valve port 2 and valve port 5, the valve port 6 is connected to the air inlet end of the corresponding first adsorption tank via a sample discharge pipe equipped with a pressure gauge and at least one sampling discharge valve, the air outlet end of the first adsorption tank is connected to the corresponding first vacuum pump, and the junction between the sample injection tube and the sample injection branch pipe is connected to the air inlet end of the first adsorption tank via an exhaust pipe equipped with a sampling exhaust valve;

[0010] A carrier gas unit, comprising a carrier gas purifier connected to a carrier gas source, wherein a first carrier gas output pipe, a second carrier gas output pipe, a third carrier gas output pipe, and a fourth carrier gas output pipe are connected in parallel to the gas outlet end of the carrier gas purifier, wherein the first carrier gas output pipe is connected to valve port 1 of the six-way valve via a corresponding first needle valve and a carrier gas switch valve, and the second carrier gas output pipe is connected to valve port 3 of the six-way valve via a second needle valve;

[0011] The detection unit includes a first detector, a second detector, and a third detector. The air inlet end of the first detector is connected to the valve port 4 of the six-way valve through a first separation column; a first four-way valve is provided between the second detector and the first detector, and the first four-way valve is provided with valve ports 7, 8, 9, and 10 in sequence. The air outlet end of the first detector is connected to the valve port 7, the air inlet end of the second detector is connected to the valve port 10 through a second separation column and a conversion column, the valve port 8 is connected to the air inlet end of the corresponding second adsorption tank through a first tail gas pipe, and the air outlet end of the second adsorption tank is connected to the corresponding second vacuum pump. The third carrier gas output pipe is connected to the valve port 9 through a corresponding third needle valve; a second four-way valve is arranged between the third detector and the second detector, and the second four-way valve is provided with valve port 11, valve port 12, valve port 13, and valve port 14 in sequence, the gas outlet end of the second detector is connected to the valve port 11, and the gas inlet end of the third detector is connected to the valve port 12 through a first protective column, a second protective column and a third separation column, the valve port 14 and the gas outlet end of the third detector are respectively connected to the gas inlet end of the second adsorption tank through a second tail gas pipe, and the fourth carrier gas output pipe is connected to the valve port 13 through a corresponding fourth needle valve.

[0012] The particulate matter filtering device includes a two-stage filtering mechanism arranged in parallel, and the two-stage filtering mechanism respectively includes a first filter and a second filter arranged in series. The air inlet end of the first filter is connected to the external sample source through the filter air inlet valve, and the air outlet end of the second filter is connected to the sample injection tube.

[0013] The first filter and the second filter are both physical barrier filters. The pore size of the first filter is 10 μm, and the pore size of the second filter is 5 μm.

[0014] The first separation column and the second separation column are fluoroether oil columns, and the third separation column is a diatom salt column.

[0015] The conversion column is a chloride column, the first protection column is a metal column, and the second protection column is a metal oxide column.

[0016] The first detector and the second detector are TCD detectors, and the third detector is a PDD detector.

[0017] Corresponding one-way valves are fixedly installed between the sample discharge pipe, the emptying pipe and the first adsorption tank, and between the first tail gas pipe, the second tail gas pipe and the second adsorption tank.

[0018] The first filter and the second filter respectively include a filter tank body and a sealing cover sealed and installed on the filter tank body, the sealing cover is rotated downward to install a corresponding filter cartridge, the filter cartridge and the inner wall of the filter tank body are spaced apart, and a number of corresponding filter holes are evenly distributed on the filter cartridge, the middle of the sealing cover is respectively provided with a corresponding filter air inlet pipe facing outward, and the bottom of the filter tank body is respectively provided with a corresponding filter exhaust pipe facing outward; the inner wall of the filter cartridge is spirally provided with a corresponding discharge trough, and the bottom of the outer wall of the filter cartridge is fixedly connected to a plurality of metal fan blades outward; the bottom end of the filter cartridge is downwardly connected to a corresponding collecting pipe through a collecting hopper, and a corresponding cleaning pipe is installed through the bottom seal of the filter tank body, the top of the cleaning pipe is sleeved on the outside of the bottom of the collecting pipe, and the fixing device between the cleaning pipe and the collecting pipe is provided with a corresponding sealing bearing, and the bottom fixing device of the cleaning pipe is provided with a corresponding cleaning valve.

[0019] The upper part of the inner side wall of the cleaning pipe is tilted downward and fixedly connected with a circle of corresponding material guide plates. A corresponding material cleaning sealing plate is movably installed in the cleaning pipe on the lower side of the material guide plate, and the material cleaning sealing plate is arranged to protrude upward in an arc shape; a corresponding pressurizing pipe is installed sealingly through the cleaning pipe, and the air outlet end of the pressurizing pipe is folded upward and forms a support for the material cleaning sealing plate. The air inlet end of the pressurizing pipe is connected to an external inert gas source through a pressurizing device. After the inert gas is pressurized, it enters the cleaning pipe along the pressurizing pipe, forms a pushing drive on the material cleaning sealing plate, so that the material cleaning sealing plate is sealed against the material guide plate, and then the cleaning valve is opened, and the filtered and collected particulate materials are discharged into the corresponding collection container along the cleaning pipe after being pressurized.

[0020] A set of corresponding limiting sliding grooves are longitudinally arranged on the inner side wall of the cleaning pipe, and both sides of the cleaning sealing plate are integrally formed with guide rods fixed outwardly and abutting against the limiting sliding grooves.

[0021] Advantages of the present invention:

[0022] 1) When sampling, the present invention first switches the six-way valve to the connection between valve port 1 and valve port 2, valve port 3 and valve port 4, and valve port 5 and valve port 6, switches the first four-way valve to the connection between valve port 7 and valve port 10, valve port 8 and valve port 9, switches the second four-way valve to the connection between valve port 11 and valve port 12, and valve port 13 and valve port 14; then, closes the sampling injection valve, opens the first needle valve, the carrier gas switch valve, the sampling discharge valve, and the second needle valve, the third needle valve, and the fourth needle valve, and then introduces the carrier gas to effectively form a carrier gas purge replacement for the entire negative pressure sampling unit and the detection unit; then, closes the first needle valve, the second needle valve, the third needle valve, and the fourth needle valve, turns on the first vacuum pump, and evacuates the passage. When the pressure When the pressure reading reaches -100 kPa, the first vacuum pump is turned off, and the carrier gas switch valve is closed. Then, the electric regulating valve, the sampling switch valve, and the sampling injection valve are opened to allow chlorine trifluoride to enter the gas quantitative loop under negative pressure conditions. When the pressure reading reaches -75±3 kPa, the quantitative sampling of chlorine trifluoride is completed. Finally, the electric regulating valve, the sampling injection valve, and the sampling exhaust valve are closed, the sampling exhaust valve is opened, and the first vacuum pump is turned on to evacuate the sample injection tube and the sample injection branch pipe. After repeating the quantitative sampling of chlorine trifluoride and the evacuation of the sample injection tube and the sample injection branch pipe three times, the chlorine trifluoride sample is passed into the gas quantitative loop until the pressure reading reaches -75±3 kPa, completing the sampling operation.

[0023] Thus, the sampling operation of the chlorine trifluoride sample is effectively realized by the negative pressure sampling / injection method, thereby ensuring that the chlorine trifluoride gas will not be leaked to the outside when the chlorine trifluoride pipeline leaks, thereby ensuring the safety of the analysts and the environment; and the purity of the chlorine trifluoride sample to be tested can be effectively maintained to ensure the accuracy of the subsequent test results.

[0024] 2) When performing sample detection, the present invention switches the six-way valve to connect valve port 1 with valve port 6, valve port 2 with valve port 3, and valve port 4 with valve port 5; switches the first four-way valve to connect valve port 7 with valve port 10, and valve port 8 with valve port 9; switches the second four-way valve to connect valve port 11 with valve port 12, and valve port 13 with valve port 14; then, the second needle valve is opened, and the carrier gas enters the quantitative loop from valve port 3 and valve port 2, driving the sample to be tested to enter the first separation column through valve port 5 and valve port 4, completing the detection injection operation; in the first separation column, the carrier gas enters ...1 In the separation column, the sample to be tested undergoes the first separation, and the components ClF, HF, ClF3 are separated from F2, O2, N2, and CF4. The sample after the first separation enters the conversion column through valve port 7 and valve port 10; after entering the conversion column and the second separation column through valve 7 and valve 10, the second four-way valve is switched to connect valve port 7 with valve port 8 and valve port 9 with valve port 10. At this time, the ClF, HF, and ClF3 in the first separation column enter the first detector for qualitative and quantitative analysis. The sample after detection enters the second adsorption tank from the first detector. After being harmlessly treated and discharged, F2, O2, N2, and CF4 enter the conversion column; in the conversion column, the F2 in the sample to be tested is converted into Cl2, and the sample to be tested continues to the second separation column for a second separation. In the second separation column, Cl2 is separated from O2, N2, and CF4. The sample after the second separation enters the second detector for qualitative and quantitative analysis. After the separated O2, N2, and CF4 enter the first guard column, the second guard column, and the third separation column through valve ports 11 and 12, the second four-way valve is switched to valve 11 and valve 14 to connect, and Cl2 is passed into the second adsorption tank for harmless treatment and then discharged; the sample after the second separation enters the first guard column and the second guard column to remove residual trace ClF, HF, ClF3, F2, and Cl2, and then enters the third separation column for a third separation. In the third separation column, O2, N2, and CF4 are separated. The sample after the third separation enters the third detector for qualitative and quantitative analysis; the sample after the test is completed enters the second adsorption tank from the second detector and the second detector for harmlessness and then is discharged.

[0025] The entire detection process can be carried out continuously, and the samples that have completed the test can enter the second adsorption tank for harmlessness and then be discharged, which can significantly reduce the mutual influence between the three tests, thereby improving the detection accuracy and greatly improving the detection efficiency of the samples.

[0026] 3) The present invention incorporates a particle filter at the inlet end of the sample inlet tube, effectively filtering chlorine trifluoride particles to a particle size of 5μm or less, ensuring that the sample more closely meets testing requirements. Because the entire sampling process is performed under negative pressure, the filter pores of the particle filter are susceptible to clogging by particulate matter. To address this issue, the present invention further improves the first and second filters of the particle filter. Through the rotatable mounting of the filter cartridge and the provision of multiple metal fan blades, the gas flowing through the filter cartridge and the filter tank effectively drives the filter cartridge to rotate, thereby increasing the filter cartridge's kinetic energy and making it less likely that particulate matter will clog the filter pores. Furthermore, a corresponding discharge groove is spirally provided on the inner sidewall of the filter cartridge, allowing particulate matter adhering to the inner wall of the filter cartridge to be fed by the spiral and collected into the purge pipe. This significantly reduces the probability of clogging the filter pores of the particle filter and improves the smooth flow of the gas sample, ensuring the smooth implementation of the negative pressure sampling of the present invention.

[0027] 4) Since the filter tank is in a vacuum state, it is impossible to directly open the purge valve to clear the filtered material, resulting in the problem that the particulate material after filtration and collection is difficult to clear, and the opening of the purge valve may cause air to enter the filter cartridge, thereby causing safety hazards and other problems. To this end, the present invention further has a guide plate fixedly connected to the upper part of the inner wall of the purge pipe, which is tilted downward, and a purge sealing plate is movably installed on the lower side of the guide plate, and a pressurized pipe is added to support the purge sealing plate that is arranged to protrude upward in an arc shape. During the particulate material removal process, the inert gas is pressurized and enters the purge pipe along the pressurized pipe. On the one hand, it can form a push drive for the purge sealing plate, so that the purge sealing plate is sealed against the guide plate; on the other hand, it can increase the pressure in the purge pipe, so that under the action of pressure, the filtered and collected particulate material is discharged along the purge pipe into the corresponding collection container. Therefore, it is possible to effectively and fully remove the filtered and collected particulate materials, and prevent the particulate materials from mixing into the outside air during the removal process, thereby further effectively improving the practical effect of the present invention.

[0028] BRIEF DESCRIPTION OF THE DRAWINGS

[0029] FIG1 is a schematic structural diagram of the present invention.

[0030] FIG2 is a schematic structural diagram of the first filter and the second filter of the present invention.

[0031] FIG3 is a partial enlarged view of FIG2 of the present invention.

[0032] DETAILED DESCRIPTION

[0033] In order to facilitate understanding by those skilled in the art, the structure of the present invention is further described in detail with reference to the embodiments and the accompanying drawings:

[0034] Example 1:

[0035] Referring to Figure 1-2, a gas chromatography analysis system for high-purity chlorine trifluoride includes

[0036] The sample pretreatment unit 1 includes a particle filter device 101. The air inlet side of the particle filter device 101 is connected to the external sample source through a corresponding filtered air inlet valve 102. The air outlet side of the particle filter device 101 is externally connected to a corresponding sample injection tube 2. The sample injection tube 2 is fixed with an electric regulating valve 201 and a set of injection switch valves 202 in sequence.

[0037] The negative pressure sampling unit 3 comprises a six-way valve 301 provided with valve ports 1, 2, 3, 4, 5 and 6 in sequence. Valve port 1 of the six-way valve 301 is connected to the sample injection tube 2 via a sample injection branch pipe 303 equipped with a group of sampling injection valves 302. A corresponding gas quantitative loop 304 is connected between the valve ports 2 and 5. The valve port 6 is connected to the air inlet end of the corresponding first adsorption tank 308 via a sample discharge pipe 307 equipped with a pressure gauge 305 and a sampling discharge valve 306. The air outlet end of the first adsorption tank 308 is connected to the corresponding first vacuum pump 309. The junction between the sample injection tube 2 and the sample injection branch pipe 303 is connected to the air inlet end of the first adsorption tank 308 via an exhaust pipe 3011 equipped with a sampling exhaust valve 3010.

[0038] The carrier gas unit 4 includes a carrier gas purifier 401 connected to a carrier gas source. A first carrier gas output pipe 402, a second carrier gas output pipe 403, a third carrier gas output pipe 404, and a fourth carrier gas output pipe 405 are connected in parallel to the gas outlet of the carrier gas purifier 401. The first carrier gas output pipe 402 is connected to the valve port 1 of the six-way valve 301 via a corresponding first needle valve 406 and a carrier gas switch valve 407. The second carrier gas output pipe 403 is connected to the valve port 3 of the six-way valve 301 via a second needle valve 408.

[0039] The detection unit 5 includes a first detector 501, a second detector 502, and a third detector 503. The air inlet end of the first detector 501 is connected to the valve port 4 of the six-way valve 301 through a first separation column 504; a first four-way valve 505 is provided between the second detector 502 and the first detector 501, and the first four-way valve 505 is provided with valve ports 7, valve ports 8, valve ports 9, and valve ports 10 in sequence. The air outlet end of the first detector 501 is connected to the valve port 7, and the air inlet end of the second detector 502 is connected to the valve port 10 through a second separation column 506 and a conversion column 507. The valve port 8 is connected to the air inlet end of the corresponding second adsorption tank 7 through a first tail gas pipe 6, and the air outlet end of the second adsorption tank 7 is connected to the corresponding second vacuum pump 8. The third carrier gas output pipe 404 is connected to the valve port 9 through the corresponding third needle valve 409; a second four-way valve 508 is arranged between the third detector 503 and the second detector 502, and the second four-way valve 508 is provided with valve port 11, valve port 12, valve port 13, and valve port 14 in sequence, the gas outlet end of the second detector 502 is connected to the valve port 11, the gas inlet end of the third detector 503 is connected to the valve port 12 through the first protective column 509, the second protective column 5010 and the third separation column 5011, the valve port 14 and the gas outlet end of the third detector 503 are respectively connected to the gas inlet end of the second adsorption tank 7 through the second tail gas pipe 9, and the fourth carrier gas output pipe 405 is connected to the valve port 13 through the corresponding fourth needle valve 4010.

[0040] The particulate matter filtering device 101 includes a two-stage filtering mechanism arranged in parallel, and the two-stage filtering mechanism respectively includes a first filter 1011 and a second filter 1012 arranged in series. The air inlet end of the first filter 1011 is connected to the external sample source through the filter air inlet valve 102, and the air outlet end of the second filter 1012 is connected to the sample injection tube 2.

[0041] The first filter 1011 and the second filter 1012 are both physical barrier filters. The pore size of the first filter 1011 is 10 μm, and the pore size of the second filter 1012 is 5 μm.

[0042] The first separation column 504 and the second separation column 506 are fluoroether oil columns, and the third separation column 5011 is a diatom salt column.

[0043] The conversion column 507 is a chloride column, the first protection column 509 is a metal column, and the second protection column 5010 is a metal oxide column.

[0044] The first detector 501 and the second detector 502 are TCD detectors, and the third detector 503 is a PDD detector.

[0045] Corresponding one-way valves 10 are fixedly installed between the sample discharge pipe 307 , the emptying pipe 3011 and the first adsorption tank 308 , and between the first tail gas pipe 6 , the second tail gas pipe 9 and the second adsorption tank 7 .

[0046] The first filter 1011 and the second filter 1012 respectively include a filter tank body 11 and a cover 12 sealed and installed on the filter tank body 11. The cover 12 is rotated downward to install a corresponding filter cartridge 13. The filter cartridge 13 is spaced apart from the inner wall of the filter tank body 11, and a plurality of corresponding filter holes are evenly distributed on the filter cartridge 13. The middle of the cover 12 is respectively provided with a corresponding filter air inlet pipe 14, and the bottom of the filter tank body 11 is respectively provided with a corresponding filter exhaust pipe 15. The filter cartridge 13 is provided with a plurality of filter holes. The inner wall is spirally provided with a corresponding discharge groove 16, and the bottom of the outer wall of the filter cartridge 13 is fixed outward with a plurality of metal fan blades 17; the bottom end of the filter cartridge 13 is downwardly connected to a corresponding collecting pipe 19 through a collecting hopper 18, and a corresponding cleaning pipe 20 is installed through the bottom seal of the filter tank body 11. The top of the cleaning pipe 20 is sleeved on the bottom outside of the collecting pipe 19, and the fixing device between the cleaning pipe 20 and the collecting pipe 19 is provided with a corresponding sealing bearing 21, and the bottom fixing device of the cleaning pipe 20 is provided with a corresponding cleaning valve 22.

[0047] The upper part of the inner side wall of the cleaning pipe 20 is fixedly connected with a circle of corresponding guide plates 23 that are tilted downward. A corresponding cleaning sealing plate 24 is movably installed in the cleaning pipe 20 on the lower side of the guide plate 23, and the cleaning sealing plate 24 is arranged to protrude upward in an arc shape; a corresponding pressurizing pipe 25 is sealed and penetrated on the cleaning pipe 20, and the air outlet end of the pressurizing pipe 25 is folded upward and supports the cleaning sealing plate 24. The air inlet end of the pressurizing pipe 25 is connected to an external inert gas source through a pressurizing device 26. After the inert gas is pressurized, it enters the cleaning pipe 20 along the pressurizing pipe 25, pushing the cleaning sealing plate 24 to make the cleaning sealing plate 24 seal against the guide plate 23. Then the cleaning valve 22 is opened, and the filtered and collected particulate material is discharged into the corresponding collection container along the cleaning pipe 20 after being pressurized.

[0048] A set of corresponding limiting sliding grooves 27 are longitudinally provided on the inner side wall of the cleaning pipe 20 , and guide rods 28 are integrally formed on both sides of the cleaning sealing plate 24 and fixed outwardly to abut against the limiting sliding grooves 27 .

[0049] Example 2:

[0050] The above-mentioned analysis method of a gas chromatography analysis system for high-purity chlorine trifluoride comprises the following specific steps:

[0051] S1, switch the six-way valve 301 to connect valve port 1 with valve port 2, valve port 3 with valve port 4, and valve port 5 with valve port 6; switch the first four-way valve 505 to connect valve port 7 with valve port 10, and valve port 8 with valve port 9; switch the second four-way valve 508 to connect valve port 11 with valve port 12, and valve port 13 with valve port 14;

[0052] S2, close the sampling injection valve 302, open the first needle valve 406, the carrier gas switching valve 407, the sampling discharge valve 306, and the second needle valve 408, the third needle valve 409, and the fourth needle valve 4010, and then introduce carrier gas to effectively purge and replace the entire negative pressure sampling unit 3 and the detection unit 5;

[0053] S3, close the first needle valve 406, the second needle valve 408, the third needle valve 409, and the fourth needle valve 4010, start the first vacuum pump 309, and evacuate the passage. When the pressure indicator reaches -100 kPa, turn off the first vacuum pump 309, and close the carrier gas switch valve 407. Then, open the electric regulating valve 201, the injection switch valve 202, and the sampling injection valve 302, and allow chlorine trifluoride to enter the gas quantitative loop 304 under negative pressure. When the pressure gauge 305 shows -75±3 kPa, the quantitative sampling of chlorine trifluoride is completed.

[0054] S4, close the electric regulating valve 201, the sampling injection valve 302 and the sampling exhaust valve 306, open the sampling exhaust valve 3010, and start the first vacuum pump 309 to evacuate the sample injection pipe 2 and the sample injection branch pipe 303;

[0055] S5, repeat the quantitative sampling of chlorine trifluoride and the evacuation of the sample injection tube 2 and the sample injection branch pipe 303 three times, then pass the chlorine trifluoride sample into the gas quantitative loop 304 until the pressure 305 reading reaches -75±3kPa, completing the sampling operation;

[0056] S6, switch the six-way valve 301 to connect valve port 1 with valve port 6, valve port 2 with valve port 3, and valve port 4 with valve port 5. Switch the first four-way valve 505 to connect valve port 7 with valve port 10, and valve port 8 with valve port 9. Switch the second four-way valve 508 to connect valve port 11 with valve port 12, and valve port 13 with valve port 14.

[0057] S7, the second needle valve 408 is opened, and the carrier gas enters the quantitative loop 304 from valve ports 3 and 2, driving the sample to be tested into the first separation column 504 through valve ports 5 and 4, completing the detection sampling operation;

[0058] S8, in the first separation column 504, the sample to be tested undergoes a first separation, and the components ClF, HF, and ClF3 are separated from F2, O2, N2, and CF4. The sample after the first separation enters the conversion column 507 through valve ports 7 and 10;

[0059] S9: After the first separation, the sample passes through valves 7 and 10 and enters the conversion column 507 and the second separation column 506. The second four-way valve 508 is switched so that valve port 7 is connected to valve port 8 and valve port 9 is connected to valve port 10. At this time, the ClF, HF, and ClF3 in the first separation column 504 enter the first detector 501 for qualitative and quantitative analysis.

[0060] S10, the sample after detection enters the second adsorption tank 7 from the first detector 501 for harmless treatment and then is discharged, and F2, O2, N2, and CF4 enter the conversion column 507. In the conversion column 507, the F2 in the sample to be detected is converted into Cl2. The sample to be detected continues to the second separation column 506 for a second separation. In the second separation column 506, Cl2 is separated from O2, N2, and CF4. The sample after the second separation enters the second detector 502 for qualitative and quantitative analysis. After the separated O2, N2, and CF4 pass through valve ports 11 and valve ports 12, they enter the first guard column 509, the second guard column 5010, and the third separation column 5011. The second four-way valve 508 is switched to connect valve 11 with valve 14, and Cl2 is passed into the second adsorption tank 7 for harmless treatment and then discharged;

[0061] S11, the sample after the second separation enters the first protective column 509 and the second protective column 5010 to remove the residual trace ClF, HF, ClF3, F2, and Cl2, and then enters the third separation column 5011 for the third separation. In the third separation column 5011, O2, N2, and CF4 are separated. The sample after the third separation enters the third detector 503 for qualitative and quantitative analysis. The sample after the detection is completed enters the second adsorption tank 7 from the second detector 502 and the second detector 503 for harmless treatment and then discharged.

[0062] The entire detection process can be carried out continuously, and the samples that have completed the detection during the detection process can enter the second adsorption tank 7 for harmless treatment and then be discharged, thereby significantly reducing the mutual influence between the three tests, thereby improving the detection accuracy and greatly improving the detection efficiency of the samples.

[0063] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as within the scope of protection of the present invention.

Claims

1. A gas chromatography analysis system for high-purity chlorine trifluoride, characterized in that: include A sample pretreatment unit (1) comprises a particle filter device (101), wherein one side of the air inlet end of the particle filter device (101) is connected to an external sample source via a corresponding filter air inlet valve (102), and the air outlet end of the particle filter device (101) is externally connected to a corresponding sample injection tube (2), wherein an electric regulating valve (201) and at least one injection switch valve (202) are fixedly mounted in sequence on the sample injection tube (2); The negative pressure sampling unit (3) comprises a six-way valve (301) provided with valve ports 1, 2, 3, 4, 5 and 6 in sequence, wherein the valve port 1 of the six-way valve (301) is connected to the sample injection tube (2) via a sample injection branch pipe (303) provided with at least one sampling injection valve (302), a corresponding gas quantitative ring (304) is connected between the valve port 2 and the valve port 5, and the valve port 6 is connected to the sample injection tube (2) via a sample injection branch pipe (303) provided with at least one sampling injection valve (302). 05) and a sample discharge pipe (307) of at least one sampling and discharging valve (306) are connected to the air inlet end of the corresponding first adsorption tank (308), the air outlet end of the first adsorption tank (308) is connected to the corresponding first vacuum pump (309), and the connection between the sample injection pipe (2) and the sample injection branch pipe (303) is connected to the air inlet end of the first adsorption tank (308) through an exhaust pipe (3011) equipped with a sampling and exhausting valve (3010); A carrier gas unit (4), comprising a carrier gas purifier (401) connected to a carrier gas source, wherein a first carrier gas output pipe (402), a second carrier gas output pipe (403), a third carrier gas output pipe (404), and a fourth carrier gas output pipe (405) are connected in parallel to the gas outlet of the carrier gas purifier (401), wherein the first carrier gas output pipe (402) is connected to valve port 1 of the six-way valve (301) via a corresponding first needle valve (406) and a carrier gas switch valve (407), and the second carrier gas output pipe (403) is connected to valve port 3 of the six-way valve (301) via a second needle valve (408); The detection unit (5) comprises a first detector (501), a second detector (502), and a third detector (503); the air inlet end of the first detector (501) is connected to the valve port 4 of the six-way valve (301) via a first separation column (504); a first four-way valve (505) is provided between the second detector (502) and the first detector (501); the first four-way valve (505) is provided with valve ports 7, 8, 9, and 10 in sequence; the air outlet end of the first detector (501) is connected to the valve port 7; the air inlet end of the second detector (502) is connected to the valve port 10 via a second separation column (506) and a conversion column (507); the valve port 8 is connected to the air inlet end of a corresponding second adsorption tank (7) via a first tail gas pipe (6); and the air outlet end of the second adsorption tank (7) is connected to a corresponding second vacuum pump (8). The third carrier gas output pipe (404) is connected to the valve port 9 through a corresponding third needle valve (409); a second four-way valve (508) is arranged between the third detector (503) and the second detector (502); the second four-way valve (508) is provided with valve ports 11, 12, 13 and 14 in sequence; the gas outlet of the second detector (502) is connected to the valve port 11; the gas inlet of the third detector (503) is connected to the valve port 12 through a first protective column (509), a second protective column (5010) and a third separation column (5011); the valve port 14 and the gas outlet of the third detector (503) are connected to the gas inlet of the second adsorption tank (7) through a second tail gas pipe (9), respectively; and the fourth carrier gas output pipe (405) is connected to the valve port 13 through a corresponding fourth needle valve (4010).

2. A gas chromatography analysis system for high-purity chlorine trifluoride according to claim 1, characterized in that: The particle filtering device (101) comprises a two-stage filtering mechanism arranged in parallel, wherein the two-stage filtering mechanism respectively comprises a first filter (1011) and a second filter (1012) arranged in series, wherein the air inlet end of the first filter (1011) is connected to an external sample source via the filtering air inlet valve (102), and the air outlet end of the second filter (1012) is connected to the sample injection tube (2).

3. A gas chromatography analysis system for high-purity chlorine trifluoride according to claim 2, characterized in that: The first filter (1011) and the second filter (1012) are both physical barrier filters; the pore size of the first filter (1011) is 10 μm, and the pore size of the second filter (1012) is 5 μm.

4. A gas chromatography analysis system for high-purity chlorine trifluoride according to claim 1, characterized in that: The first separation column (504) and the second separation column (506) are fluoroether oil columns, and the third separation column (5011) is a diatom salt column.

5. A gas chromatography analysis system for high-purity chlorine trifluoride according to claim 1, characterized in that: The conversion column (507) is a chloride column, the first protection column (509) is a metal column, and the second protection column (5010) is a metal oxide column.

6. A gas chromatography analysis system for high-purity chlorine trifluoride according to claim 1, characterized in that: The first detector (501) and the second detector (502) are TCD detectors, and the third detector (503) is a PDD detector.

7. A gas chromatography analysis system for high-purity chlorine trifluoride according to claim 1, characterized in that: Corresponding one-way valves (10) are fixedly installed between the sample discharge pipe (307), the exhaust pipe (3011) and the first adsorption tank (308), and between the first tail gas pipe (6), the second tail gas pipe (9) and the second adsorption tank (7).

8. A gas chromatography analysis system for high-purity chlorine trifluoride according to claim 1, characterized in that: The first filter (1011) and the second filter (1012) respectively comprise a filter tank body (11), and a cover (12) sealed and mounted on the filter tank body (11); the cover (12) is rotated downward and mounted with a corresponding filter cartridge (13); the filter cartridge (13) and the inner side wall of the filter tank body (11) are arranged at intervals, and a plurality of corresponding filter holes are evenly distributed on the filter cartridge (13); the middle of the cover (12) is respectively provided with a corresponding filter air inlet pipe (14) facing outwards, and the bottom of the filter tank body (11) is respectively provided with a corresponding filter air exhaust pipe (15) facing outwards; the filter cartridge (13) The inner wall of the filter cartridge (13) is spirally provided with a corresponding discharge groove (16); the bottom of the outer wall of the filter cartridge (13) is fixedly connected to a plurality of metal fan blades (17) outwardly; the bottom end of the filter cartridge (13) is downwardly connected to a corresponding material collecting pipe (19) through a material collecting hopper (18); a corresponding material cleaning pipe (20) is installed through the bottom seal of the filter tank body (11); the top of the material cleaning pipe (20) is sleeved on the outer side of the bottom of the material collecting pipe (19); a corresponding sealing bearing (21) is fixed between the material cleaning pipe (20) and the material collecting pipe (19); and a corresponding material cleaning valve (22) is fixed at the bottom of the material cleaning pipe (20).

9. A gas chromatography analysis system for high-purity chlorine trifluoride according to claim 8, characterized in that: The upper part of the inner side wall of the cleaning pipe (20) is fixedly connected with a circle of corresponding material guide plates (23) tilted downward, and a corresponding material cleaning sealing plate (24) is movably installed in the cleaning pipe (20) below the material guide plate (23), and the material cleaning sealing plate (24) is arranged to protrude upward in an arc shape; a corresponding pressurizing pipe (25) is installed and sealed through the cleaning pipe (20), and the air outlet end of the pressurizing pipe (25) is folded upward and contacts the cleaning sealing plate (24). The support is formed, and the air inlet end of the pressurizing pipe (25) is connected to an external inert gas source through a pressurizing device (26). After the inert gas is pressurized, it enters the cleaning pipe (20) along the pressurizing pipe (25), and pushes the cleaning sealing plate (24) to make the cleaning sealing plate (24) seal against the guide plate (23). Then, the cleaning valve (22) is opened, and the filtered and collected particulate materials are discharged along the cleaning pipe (20) into the corresponding collection container after being pressurized.

10. A gas chromatography analysis system for high-purity chlorine trifluoride according to claim 9, characterized in that: A group of corresponding limiting sliding grooves (27) are longitudinally arranged on the inner side wall of the cleaning pipe (20), and guide rods (28) are integrally formed on both sides of the cleaning sealing plate (24) and fixedly connected outwardly to the limiting sliding grooves (27).

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