CN114609283B - System and method for measuring decomposition products in perfluoroisobutyronitrile - Google Patents

System and method for measuring decomposition products in perfluoroisobutyronitrile Download PDF

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Publication number
CN114609283B
CN114609283B CN202210257393.9A CN202210257393A CN114609283B CN 114609283 B CN114609283 B CN 114609283B CN 202210257393 A CN202210257393 A CN 202210257393A CN 114609283 B CN114609283 B CN 114609283B
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way valve
automatic switching
carrier gas
port
chromatographic column
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CN114609283A (en
Inventor
刘伟
赵得先
郭恒新
朱姗
杭忱
曹骏
李建浩
王富德
杨坤
王祥科
李硕
李朝清
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Lansis Instruments Shanghai Co ltd
Electric Power Research Institute of State Grid Anhui Electric Power Co Ltd
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Lansis Instruments Shanghai Co ltd
Electric Power Research Institute of State Grid Anhui Electric Power Co Ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/38—Flow patterns
    • G01N30/46—Flow patterns using more than one column
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/64—Electrical detectors
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/62—Detectors specially adapted therefor
    • G01N30/64—Electrical detectors
    • G01N30/68—Flame ionisation detectors

Abstract

The invention relates to a system and a method for measuring decomposition products in perfluoroisobutyronitrile, wherein the system comprises the following steps: the device comprises a quantitative sampling device, a carrier gas assembly, a first separation device, a second separation device, a third separation device, a hydrogen flame ionization detector and a pulse discharge helium ionization detector; the quantitative sampling device is connected with the gas sample storage device and is also respectively connected with the carrier gas component, the first separation device, the second separation device and the third separation device; the first separation device is connected with the hydrogen flame ionization detector, the second separation device is connected with the pulse discharge helium ionization detector, and the third separation device is connected with the pulse discharge helium ionization detector. The invention is provided with a carrier gas component, three separation devices and two detectors to realize separation and detection of different decomposition products.

Description

System and method for measuring decomposition products in perfluoroisobutyronitrile
Technical Field
The invention relates to the technical field of gas chromatography analysis and detection, in particular to a system and a method for measuring decomposition products in perfluoroisobutyronitrile.
Background
Sulfur hexafluoride (SF) 6 ) Because of its excellent chemical stability, good arc extinguishing performance and thermodynamic stability, it is widely used in the industries of gas-insulated combined electrical equipment, semiconductor etching and smelting, but sulfur hexafluoride (SF) 6 ) Is 23500 times greater than carbon dioxide (CO 2) and is stable in the atmosphere for 3200 years. To reduceSulfur hexafluoride (SF) 6 ) Is required to find sulfur hexafluoride (SF) 6 ) Alternative insulating gases. In 2014, 3M company of united states of Alston corporation, france has commonly introduced an environment-friendly mixed gas in which perfluoroisobutyronitrile (C 4 F 7 N) mainly mixed insulating gas, and C is realized by special project of national key research and development plan of China on environment-friendly pipeline transmission key technology 4 F 7 Domestic preparation of N gas and raising C in China 4 F 7 Development and application of N gas is hot.
C 4 F 7 During the operation of N-gas insulated equipment, tetrafluoroethylene (C 2 F 4 ) Hexafluoroethane (C) 2 F 6 ) Hexafluoropropylene (C) 3 F 6 ) Octafluoropropane (C) 3 F 8 ) Trifluoroacetonitrile (CF) 3 CN), ethanedinitrile (CNCN), pentafluoropropionitrile (C) 2 F 5 CN), dimethyl difluorobutene ((CH) 3 ) 2 C＝CF 2 ) The equally decomposed product has important significance for measuring and analyzing nmol/mol grade impurity components in the perfluoroisobutyronitrile and for researching and applying the perfluoroisobutyronitrile performance.
Disclosure of Invention
In view of the above, the present invention provides a system and a method for determining decomposition products in perfluoroisobutyronitrile, so as to determine decomposition products in perfluoroisobutyronitrile.
In order to achieve the above object, the present invention provides the following solutions:
an assay system for the decomposition products in perfluoroisobutyronitrile, said assay system comprising: the device comprises a quantitative sampling device, a carrier gas assembly, a first separation device, a second separation device, a third separation device, a hydrogen flame ionization detector and a pulse discharge helium ionization detector;
the quantitative sampling device is connected with the gas sample storage device and is also respectively connected with the carrier gas component, the first separation device, the second separation device and the third separation device;
the carrier gas component is used for loading the gas sample stored in the quantitative sampling device into the first separation device, the second separation device and the third separation device;
the first separation device is connected with the hydrogen flame ionization detector and is used for separating a first decomposition product from the gas sample; the first decomposition product comprises trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and/or dimethyldifluorobutene; the hydrogen flame ionization detector is used for detecting the content of each component in the first decomposition product;
The second separation device is connected with the pulse discharge helium ionization detector and is used for separating a second decomposition product from the gas sample; the second decomposition product comprises carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and/or octafluoropropane; the pulse discharge helium ionization detector is used for detecting the content of each component in the second decomposition product;
the third separation device is connected with the pulse discharge helium ionization detector and is used for separating a third decomposition product from the gas sample; the third decomposition product comprises carbon monoxide and/or carbon tetrafluoride; the pulsed discharge helium ionization detector is also used to detect the content of each component in the third decomposition product.
Optionally, the quantitative sampling device comprises a first quantitative ring, a second quantitative ring and a third quantitative ring which are sequentially connected;
the first metering ring is also respectively connected with the gas sample storage device, the carrier gas component and the first separation device;
the second quantitative ring is also respectively connected with the carrier gas component and the second separation device;
The third metering ring is also respectively connected with the carrier gas component, the third separation device and the tail gas recovery device.
Optionally, the first separation device comprises a first chromatographic column, the second separation device comprises a second chromatographic column and a third chromatographic column, the second chromatographic column is used for pre-separating a second decomposition product in the gas sample, and the third chromatographic column is used for secondarily separating the pre-separated second decomposition product; the third separation device comprises a fourth chromatographic column and a fifth chromatographic column, wherein the fourth chromatographic column is used for pre-separating third decomposition products in the gas sample, and the fifth chromatographic column is used for carrying out secondary separation on the pre-separated third decomposition products.
Optionally, the carrier gas assembly includes a first carrier gas channel, a third carrier gas channel, a second carrier gas channel, a fifth carrier gas channel, and a fourth carrier gas channel;
one end of the first carrier gas channel is connected with the first quantitative ring, and the first carrier gas channel is used for loading a gas sample in the first quantitative ring into the first chromatographic column;
one end of the third gas carrying channel is connected with the second quantitative ring, and the third gas carrying channel is used for loading the gas sample in the second quantitative ring into the second chromatographic column;
One end of the second carrier gas channel is connected with the second chromatographic column, and the second carrier gas channel is used for loading the pre-separated second decomposition product in the second chromatographic column into the third chromatographic column;
one end of the fifth carrier gas channel is connected with the third quantitative ring, and the fifth carrier gas channel is used for loading the gas sample in the third quantitative ring into the fourth chromatographic column;
one end of the fourth carrier gas channel is connected with the fourth chromatographic column, and the fourth carrier gas channel is used for loading heavy components in the fourth chromatographic column into the exhaust channel;
the other ends of the first carrier gas channel, the third carrier gas channel, the second carrier gas channel, the fifth carrier gas channel and the fourth carrier gas channel are respectively connected to a carrier gas storage device.
Optionally, the measurement system further comprises an automatic switching six-way valve, a first automatic switching ten-way valve, a second automatic switching ten-way valve and a first automatic switching four-way valve;
the first port of the automatic switching six-way valve is connected with the gas sample storage device, the second port of the automatic switching six-way valve is connected with the first port of the first automatic switching ten-way valve, the third port and the sixth port of the automatic switching six-way valve are respectively connected with two ends of the first quantitative ring, the fourth port of the automatic switching six-way valve is connected with the first chromatographic column, and the fifth port of the automatic switching six-way valve is connected with one end of the first carrier gas channel;
The second port of the first automatic switching ten-way valve is connected with the first port of the second automatic switching ten-way valve, the third port and the tenth port of the first automatic switching ten-way valve are respectively connected with two ends of the second quantitative ring, the fourth port of the first automatic switching ten-way valve is connected with one end of the third carrier gas channel, the fifth port of the first automatic switching ten-way valve is connected to the first exhaust channel, the sixth port and the ninth port of the first automatic switching ten-way valve are respectively connected with two ends of the second chromatographic column, the seventh port of the first automatic switching ten-way valve is connected with one end of the third chromatographic column, and the eighth port of the first automatic switching ten-way valve is connected with one end of the second carrier gas channel;
the second port of the second automatic switching ten-way valve is connected with the tail gas recovery device, the third port and the tenth port of the second automatic switching ten-way valve are respectively connected with two ends of the third metering ring, the fourth port of the second automatic switching ten-way valve is connected with one end of the fifth carrier gas channel, the fifth port of the second automatic switching ten-way valve is connected with one end of the fifth chromatographic column, the sixth port and the ninth port of the second automatic switching ten-way valve are respectively connected with two ends of the fourth chromatographic column, the seventh port of the second automatic switching ten-way valve is connected to the second exhaust channel, a second needle valve is arranged on the third exhaust channel, and the eighth port of the second automatic switching ten-way valve is connected with one end of the fourth carrier gas channel;
The first port of the first automatic switching four-way valve is connected with the other end of the third chromatographic column, the second port of the first automatic switching four-way valve is connected with the pulse discharge helium ionization detector, the third port of the first automatic switching four-way valve is connected with the other end of the fifth chromatographic column, and the fourth port of the first automatic switching four-way valve is connected to a third exhaust channel.
Optionally, the measurement system further comprises a second automatic switching four-way valve;
the first port of the second automatic switching four-way valve is connected with the carrier gas storage device, and the second port of the second automatic switching four-way valve is connected with the first carrier gas channel, the third carrier gas channel, the second carrier gas channel, the fifth carrier gas channel and the other end of the fourth carrier gas channel; the third port of the second automatic switching four-way valve is connected to the other ends of the first exhaust channel, the second exhaust channel and the third exhaust channel; and the fourth port of the second automatic switching four-way valve is connected with a third needle valve.
Optionally, the measurement system further comprises a first planar tee, a second planar tee, a first planar four-way and a second planar four-way;
The three ports of the first plane tee are respectively connected with a first carrier gas channel, a second carrier gas channel and one port of the first plane four-way joint;
the other three ports of the first plane four-way valve are respectively connected with a third gas carrying channel, one port of the second plane three-way valve and a second port of the second automatic switching four-way valve;
the other two ports of the second planar tee are respectively connected with a fifth carrier gas channel and a fourth carrier gas channel;
and the four ports of the second planar four-way valve are respectively connected with the first exhaust channel, the second exhaust channel, the third exhaust channel and the third port of the second automatic switching four-way valve.
Optionally, the first exhaust channel, the second exhaust channel and the third exhaust channel are respectively provided with a first needle valve, a second needle valve and a fourth needle valve, and the outlet positions of the gas sample storage device and the carrier gas storage device are respectively provided with a first pressure reducing valve and a second pressure reducing valve.
A method for determining decomposition products in perfluoroisobutyronitrile, wherein the method is applied to a determination system, the method comprising the steps of:
switching the measurement system to a first state in which the gas sample in the gas sample storage device is stored in the quantitative sampling device;
Switching the measurement system to a second state, in the second state, loading a gas sample in a quantitative sampling device into a first separation device and a second separation device by a carrier gas device, wherein the first separation device separates a first decomposition product from the gas sample, the second separation device pre-separates the gas sample to obtain a pre-separated second decomposition product, and a hydrogen flame ionization detector detects the content of each component in the first decomposition product;
switching the measurement system to a third state, and in the third state, performing secondary separation on the pre-separated second decomposition product by a second separation device, and detecting the content of each component in the second decomposition product by a pulse discharge helium ionization detector;
switching the measurement system to a fourth state in which a carrier gas device loads a gas sample in a quantitative sampling device into a third separation device, the third separation device separates a third decomposition product from the gas sample, and a pulse discharge helium ionization detector detects the content of each component in the third decomposition product;
and switching the measuring system to a fifth state, wherein the measuring system is in a closed state in the fifth state.
Optionally, in the first state, the automatic six-way valve, the first automatic ten-way valve and the second automatic ten-way valve are in a second communication state; the gas sample flows out of the gas sample storage device and fills the first metering ring, the second metering ring and the third metering ring;
in the second state, the automatic switching six-way valve and the first automatic switching ten-way valve are in a first communication state, and the second automatic switching ten-way valve is in a second communication state; the second automatic switching four-way valve is in a first communication state; the carrier gas in the first carrier gas channel loads the gas sample in the first quantitative ring into the first chromatographic column for separation, the obtained first decomposition product enters the hydrogen flame ionization detector for detecting the component content, the carrier gas in the third carrier gas channel loads the gas sample in the second quantitative ring into the second chromatographic column for pre-separation, and the light component obtained by the pre-separation is emptied through the first needle valve;
in the third state, the automatic switching six-way valve, the first automatic switching ten-way valve and the second automatic switching ten-way valve are in a second communication state, and the first automatic switching four-way valve and the second automatic switching four-way valve are in a first communication state; the carrier gas in the second carrier gas channel loads the pre-separated second decomposition product in the second chromatographic column into a third chromatographic column, the third chromatographic column carries out secondary separation on the pre-separated second decomposition product, and the obtained second decomposition product enters a pulse discharge helium ionization detector to detect the component content;
In the fourth state, the automatic switching six-way valve, the first automatic switching ten-way valve and the first automatic switching four-way valve are in a second communication state, the second automatic switching ten-way valve and the second automatic switching four-way valve are in a first communication state, a fifth carrier gas channel loads a gas sample in a third quantitative ring into a fourth chromatographic column for pre-separation, a pre-separated third decomposition product enters a fifth chromatographic column for secondary separation, and a secondarily separated third decomposition product enters a pulse discharge helium ionization detector for detecting the component content;
in the fifth state, the automatic switching six-way valve, the first automatic switching ten-way valve, the second automatic switching ten-way valve, the first automatic switching four-way valve and the second automatic switching four-way valve are all in a second communication state, and heavy components in the fourth chromatographic column are emptied through a second needle valve.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the invention discloses a determination system for decomposition products in perfluoroisobutyronitrile, which comprises: the device comprises a quantitative sampling device, a carrier gas assembly, a first separation device, a second separation device, a third separation device, a hydrogen flame ionization detector and a pulse discharge helium ionization detector; the quantitative sampling device is connected with the gas sample storage device and is also respectively connected with the carrier gas component, the first separation device, the second separation device and the third separation device; the first separation device is connected with the hydrogen flame ionization detector, the second separation device is connected with the pulse discharge helium ionization detector, and the third separation device is connected with the pulse discharge helium ionization detector. The invention is provided with a carrier gas component, three separation devices and two detectors to realize separation and detection of different decomposition products.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions of the prior art, the drawings that are needed in the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of a structure and a communication state of a measurement system in a first state according to an embodiment of the present invention;
FIG. 2 is a schematic diagram showing the structure and communication state of the measurement system in the second state according to the embodiment of the present invention;
FIG. 3 is a schematic diagram showing the structure and communication state of a measurement system in a secondary separation stage in a third state according to an embodiment of the present invention;
FIG. 4 is a schematic diagram showing the structure and communication state of a measurement system in a third detection stage according to an embodiment of the present invention;
FIG. 5 is a schematic diagram showing the structure and communication state of a measurement system in a fourth detection stage according to an embodiment of the present invention;
FIG. 6 is a schematic diagram showing the structure and communication state of a measurement system in a detection stage in a fifth state according to an embodiment of the present invention;
The device comprises a 1-gas sample storage device, a 2-first pressure reducing valve, a 3-first quantitative ring, a 4-second quantitative ring, a 5-third quantitative ring, a 6-tail gas recovery device, a 7-first automatic switching six-way valve, an 8-first automatic switching ten-way valve, a 9-second automatic switching ten-way valve, a 10-first carrier gas channel, a 11-first chromatographic column, a 12-hydrogen flame ionization detector, a 13-second chromatographic column, a 14-second carrier gas channel, a 15-first plane tee joint, a 16-third chromatographic column, a 17-first needle valve, a 18-third carrier gas channel, a 19-fourth chromatographic column, a 20-fourth carrier gas channel, a 21-second needle valve, a 22-fifth chromatographic column, a 23-fifth carrier gas channel, a 24-second pressure reducing valve, a 25-carrier gas storage device, a 26-second automatic switching four-way valve, a 27-third needle valve, a 28-second plane four-way valve, a 29-fourth needle valve, a 30-fifth automatic switching four-way valve and a 31-pulse ionization detector.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The invention aims to provide a system and a method for measuring decomposition products in perfluoroisobutyronitrile, so as to realize the measurement of the decomposition products in perfluoroisobutyronitrile.
In order that the above-recited objects, features and advantages of the present invention will become more readily apparent, a more particular description of the invention will be rendered by reference to the appended drawings and appended detailed description.
As shown in fig. 1 to 6, reference numerals (1), (2), (3) and the like in fig. 1 to 6 of the present invention are reference numerals for automatically switching a six-way valve, automatically switching a ten-way valve and automatically switching a four-way valve, and correspond to a first port, a second port, a third port and the like in the embodiment of the present invention, respectively, and also correspond to a first port (minimum reference numeral (1)) and a last port (maximum reference numeral, for example, (6), and (4)) in the embodiment of the present invention.
In order to achieve the above object, an embodiment of the present invention provides an assay system for decomposition products in perfluoroisobutyronitrile, the assay system should include:
the device for measuring the content of the trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethylbutene comprises a separation passage, wherein a first chromatographic column 11 for separating the trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethylbutene is arranged on the separation passage, a first carrier gas passage 10 for introducing a gas sample into the first chromatographic column 11 is communicated with the carrier gas end of the separation passage through a multi-way switching valve, a first chromatographic column 11 for separating the trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethylbutene is communicated with the outlet end of the separation passage through a first automatic switching six-way valve 7, the first carrier gas passage 10, the first chromatographic column 11 are sequentially communicated in the direction of gas flow, and a hydrogen flame ionization detector 12 for detecting the content of the trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethylbutene is arranged at the outlet end of the first chromatographic column 11;
The device for measuring the content of the carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane components comprises a separation passage, wherein a second chromatographic column 13 and a third chromatographic column 16 for separating the carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane components are arranged on the separation passage, a carrier gas end of the separation passage is communicated with a third gas carrying passage 18 for introducing a gas sample into the second chromatographic column 13 through a first automatic switching ten-way valve 8, an outlet end of the separation passage is communicated with a second chromatographic column 13 for separating the carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane through the first automatic switching ten-way valve 8, the third gas carrying passage 18, a second quantitative ring 4, the second chromatographic column 13, the second carrier gas passage 14 and the third chromatographic column 16 are sequentially communicated along the direction of gas flow, and a pulse ionization detector 31 for detecting the content of the carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane components is arranged at an outlet end of the third chromatographic column 16;
The device for measuring the content of the carbon monoxide and the carbon tetrafluoride component comprises a separation passage, wherein a fourth chromatographic column 19 and a fifth chromatographic column 22 for separating the carbon monoxide and the carbon tetrafluoride component are arranged on the separation passage, a fifth carrier gas passage 23 for introducing a gas sample into the fourth chromatographic column 19 is communicated with the carrier gas end of the separation passage through a second automatic switching ten-way valve 9, a fifth chromatographic column 22 for separating the carbon monoxide and the carbon tetrafluoride component is communicated with the outlet end of the separation passage through the second automatic switching ten-way valve 9, the fifth carrier gas passage 23, a third quantitative ring 5, the fourth chromatographic column 19, the fourth carrier gas passage 20 and the fifth chromatographic column 22 are sequentially communicated in the direction of gas flow, and a pulse discharge helium ionization detector 31 for detecting the content of the carbon monoxide and the carbon tetrafluoride component is arranged at the outlet end of the fifth chromatographic column 22.
The system for measuring the decomposition products in the perfluoroisobutyronitrile further comprises a quantitative measuring device for carbon monoxide, carbon tetrafluoride, carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene, octafluoropropane, trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethyl difluorobutene, wherein the quantitative measuring device is arranged on a gas sample passage, and is a quantitative ring for accurately measuring carbon monoxide, carbon tetrafluoride, carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene, octafluoropropane, trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethyl difluorobutene in the gas sample.
Specifically, as shown in fig. 1-6, an embodiment of the present invention provides an assay system for a decomposition product in perfluoroisobutyronitrile, the assay system comprising: a quantitative sampling device, a carrier gas assembly, a first separation device, a second separation device, a third separation device, a hydrogen flame ionization detector 12, and a pulsed discharge helium ionization detector 31; the quantitative sampling device is connected with the gas sample storage device and is also respectively connected with the carrier gas component, the first separation device, the second separation device and the third separation device; the carrier gas component is used for loading the gas sample stored in the quantitative sampling device into the first separation device, the second separation device and the third separation device; said first separation means being connected to said hydrogen flame ionization detector 12, said first separation means being for separating a first decomposition product from said gas sample; the first decomposition product comprises trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and/or dimethyldifluorobutene; the hydrogen flame ionization detector 12 is for detecting the content of each component in the first decomposition product; the second separation device is connected with the pulse discharge helium ionization detector 31 and is used for separating a second separation product from the gas sample; the second decomposition product comprises carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and/or octafluoropropane; the pulse discharge helium ionization detector 31 is for detecting the content of each component in the second decomposition product; the third separation device is connected with the pulse discharge helium ionization detector 31 and is used for separating a third decomposition product from the gas sample; the third decomposition product comprises carbon monoxide and/or carbon tetrafluoride; the pulse discharge helium ionization detector 31 is also used to detect the content of each component in the third decomposition product.
The quantitative sampling device comprises a first quantitative ring 3, a second quantitative ring 4 and a third quantitative ring 5 which are sequentially connected; the first metering ring 3 is also respectively connected with the gas sample storage device, the carrier gas component and the first separation device; the second quantitative ring 4 is also connected with the carrier gas component and the second separation device respectively; the third metering ring 5 is also connected to the carrier gas assembly, the third separation device and the tail gas recovery device 6, respectively. The first dosing ring 3, the second dosing ring 4 and the third dosing ring 5 in the embodiment of the invention are all arranged on the gas sample path.
The first separation device comprises a first chromatographic column 11, the second separation device comprises a second chromatographic column 13 and a third chromatographic column 16, the second chromatographic column 13 is used for pre-separating a second decomposed product in the gas sample, and the third chromatographic column 16 is used for secondarily separating the pre-separated second decomposed product; the third separation device comprises a fourth chromatographic column 19 and a fifth chromatographic column 22, the fourth chromatographic column 19 is used for pre-separating the third decomposition products in the gas sample, and the fifth chromatographic column 22 is used for secondarily separating the pre-separated third decomposition products.
The carrier gas assembly includes a first carrier gas channel 10, a third carrier gas channel 18, a second carrier gas channel 14, a fifth carrier gas channel 23, and a fourth carrier gas channel 20; one end of the first carrier gas channel 10 is connected with the first quantitative ring 3, and the first carrier gas channel 10 is used for loading a gas sample in the first quantitative ring 3 into the first chromatographic column 11; one end of the third gas carrying channel 18 is connected to the second quantitative ring 4, and the third gas carrying channel 18 is used for carrying the gas sample in the second quantitative ring 4 into the second chromatographic column 13; one end of the second carrier gas channel 14 is connected to the second chromatographic column 13, and the second carrier gas channel 14 is used for loading the pre-separated second decomposition product in the second chromatographic column 13 into the third chromatographic column 16; one end of the fifth carrier gas channel 23 is connected to the third metering ring 5, and the fifth carrier gas channel 23 is used for loading the gas sample in the third metering ring 5 into the fourth chromatographic column 19; one end of the fourth carrier gas channel 20 is connected with the fourth chromatographic column 19, and the fourth carrier gas channel 20 is used for loading heavy components in the fourth chromatographic column 19 into an exhaust channel; the other ends of the first carrier gas passage 10, the third carrier gas passage 18, the second carrier gas passage 14, the fifth carrier gas passage 23, and the fourth carrier gas passage 20 are connected to a carrier gas storage device 25, respectively.
The measuring system further comprises an automatic switching six-way valve, a first automatic switching ten-way valve 8, a second automatic switching ten-way valve 9 and a first automatic switching four-way valve 30; the first port of the automatic six-way switching valve is connected with the gas sample storage device, the second port of the automatic six-way switching valve is connected with the first port of the first automatic ten-way switching valve 8, the third port and the sixth port of the automatic six-way switching valve are respectively connected with the two ends of the first quantitative ring 3, the fourth port of the automatic six-way switching valve is connected with the first chromatographic column 11, and the fifth port of the automatic six-way switching valve is connected with one end of the first carrier gas channel 10; the second port of the first automatic switching ten-way valve 8 is connected with the first port of the second automatic switching ten-way valve 9, the third port and the tenth port of the first automatic switching ten-way valve 8 are respectively connected with two ends of the second quantitative ring 4, the fourth port of the first automatic switching ten-way valve 8 is connected with one end of the third carrier gas channel 18, the fifth port of the first automatic switching ten-way valve 8 is connected with the first exhaust channel, the sixth port and the ninth port of the first automatic switching ten-way valve 8 are respectively connected with two ends of the second chromatographic column 13, the seventh port of the first automatic switching ten-way valve 8 is connected with one end of the third chromatographic column 16, and the eighth port of the first automatic switching ten-way valve 8 is connected with one end of the second carrier gas channel 14; the second port of the second automatic switching tenth-way valve 9 is connected with the tail gas recovery device 6, the third port and the tenth port of the second automatic switching tenth-way valve 9 are respectively connected with two ends of the third quantitative ring 5, the fourth port of the second automatic switching tenth-way valve 9 is connected with one end of the fifth carrier gas channel 23, the fifth port of the second automatic switching tenth-way valve 9 is connected with one end of the fifth chromatographic column 22, the sixth port and the ninth port of the second automatic switching tenth-way valve 9 are respectively connected with two ends of the fourth chromatographic column 19, the seventh port of the second automatic switching tenth-way valve 9 is connected to a second exhaust channel, a second needle valve 21 is arranged on the third exhaust channel, and the eighth port of the second automatic switching tenth-way valve 9 is connected with one end of the fourth carrier gas channel 20; the first port of the first automatic switching four-way valve 30 is connected to the other end of the third chromatographic column 16, the second port of the first automatic switching four-way valve 30 is connected to the pulsed discharge helium ionization detector 31, the third port of the first automatic switching four-way valve 30 is connected to the other end of the fifth chromatographic column 22, and the fourth port of the first automatic switching four-way valve 30 is connected to a third exhaust passage.
The assay system also includes a second automatically switching four-way valve 26; a first port of the second automatic switching four-way valve 26 is connected with the carrier gas storage device 25, and a second port of the second automatic switching four-way valve 26 is connected with the first carrier gas channel 10, the third carrier gas channel 18, the second carrier gas channel 14, the fifth carrier gas channel 23 and the other end of the fourth carrier gas channel 20; the third port of the second automatic switching four-way valve 26 is connected to the other ends of the first exhaust passage, the second exhaust passage and the third exhaust passage; the fourth port of the second automatic switching four-way valve 26 is connected with a third needle valve 27.
The measuring system further comprises a first plane tee 15, a second plane tee, a first plane four-way and a second plane four-way 28; the three ports of the first plane tee 15 are respectively connected with the first carrier gas channel 10, the second carrier gas channel 14 and one port of the first plane tee; the other three ports of the first plane four-way are respectively connected with the third carrier gas channel 18, one port of the second plane three-way and the second port of the second automatic switching four-way valve 26; the other two ports of the second planar tee are respectively connected with a fifth carrier gas channel 23 and a fourth carrier gas channel 20; the four ports of the second planar four-way valve 28 are respectively connected to the first exhaust passage, the second exhaust passage, the third exhaust passage and the third port of the second automatic switching four-way valve 26.
The first exhaust passage, the second exhaust passage and the third exhaust passage are respectively provided with a first needle valve 17, a second needle valve 21 and a fourth needle valve 29, and the outlet positions of the gas sample storage device and the carrier gas storage device 25 are respectively provided with a first pressure reducing valve 2 and a second pressure reducing valve 24.
The embodiment of the invention also provides a method for measuring the decomposition products in the perfluoroisobutyronitrile, which comprises the following steps:
the components of the trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethyl difluorobutene are determined in the following steps: quantitatively measuring a gas sample: preparing a gas sample passage, wherein a first quantitative ring 3 is arranged on the gas sample passage, introducing a gas sample into the gas sample passage, and quantitatively measuring the gas sample through the first quantitative ring 3; detecting the components of trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethyl difluorobutene: the tail end of the analysis chromatographic column is communicated with a hydrogen flame ionization detector 12, and the trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethylbutylene components which flow out of the first chromatographic column 11 enter the hydrogen flame ionization detector 12, and the content of the trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethylbutylene components is measured by the hydrogen flame ionization detector 12.
Carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane component content determination process: quantitatively measuring a gas sample: preparing a gas sample passage, wherein a second quantitative ring 4 is arranged on the gas sample passage, introducing a gas sample into the gas sample passage, and quantitatively measuring the gas sample through the second quantitative ring 4; detecting carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane components: the gas outlet end of the third chromatographic column 16 is communicated with a pulse discharge helium ionization detector 31, and the carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane components flowing out of the third chromatographic column 16 enter the pulse discharge helium ionization detector 31, and the content of the components is measured by the pulse discharge helium ionization detector 31.
The content measurement process of carbon monoxide and carbon tetrafluoride components comprises the following steps: quantitatively measuring a gas sample: preparing a gas sample passage, wherein a third quantitative ring 5 is arranged on the gas sample passage, introducing a gas sample into the gas sample passage, and quantitatively measuring the gas sample through the third quantitative ring 5; detecting carbon monoxide and carbon tetrafluoride components: the gas outlet end of the fifth chromatographic column 22 is communicated with a pulse discharge helium ionization detector 31, and carbon monoxide and carbon tetrafluoride components flowing out of the fifth chromatographic column 22 enter the pulse discharge helium ionization detector 31, and the content of the carbon monoxide and carbon tetrafluoride components is measured by the pulse discharge helium ionization detector 31.
The invention provides a method for measuring decomposition products in perfluoroisobutyronitrile, which comprises the following steps:
the measurement system is switched to a first state in which the gas sample in the gas sample storage device 1 is stored in the quantitative sampling device. In the first state, the automatic switching six-way valve, the first automatic switching ten-way valve 8 and the second automatic switching ten-way valve 9 are in a second communication state; the gas sample flows out of the gas sample storage device and fills the first dosing ring 3, the second dosing ring 4 and the third dosing ring 5. Namely, the process is a quantitative gas sample measuring process, and the specific implementation mode is as follows: as shown in fig. 1, after the gas sample component is depressurized through the first depressurization valve 2 from the gas sample gas storage device 1, the gas sample component is connected to the No. 1 interface, the No. 6 interface, the first dosing ring 3 and the No. 3 interface of the first automatic switching six-way valve 7 through a gas path connecting pipeline, flows from the No. 2 interface to the No. 1 interface, the No. 10 interface, the second dosing ring 4 and the No. 3 interface of the first automatic switching ten-way valve 8, flows from the No. 2 interface to the No. 1 interface, the No. 10 interface, the third dosing ring 5 and the No. 3 interface of the second automatic switching ten-way valve 9, and finally flows from the No. 2 interface to the tail gas recovery device 6. The embodiment of the invention quantitatively measures the gas sample by one-time ventilation, ensures carbon monoxide (CO) and carbon tetrafluoride (CF) 4 ) Carbon dioxide (CO) 2) Tetrafluoroethylene (C) 2 F 4 ) Hexafluoroethane (C) 2 F 6 ) Hexafluoropropylene (C) 3 F 6 ) Octafluoropropane (C) 3 F 8 ) Trifluoroacetonitrile (CF) 3 CN), ethanedinitrile (CNCN), pentafluoropropionitrile (C) 2 F 5 CN), dimethyl difluorobutene ((CH) 3 ) 2 C＝CF 2 ) The separation degree of the components and also the separation degree of the components on carbon monoxide (CO) and carbon tetrafluoride (CF) 4 ) Carbon dioxide (CO) 2) Tetrafluoroethylene (C) 2 F 4 ) Hexafluoroethane (C) 2 F 6 ) Hexafluoropropylene (C) 3 F 6 ) Octafluoropropane (C) 3 F 8 ) Trifluoroacetonitrile (CF) 3 CN), ethanedinitrile (CNCN), pentafluoropropionitrile (C) 2 F 5 CN), dimethyl difluorobutene ((CH) 3 ) 2 C＝CF 2 ) The accuracy of component detection and the analysis period are short. The components are not interfered with each other, and the separation degree R is more than or equal to 1.5。
Switching the measurement system to a second state in which a carrier gas device loads a gas sample in a quantitative sampling device into a first separation device and a second separation device, wherein the first separation device separates a first decomposition product from the gas sample, the second separation device pre-separates the gas sample to obtain a pre-separated second decomposition product, and a hydrogen flame ionization detector 12 detects the content of each component in the first decomposition product; in the second state, the automatic switching six-way valve and the first automatic switching ten-way valve 8 are in a first communication state, and the second automatic switching ten-way valve 9 is in a second communication state; the second automatic switching four-way valve 26 is in the first communication state; the carrier gas in the first carrier gas channel 10 loads the gas sample in the first quantitative loop 3 into the first chromatographic column 11 for separation, the obtained first decomposition product enters the hydrogen flame ionization detector 12 for component content detection, the carrier gas in the third carrier gas channel 18 loads the gas sample in the second quantitative loop 4 into the second chromatographic column 13 for pre-separation, and the light component obtained by the pre-separation is emptied through the first needle valve 17. The carrier gas in the first carrier gas channel 10 loads the gas sample in the first quantitative ring 3 into the first chromatographic column 11 for separation, and the obtained first decomposition product enters the hydrogen flame ionization detector 12 for component content detection, wherein the component content detection process comprises the steps of detecting the components of trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethyldifluorobutene: as shown in fig. 2, the first carrier gas channel 10 carries the gas sample in the first quantitative ring 3 to enter the first chromatographic column 11 for separation, and the first carrier gas channel 10 carries the components of trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethyldifluorobutene separated in the first chromatographic column 11 for measurement by the flame ionization detector 12.
The carrier gas in the third carrier gas channel 18 loads the gas sample in the second quantitative ring 4 into the second chromatographic column 13 for pre-separation, and the process of evacuating the light component obtained by the pre-separation through the first needle valve 17 is the process of predicting the contents of carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane components: as shown in fig. 2, the third gas carrying channel 18 carries the gas sample in the second quantifying ring 4 into the second chromatographic column 13, and the light components such as oxygen and nitrogen separated by the second chromatographic column 13 are emptied by the first needle valve 17.
Switching the measurement system to a third state in which the second separation device performs secondary separation of the pre-separated second decomposition product, and the pulse discharge helium ionization detector 31 detects the content of each component in the second decomposition product; in the third state, the automatic switching six-way valve, the first automatic switching ten-way valve 8 and the second automatic switching ten-way valve 9 are in a second communication state, and the first automatic switching four-way valve 30 and the second automatic switching four-way valve 26 are in a first communication state; the carrier gas in the second carrier gas channel 14 loads the pre-separated second decomposition product in the second chromatographic column 13 into the third chromatographic column 16, the third chromatographic column 16 carries out secondary separation on the pre-separated second decomposition product, and the obtained second decomposition product enters the pulse discharge helium ionization detector 31 for detecting the component content. This process is a secondary measurement process of the contents of carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane components, as shown in fig. 2, when the carbon dioxide components are separated from the second chromatographic column 13, fig. 2 is switched to fig. 3, further switched to the state of fig. 4, the second carrier gas channel 14 carries the carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane components in the second chromatographic column 13 to the third chromatographic column 16, and the third chromatographic column 16 further separates the carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane components, which is measured by the pulse discharge helium ionization detector 31.
Switching the measurement system to a fourth state in which a carrier gas device loads a gas sample in a quantitative sampling device into a third separation device, the third separation device separates a third decomposition product from the gas sample, and a pulse discharge helium ionization detector 31 detects the content of each component in the third decomposition product; in the fourth state, the automatic switching six-way valve, the first automatic switching ten-way valve 8 and the first automatic switching four-way valve 30 are in a second communication state, the second automatic switching ten-way valve 9 and the second automatic switching four-way valve 26 are in a first communication state, the fifth carrier gas channel 23 loads the gas sample in the third metering ring 5 into the fourth chromatographic column 19 for pre-separation, the pre-separated third decomposition product enters the fifth chromatographic column 22 for secondary separation, and the secondarily separated third decomposition product enters the pulse discharge helium ionization detector 31 for detecting the component content. The process is a determination process of the content of carbon monoxide and carbon tetrafluoride components: as shown in fig. 5, the fifth carrier gas channel 23 carries the gas sample in the third metering ring 5 into the fourth chromatographic column 19, the fourth chromatographic column 19 pre-separates carbon monoxide from the carbon tetrafluoride component, the pre-separated carbon monoxide and carbon tetrafluoride component flow into the fifth chromatographic column 22 through the fifth carrier gas channel 23, and after further separation, the carbon monoxide and carbon tetrafluoride component are detected by the pulse discharge helium ionization detector 31.
And switching the measuring system to a fifth state, wherein the measuring system is in a closed state in the fifth state. In the fifth state, the automatic switching six-way valve, the first automatic switching ten-way valve 8, the second automatic switching ten-way valve 9, the first automatic switching four-way valve 30 and the second automatic switching four-way valve 26 are all in the second communication state, and the heavy component in the fourth chromatographic column 19 is emptied through the second needle valve 21. The process includes the process of emptying the hexafluoropropylene, octafluoropropane and other heavy components in the fourth chromatographic column 19 through the second needle valve 21, as shown in fig. 6, at this time, the second automatic switching four-way valve 26 is automatically switched to the state of fig. 6, and the system is in a closed state, so that the system is prevented from penetrating air in an analysis state, and the next starting-up stability time is affected.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the invention uses multiple carrier gases and multiple chromatographic columns to make the carbon monoxide (CO) and carbon tetrafluoride (CF) 4 ) Carbon dioxide (CO) 2) Tetrafluoroethylene (C) 2 F 4 ) Hexafluoroethane (C) 2 F 6 ) Hexafluoropropylene (C) 3 F 6 ) Octafluoropropane (C) 3 F 8 ) Trifluoroacetonitrile (CF) 3 CN), ethanedinitrile (CNCN), pentaFluoropropionitrile (C) 2 F 5 CN), dimethyl difluorobutene ((CH) 3 ) 2 C＝CF 2 ) The components are completely separated, and the carbon monoxide (CO) and the carbon tetrafluoride (CF) are ensured 4 ) Carbon dioxide (CO) 2) Tetrafluoroethylene (C) 2 F 4 ) Hexafluoroethane (C) 2 F 6 ) Hexafluoropropylene (C) 3 F 6 ) Octafluoropropane (C) 3 F 8 ) Trifluoroacetonitrile (CF) 3 CN), ethanedinitrile (CNCN), pentafluoropropionitrile (C) 2 F 5 CN), dimethyl difluorobutene ((CH) 3 ) 2 C＝CF 2 ) The accuracy of component detection and the analysis period are short.
In the present specification, each embodiment is described in a progressive manner, and each embodiment is mainly described in a different point from other embodiments, and identical and similar parts between the embodiments are all enough to refer to each other.
The principles and embodiments of the present invention have been described herein with reference to specific examples, the description of which is intended only to assist in understanding the methods of the present invention and the core ideas thereof; also, it is within the scope of the present invention to be modified by those of ordinary skill in the art in light of the present teachings. In view of the foregoing, this description should not be construed as limiting the invention.

Claims (5)

1. A system for determining decomposition products in perfluoroisobutyronitrile, the system comprising: the device comprises a quantitative sampling device, a carrier gas assembly, a first separation device, a second separation device, a third separation device, a hydrogen flame ionization detector and a pulse discharge helium ionization detector;
The quantitative sampling device is connected with the gas sample storage device and is also respectively connected with the carrier gas component, the first separation device, the second separation device and the third separation device;
the carrier gas component is used for loading the gas sample stored in the quantitative sampling device into the first separation device, the second separation device and the third separation device;
the first separation device is connected with the hydrogen flame ionization detector and is used for separating a first decomposition product from the gas sample; the first decomposition product comprises trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and/or dimethyldifluorobutene; the hydrogen flame ionization detector is used for detecting the content of each component in the first decomposition product;
the second separation device is connected with the pulse discharge helium ionization detector and is used for separating a second decomposition product from the gas sample; the second decomposition product comprises carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and/or octafluoropropane; the pulse discharge helium ionization detector is used for detecting the content of each component in the second decomposition product;
The third separation device is connected with the pulse discharge helium ionization detector and is used for separating a third decomposition product from the gas sample; the third decomposition product comprises carbon monoxide and/or carbon tetrafluoride; the pulsed discharge helium ionization detector is further configured to detect a content of each component in the third decomposition product;
the quantitative sampling device comprises a first quantitative ring, a second quantitative ring and a third quantitative ring which are sequentially connected;
the first metering ring is also respectively connected with the gas sample storage device, the carrier gas component and the first separation device;
the second quantitative ring is also respectively connected with the carrier gas component and the second separation device;
the third metering ring is also respectively connected with the carrier gas component, the third separation device and the tail gas recovery device;
the first separation device comprises a first chromatographic column for separating a first decomposition product in a gas sample, the second separation device comprises a second chromatographic column for pre-separating a second decomposition product in the gas sample and a third chromatographic column for secondarily separating the pre-separated second decomposition product; the third separation device comprises a fourth chromatographic column and a fifth chromatographic column, the fourth chromatographic column is used for pre-separating a third decomposition product in the gas sample, and the fifth chromatographic column is used for secondarily separating the pre-separated third decomposition product;
The carrier gas assembly comprises a first carrier gas channel, a second carrier gas channel, a third carrier gas channel, a fourth carrier gas channel and a fifth carrier gas channel;
one end of the first carrier gas channel is connected with the first quantitative ring, and the first carrier gas channel is used for loading a gas sample in the first quantitative ring into the first chromatographic column;
one end of the third gas carrying channel is connected with the second quantitative ring, and the third gas carrying channel is used for loading the gas sample in the second quantitative ring into the second chromatographic column;
one end of the second carrier gas channel is connected with the second chromatographic column, and the second carrier gas channel is used for loading the pre-separated second decomposition product in the second chromatographic column into the third chromatographic column;
one end of the fifth carrier gas channel is connected with the third quantitative ring, and the fifth carrier gas channel is used for loading the gas sample in the third quantitative ring into the fourth chromatographic column;
one end of the fourth carrier gas channel is connected with the fourth chromatographic column, and the fourth carrier gas channel is used for loading heavy components in the fourth chromatographic column into the exhaust channel;
the other ends of the first carrier gas channel, the third carrier gas channel, the second carrier gas channel, the fifth carrier gas channel and the fourth carrier gas channel are respectively connected to a carrier gas storage device;
The measuring system further comprises an automatic switching six-way valve, a first automatic switching ten-way valve, a second automatic switching ten-way valve and a first automatic switching four-way valve;
the first port of the automatic switching six-way valve is connected with the gas sample storage device, the second port of the automatic switching six-way valve is connected with the first port of the first automatic switching ten-way valve, the third port and the sixth port of the automatic switching six-way valve are respectively connected with two ends of the first quantitative ring, the fourth port of the automatic switching six-way valve is connected with the first chromatographic column, and the fifth port of the automatic switching six-way valve is connected with one end of the first carrier gas channel;
the second port of the first automatic switching ten-way valve is connected with the first port of the second automatic switching ten-way valve, the third port and the tenth port of the first automatic switching ten-way valve are respectively connected with two ends of the second quantitative ring, the fourth port of the first automatic switching ten-way valve is connected with one end of the third carrier gas channel, the fifth port of the first automatic switching ten-way valve is connected to the first exhaust channel, the sixth port and the ninth port of the first automatic switching ten-way valve are respectively connected with two ends of the second chromatographic column, the seventh port of the first automatic switching ten-way valve is connected with one end of the third chromatographic column, and the eighth port of the first automatic switching ten-way valve is connected with one end of the second carrier gas channel;
The second port of the second automatic switching ten-way valve is connected with the tail gas recovery device, the third port and the tenth port of the second automatic switching ten-way valve are respectively connected with two ends of the third metering ring, the fourth port of the second automatic switching ten-way valve is connected with one end of the fifth carrier gas channel, the fifth port of the second automatic switching ten-way valve is connected with one end of the fifth chromatographic column, the sixth port and the ninth port of the second automatic switching ten-way valve are respectively connected with two ends of the fourth chromatographic column, the seventh port of the second automatic switching ten-way valve is connected to a second exhaust channel, a second needle valve is arranged on the second exhaust channel, and the eighth port of the second automatic switching ten-way valve is connected with one end of the fourth carrier gas channel;
a first port of the first automatic switching four-way valve is connected with the other end of the third chromatographic column, a second port of the first automatic switching four-way valve is connected with the pulse discharge helium ionization detector, a third port of the first automatic switching four-way valve is connected with the other end of the fifth chromatographic column, and a fourth port of the first automatic switching four-way valve is connected to a third exhaust channel;
The measuring system further comprises a second automatic switching four-way valve;
the first port of the second automatic switching four-way valve is connected with the carrier gas storage device, and the second port of the second automatic switching four-way valve is connected with the first carrier gas channel, the third carrier gas channel, the second carrier gas channel, the fifth carrier gas channel and the other end of the fourth carrier gas channel; the third port of the second automatic switching four-way valve is connected to the other ends of the first exhaust channel, the second exhaust channel and the third exhaust channel; and the fourth port of the second automatic switching four-way valve is connected with a third needle valve.
2. The system for measuring decomposition products in perfluoroisobutyronitrile according to claim 1, further comprising a first planar tee, a second planar tee, a first planar tee, and a second planar tee;
the three ports of the first plane tee are respectively connected with a first carrier gas channel, a second carrier gas channel and one port of the first plane four-way joint;
the other three ports of the first plane four-way valve are respectively connected with a third gas carrying channel, one port of the second plane three-way valve and a second port of the second automatic switching four-way valve;
The other two ports of the second planar tee are respectively connected with a fifth carrier gas channel and a fourth carrier gas channel;
and the four ports of the second planar four-way valve are respectively connected with the first exhaust channel, the second exhaust channel, the third exhaust channel and the third port of the second automatic switching four-way valve.
3. The system according to claim 1, wherein a first needle valve, a second needle valve and a fourth needle valve are provided in the first exhaust passage, the second exhaust passage and the third exhaust passage, respectively, and a first pressure reducing valve and a second pressure reducing valve are provided in outlet positions of the gas sample storage device and the carrier gas storage device, respectively.
4. A method for determining decomposition products in perfluoroisobutyronitrile, characterized in that the method is applied to the determination system according to any one of claims 1 to 3, comprising the steps of:
switching the measurement system to a first state in which the gas sample in the gas sample storage device is stored in the quantitative sampling device;
switching the measurement system to a second state, in the second state, loading a gas sample in a quantitative sampling device into a first separation device and a second separation device by a carrier gas device, wherein the first separation device separates a first decomposition product from the gas sample, the second separation device pre-separates the gas sample to obtain a pre-separated second decomposition product, and a hydrogen flame ionization detector detects the content of each component in the first decomposition product;
Switching the measurement system to a third state, and in the third state, performing secondary separation on the pre-separated second decomposition product by a second separation device, and detecting the content of each component in the second decomposition product by a pulse discharge helium ionization detector;
switching the measurement system to a fourth state in which a carrier gas device loads a gas sample in a quantitative sampling device into a third separation device, the third separation device separates a third decomposition product from the gas sample, and a pulse discharge helium ionization detector detects the content of each component in the third decomposition product;
and switching the measuring system to a fifth state, wherein the measuring system is in a closed state in the fifth state.
5. The method according to claim 4, wherein in the first state, the automatic switching six-way valve, the first automatic switching ten-way valve, and the second automatic switching ten-way valve are in a second communication state; the gas sample flows out of the gas sample storage device and fills the first metering ring, the second metering ring and the third metering ring; the second communication state is that the first port and the last port are used as a communication group, and every two ports of the other ports are used as a communication group according to the sequence from the second port to the last-to-last port; the two ports in the communication group are communicated with each other;
In the second state, the automatic switching six-way valve and the first automatic switching ten-way valve are in a first communication state, and the second automatic switching ten-way valve is in a second communication state; the second automatic switching four-way valve is in a first communication state; the carrier gas in the first carrier gas channel loads the gas sample in the first quantitative ring into the first chromatographic column for separation, the obtained first decomposition product enters the hydrogen flame ionization detector for detecting the component content, the carrier gas in the third carrier gas channel loads the gas sample in the second quantitative ring into the second chromatographic column for pre-separation, and the light component obtained by the pre-separation is emptied through the first needle valve; the first communication state is that every two ports are used as a communication group according to the sequence from the first port to the last port;
in the third state, the automatic switching six-way valve, the first automatic switching ten-way valve and the second automatic switching ten-way valve are in a second communication state, and the first automatic switching four-way valve and the second automatic switching four-way valve are in a first communication state; the carrier gas in the second carrier gas channel loads the pre-separated second decomposition product in the second chromatographic column into a third chromatographic column, the third chromatographic column carries out secondary separation on the pre-separated second decomposition product, and the obtained second decomposition product enters a pulse discharge helium ionization detector to detect the component content;
In the fourth state, the automatic switching six-way valve, the first automatic switching ten-way valve and the first automatic switching four-way valve are in a second communication state, the second automatic switching ten-way valve and the second automatic switching four-way valve are in a first communication state, a fifth carrier gas channel loads a gas sample in a third quantitative ring into a fourth chromatographic column for pre-separation, a pre-separated third decomposition product enters a fifth chromatographic column for secondary separation, and a secondarily separated third decomposition product enters a pulse discharge helium ionization detector for detecting the component content;
in the fifth state, the automatic switching six-way valve, the first automatic switching ten-way valve, the second automatic switching ten-way valve, the first automatic switching four-way valve and the second automatic switching four-way valve are all in a second communication state, and heavy components in the fourth chromatographic column are emptied through a second needle valve.
CN202210257393.9A 2022-03-16 2022-03-16 System and method for measuring decomposition products in perfluoroisobutyronitrile Active CN114609283B (en)

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