CN114609283A - 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
CN114609283A
CN114609283A CN202210257393.9A CN202210257393A CN114609283A CN 114609283 A CN114609283 A CN 114609283A CN 202210257393 A CN202210257393 A CN 202210257393A CN 114609283 A CN114609283 A CN 114609283A
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way valve
automatic switching
carrier gas
port
chromatographic column
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CN114609283B (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 a decomposition product in perfluoroisobutyronitrile, wherein the system comprises the following components: the device comprises a quantitative sampling device, a carrier gas component, 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 the 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 determining a decomposition product in perfluoroisobutyronitrile.
Background
Sulfur hexafluoride (SF)6) The sulfur hexafluoride (SF) is widely applied to industries such as gas insulation combined electrical equipment, semiconductor etching, smelting and the like due to excellent chemical stability, good arc extinguishing performance and thermodynamic stability6) Has a global warming potential of 23500 times that of carbon dioxide (CO2), and can be stably existed in the atmosphere for 3200 years. To reduce sulfur hexafluoride (SF)6) Emission of sulfur hexafluoride (SF) is sought6) An alternative insulating gas. In 2014, AlSton, France, in combination with 3M of the United states, introduced environmentally friendly hybrid gas as perfluorobutaneNitrile (C)4F7N) as the main mixed insulating gas, and the environmental protection type pipeline transmission key technology which is a special item of the national key research and development plan realizes C4F7The domestic preparation of N gas raises C in China4F7Development and application of N gas are hot.
C4F7In the process of operating N gas insulation equipment, the production of tetrafluoroethylene (C) is inevitable2F4) Hexafluoroethane (C)2F6) Hexafluoropropylene (C)3F6) Octafluoropropane (C)3F8) Trifluoro-acetonitrile (CF)3CN), ethanedinitrile (CNCN), pentafluoropropionitrile (C)2F5CN), dimethyldifluorobutene ((CH)3)2C＝CF2) The products of the equal decomposition have important significance for the research and application of the performance of the perfluoroisobutyronitrile by measuring and analyzing nmol/mol level impurity components in the perfluoroisobutyronitrile.
Disclosure of Invention
In view of this, the present invention provides a system and a method for determining a decomposition product in perfluoroisobutyronitrile, so as to achieve determination of the decomposition product in perfluoroisobutyronitrile.
In order to achieve the purpose, the invention provides the following scheme:
an assay system for decomposition products in perfluoroisobutyronitrile, the assay system comprising: the device comprises a quantitative sampling device, a carrier gas component, 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 a 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 pulsed 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 pulsed discharge helium ionization detector is used for detecting the content of each component in the second decomposition product;
said third separation means being connected to said pulsed discharge helium ionization detector, said third separation means being for separating a third decomposition product from said 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 includes a first quantitative ring, a second quantitative ring and a third quantitative ring which are connected in sequence;
the first quantitative 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 quantitative 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 the second decomposition product in the gas sample, and the third chromatographic column is used for secondary separation of 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 carrying out secondary separation on the pre-separated third decomposition product.
Optionally, the carrier gas component 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 the 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 second decomposition product pre-separated 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 the heavy component 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 measuring system further includes 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;
a first port of the automatic switching six-way valve is connected with the gas sample storage device, a second port of the automatic switching six-way valve is connected with a first port of the first automatic switching ten-way valve, a third port and a sixth port of the automatic switching six-way valve are respectively connected with two ends of the first quantitative ring, a fourth port of the automatic switching six-way valve is connected with the first chromatographic column, and a 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 gas carrying 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 gas carrying channel;
a second port of the second automatic switching ten-way valve is connected with the tail gas recovery device, a third port and a tenth port of the second automatic switching ten-way valve are respectively connected with two ends of the third quantitative ring, a fourth port of the second automatic switching ten-way valve is connected with one end of the fifth carrier gas channel, a fifth port of the second automatic switching ten-way valve is connected with one end of the fifth chromatographic column, a sixth port and a ninth port of the second automatic switching ten-way valve are respectively connected with two ends of the fourth chromatographic column, a 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 third exhaust channel, and an 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 the third exhaust channel.
Optionally, the measuring system further comprises a second automatic switching four-way valve;
a first port of the second automatic switching four-way valve is connected with the carrier gas storage device, and a second port of the second automatic switching four-way valve is connected with 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; a 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 a fourth port of the second automatic switching four-way valve is connected with a third needle valve.
Optionally, the measuring system further comprises a first planar tee, a second planar tee, a first planar four-way and a second planar four-way;
three ports of the first plane tee joint are respectively connected with a first carrier gas channel, a second carrier gas channel and one port of the first plane tee joint;
the other three ports of the first planar four-way valve are respectively connected with a third gas carrying channel, one port of the second planar three-way valve and a second port of the second automatic switching four-way valve;
the other two ports of the second planar tee joint are respectively connected with a fifth carrier gas channel and a fourth carrier gas channel;
and four ports of the second plane four-way valve are respectively connected with the first exhaust channel, the second exhaust channel, the third exhaust channel and a third port of the second automatic switching four-way valve.
Optionally, a first needle valve, a second needle valve, and a fourth needle valve are respectively disposed on the first exhaust channel, the second exhaust channel, and the third exhaust channel, and a first pressure reducing valve and a second pressure reducing valve are respectively disposed at outlet positions of the gas sample storage device and the carrier gas storage device.
A method for measuring a decomposition product in perfluoroisobutyronitrile is characterized by being applied to a measurement system and comprising the following steps:
switching the assay 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 measuring system to a second state, wherein a gas carrier device loads a gas sample in a quantitative sampling device into a first separation device and a second separation device, 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 assay system to a third state in which the second separation device performs a second separation of the pre-separated second decomposition product and the pulsed discharge helium ionization detector detects the content of each component in the second decomposition product;
switching the assay system to a fourth state in which the carrier gas means loads the gas sample in the quantitative sampling means into a third separation means which separates a third decomposition product from the gas sample, the pulsed discharge helium ionization detector detecting the content of each component in the third decomposition product;
switching the assay system to a fifth state in which the assay system is in a closed state.
Optionally, 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 quantitative ring, the second quantitative ring and the third quantitative 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 component content detection, 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 pre-separated light component is evacuated 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 for component content detection;
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 the second separated third decomposition product enters a pulse discharge helium ionization detector for component content detection;
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 a 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 system for measuring decomposition products in perfluoroisobutyronitrile, which comprises: the device comprises a quantitative sampling device, a carrier gas component, 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 pulsed discharge helium ionization detector, and the third separation device is connected with the pulsed discharge helium ionization detector. The invention is provided with a carrier gas component, three separation devices and two detectors to realize the separation and detection of different decomposition products.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a schematic diagram of the configuration and communication of an assay system in a first state according to an embodiment of the present invention;
FIG. 2 is a schematic diagram of the structure and communication status of the measurement system in a second state according to the embodiment of the present invention;
FIG. 3 is a schematic diagram showing the structure and communication status of a second separation stage measurement system according to an embodiment of the present invention;
FIG. 4 is a schematic diagram illustrating the structure and communication status of a measurement system in a third detection stage according to an embodiment of the present invention;
FIG. 5 is a schematic diagram illustrating the structure and communication status of a measurement system at a detection stage in a fourth state according to an embodiment of the present invention;
FIG. 6 is a schematic diagram illustrating the structure and communication status of a measurement system at a detection stage in a fifth state according to an embodiment of the present invention;
wherein, 1-a gas sample storage device, 2-a first pressure reducing valve, 3-a first quantitative ring, 4-a second quantitative ring, 5-a third quantitative ring, 6-a tail gas recovery device, 7-a first automatic switching six-way valve, 8-a first automatic switching ten-way valve, 9-a second automatic switching ten-way valve, 10-a first carrier gas channel, 11-a first chromatographic column, 12-a hydrogen flame ionization detector, 13-a second chromatographic column, 14-a second carrier gas channel, 15-a first plane tee, 16-a third chromatographic column, 17-a first needle valve, 18-a third carrier gas channel, 19-a fourth chromatographic column, 20-a fourth carrier gas channel, 21-a second needle valve, 22-a fifth chromatographic column, 23-a fifth carrier gas channel, 24-a second pressure reducing valve, 25-a carrier gas storage device, 26-a second automatic switching four-way valve, 27-a third needle valve, 28-a second plane four-way valve, 29-a fourth needle valve, 30-a fifth automatic switching four-way valve and 31-a pulse discharge helium ionization detector.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention aims to provide a system and a method for measuring a decomposition product in perfluoroisobutyronitrile, so as to realize the measurement of the decomposition product in perfluoroisobutyronitrile.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
As shown in fig. 1 to 6, reference numerals (i), (ii), and (iii) in fig. 1 to 6 of the present invention are reference numerals of ports of an automatic switching six-way valve, an automatic switching ten-way valve, and an automatic switching four-way valve, which respectively correspond to a first port, a second port, a third port, and the like in the embodiment of the present invention, and also correspond to a first port (minimum reference numeral (i)) and a last port (maximum reference numerals, for example, maximum reference numerals (e.g., sixth, third, and fourth)) 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 a decomposition product in perfluoroisobutyronitrile, which should include:
the device for measuring the content of the components of trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethyl difluorobutene comprises a separation passage, wherein a first chromatographic column 11 for separating trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethyl difluorobutene is arranged on the separation passage, a carrier gas end of the separation passage is communicated with a first carrier gas channel 10 for introducing a gas sample into the first chromatographic column 11 through a multi-way switching valve, an outlet end of the separation passage is communicated with a first chromatographic column 11 for separating trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethyl difluorobutene through a first automatic switching six-way valve 7, the first carrier gas channel 10, the first chromatographic column 11 are sequentially communicated along the gas flowing direction, and an outlet end of the first chromatographic column 11 is provided with a device for detecting trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethyl difluorobutene, A hydrogen flame ionization detector 12 for detecting the contents of ethanedinitrile, pentafluoropropionitrile, and dimethyldifluorobutene components;
the device for measuring the content of the components of carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane comprises a separation passage, wherein a second chromatographic column 13 and a third chromatographic column 16 for separating the components of carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane are arranged on the separation passage, a carrier gas end of the separation passage is communicated with a third carrier gas channel 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 the second chromatographic column 13 for separating the components of carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane through the first automatic switching ten-way valve 8, and the third carrier gas channel 18, a second quantitative ring 4, the second chromatographic column 13, The second carrier gas channel 14 and the third chromatographic column 16 are sequentially communicated along the gas flowing direction, and the outlet end of the third chromatographic column 16 is provided with a pulse discharge helium ionization detector 31 for detecting the contents of the components of carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane;
the device for measuring the component content of carbon monoxide and carbon tetrafluoride 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 are arranged on the separation passage, the carrier gas end of the separation passage is communicated with a fifth carrier gas channel 23 for introducing a gas sample into the fourth chromatographic column 19 through a second automatic switching ten-way valve 9, the outlet end of the separation passage is communicated with a fifth chromatographic column 22 for separating carbon monoxide and carbon tetrafluoride through the second automatic switching ten-way valve 9, the fifth carrier gas channel 23, the third quantitative ring 5, the fourth chromatographic column 19, the fourth carrier gas channel 20 and the fifth chromatographic column 22 are sequentially communicated along the direction of gas flow, the outlet end of the fifth chromatographic column 22 is provided with a pulse discharge helium ionization detector 31 for detecting the component contents of carbon monoxide and carbon tetrafluoride.
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 components, wherein the quantitative measuring device is arranged on a gas sample passage and is a quantitative ring, and the carbon monoxide, the carbon tetrafluoride, the carbon dioxide, the tetrafluoroethylene, the hexafluoroethane, the hexafluoropropylene, the octafluoropropane, the trifluoroacetonitrile, the ethanedinitrile, the pentafluoropropionitrile and the dimethyl difluorobutene components in the gas sample are accurately measured.
Specifically, as shown in fig. 1 to 6, an embodiment of the present invention provides a system for measuring a decomposition product in perfluoroisobutyronitrile, including: a quantitative sampling device, a carrier gas component, a first separation device, a second separation device, a third separation device, a hydrogen flame ionization detector 12 and a pulse discharge helium ionization detector 31; the quantitative sampling device is connected with a 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 12, 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 12 is used for detecting the content of each component in the first decomposition product; the second separation device is connected with the pulsed discharge helium ionization detector 31, 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 pulsed discharge helium ionization detector 31 is used for detecting the content of each component in the second decomposition product; said third separation means being connected to said pulsed discharge helium ionization detector 31 for separating a third decomposition product from said gas sample; the third decomposition product comprises carbon monoxide and/or carbon tetrafluoride; the pulsed 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 connected in sequence; the first quantitative ring 3 is also connected with the gas sample storage device, the carrier gas component and the first separation device respectively; the second quantitative ring 4 is also connected with the carrier gas component and the second separation device respectively; the third quantitative ring 5 is also respectively connected with the carrier gas component, the third separation device and the tail gas recovery device 6. The first dosing ring 3, the second dosing ring 4 and the third dosing ring 5 in the present embodiment 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 decomposition product in the gas sample, and the third chromatographic column 16 is used for carrying out secondary separation on the pre-separated second decomposition product; the third separation device comprises a fourth chromatographic column 19 and a fifth chromatographic column 22, wherein the fourth chromatographic column 19 is used for pre-separating the third decomposition product in the gas sample, and the fifth chromatographic column 22 is used for carrying out secondary separation on the pre-separated third decomposition product.
The carrier gas component comprises 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 to the first quantitative ring 3, and the first carrier gas channel 10 is used for loading the 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 quantitative ring 5, and the fifth carrier gas channel 23 is used for loading the gas sample in the third quantitative 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 the heavy component in the fourth chromatographic column 19 into the 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 also 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; a first port of the automatic switching six-way valve is connected with the gas sample storage device, a second port of the automatic switching six-way valve is connected with a first port of the first automatic switching ten-way valve 8, a third port and a sixth port of the automatic switching six-way valve are respectively connected with two ends of the first quantitative ring 3, a fourth port of the automatic switching six-way valve is connected with the first chromatographic column 11, and a fifth port of the automatic switching six-way valve is connected with one end of the first carrier gas channel 10; a second port of the first automatic switching ten-way valve 8 is connected to a first port of the second automatic switching ten-way valve 9, a third port and a tenth port of the first automatic switching ten-way valve 8 are respectively connected to two ends of the second quantitative ring 4, a fourth port of the first automatic switching ten-way valve 8 is connected to one end of the third carrier gas channel 18, a fifth port of the first automatic switching ten-way valve 8 is connected to the first exhaust gas channel, a sixth port and a ninth port of the first automatic switching ten-way valve 8 are respectively connected to two ends of the second chromatographic column 13, a seventh port of the first automatic switching ten-way valve 8 is connected to one end of the third chromatographic column 16, and an eighth port of the first automatic switching ten-way valve 8 is connected to one end of the second carrier gas channel 14; a second port of the second automatic switching ten-way valve 9 is connected with the tail gas recovery device 6, a third port and a tenth port of the second automatic switching ten-way valve 9 are respectively connected with two ends of the third quantitative ring 5, a fourth port of the second automatic switching ten-way valve 9 is connected with one end of the fifth carrier gas channel 23, a fifth port of the second automatic switching ten-way valve 9 is connected with one end of the fifth chromatographic column 22, a sixth port and a ninth port of the second automatic switching ten-way valve 9 are respectively connected with two ends of the fourth chromatographic column 19, a seventh port of the second automatic switching ten-way valve 9 is connected with a second exhaust channel, a second needle valve 21 is arranged on the third exhaust channel, and an eighth port of the second automatic switching ten-way valve 9 is connected with one end of the fourth carrier gas channel 20; a first port of the first automatic switching four-way valve 30 is connected to the other end of the third chromatographic column 16, a second port of the first automatic switching four-way valve 30 is connected to the pulsed discharge helium ionization detector 31, a third port of the first automatic switching four-way valve 30 is connected to the other end of the fifth chromatographic column 22, and a fourth port of the first automatic switching four-way valve 30 is connected to a third exhaust channel.
The assay system further comprises a second automatic switching four-way valve 26; a first port of the second automatic switching four-way valve 26 is connected to the carrier gas storage device 25, and a second port of the second automatic switching four-way valve 26 is connected to the other ends of 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 fourth carrier gas channel 20; a 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 to a third needle valve 27.
The measuring system also comprises a first plane tee 15, a second plane tee, a first plane cross and a second plane cross 28; 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 planar four-way are respectively connected with the third air carrying channel 18, one port of the second planar 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 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, respectively.
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 determining decomposition products in perfluoroisobutyronitrile, which comprises the following steps:
the determination process of the components of the trifluoroacetonitrile, the ethanedinitrile, the pentafluoropropionitrile and the dimethyl difluorobutene comprises 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 components of trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethyl difluorobutene: the tail gas outlet end of the analysis chromatographic column is communicated with a hydrogen flame ionization detector 12, components of trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethyl difluorobutene which flow out of the first chromatographic column 11 enter the hydrogen flame ionization detector 12, and the content of the components is measured by the hydrogen flame ionization detector 12.
The content determination process of the components of carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane is as follows: 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 the components of carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane: the gas outlet tail end of the third chromatographic column 16 is communicated with a pulse discharge helium ionization detector 31, components of carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane 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 determination process of the 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 the components of carbon monoxide and carbon tetrafluoride: the tail gas outlet end of the fifth chromatographic column 22 is communicated with a pulse discharge helium ionization detector 31, 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 components is measured by the pulse discharge helium ionization detector 31.
The method for determining the decomposition product in the perfluoroisobutyronitrile provided by the invention 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 six-way valve and the first automatic valve are automatically switchedThe ten-way switching valve 8 and the ten-way second automatic switching valve 9 are in a second communication state; the gas sample flows from the gas sample storage means and fills the first dosing ring 3, the second dosing ring 4 and the third dosing ring 5. Namely, the process is a process of quantitatively measuring a gas sample, and the specific implementation mode is as follows: as shown in fig. 1, after the gas sample components are decompressed from the gas sample storage device 1 through the first decompression valve 2, the gas sample components are connected to the No. 1 port, the No. 6 port, the first quantitative ring 3, and the No. 3 port of the first automatic switching six-way valve 7 through the gas path connecting pipe, then flow from the No. 2 port to the No. 1 port, the No. 10 port, the second quantitative ring 4, and the No. 3 port of the first automatic switching ten-way valve 8, flow from the No. 2 port to the No. 1 port, the No. 10 port, the third quantitative ring 5, and the No. 3 port of the second automatic switching ten-way valve 9, and finally flow from the No. 2 port to the tail gas recovery device 6. The embodiment of the invention quantitatively measures the gas sample by one-time ventilation, thereby ensuring carbon monoxide (CO) and carbon tetrafluoride (CF)4) Carbon dioxide (CO)2)Tetrafluoroethylene (C)2F4) Hexafluoroethane (C)2F6) Hexafluoropropylene (C)3F6) Octafluoropropane (C)3F8) Trifluoro-acetonitrile (CF)3CN), ethanedinitrile (CNCN), pentafluoropropionitrile (C)2F5CN), dimethyldifluorobutene ((CH)3)2C＝CF2) The separation degree of the components also ensures the separation of carbon monoxide (CO) and carbon tetrafluoride (CF)4) Carbon dioxide (CO)2)Tetrafluoroethylene (C)2F4) Hexafluoroethane (C)2F6) Hexafluoropropylene (C)3F6) Octafluoropropane (C)3F8) Trifluoro-acetonitrile (CF)3CN), ethanedinitrile (CNCN), pentafluoropropionitrile (C)2F5CN), dimethyldifluorobutene ((CH)3)2C＝CF2) The accuracy of component detection and the analysis period are short. The components do not interfere 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 the carrier gas device loads the gas sample in the quantitative sampling device into a first separation device and a second separation device, 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 the 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 connection state; 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, 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 ring 4 into the second chromatographic column 13 for pre-separation, and the light component obtained by pre-separation is exhausted through the first needle valve 17. The process of detecting the component content of the first decomposition product entering the hydrogen flame ionization detector 12 by the carrier gas in the first carrier gas channel 10 to load the gas sample in the first quantitative ring 3 into the first chromatographic column 11 for separation is the determination process of the component content 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 separated trifluoroacetonitrile, ethanedinitrile, pentafluoropropionitrile and dimethyldifluorobutene components in the first chromatographic column 11 for measurement by the hydrogen 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 emptying the pre-separated light component through the first needle valve 17 is a pre-determination process of the content of the components of carbon dioxide, tetrafluoroethylene, hexafluoroethane, hexafluoropropylene and octafluoropropane: as shown in fig. 2, the third gas carrying channel 18 carries the gas sample in the second quantitative ring 4 into the second chromatographic column 13, and the light components such as oxygen and nitrogen separated from the second chromatographic column 13 are evacuated by the first needle valve 17.
Switching the assay system to a third state in which the second separation device performs a second separation of the pre-separated second decomposition product and the pulsed 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 the second communication state, and the first automatic switching four-way valve 30 and the second automatic switching four-way valve 26 are in the 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 performs secondary separation on the pre-separated second decomposition product, and the obtained second decomposition product enters the pulse discharge helium ionization detector 31 for component content detection. The 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 component is separated from the second chromatographic column 13, fig. 2 is switched to fig. 3, and is 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 are measured by the pulse discharge helium ionization detector 31.
Switching the assay system to a fourth state in which the carrier gas means loads the gas sample in the quantitative sampling means into a third separation means which separates a third decomposition product from the gas sample, the pulsed discharge helium ionization detector 31 detecting 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 the second communication state, the second automatic switching ten-way valve 9 and the second automatic switching four-way valve 26 are in the first communication state, the fifth carrier gas channel 23 loads the gas sample in the third quantitative loop 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 second separated third decomposition product enters the pulse discharge helium ionization detector 31 for component content detection. The process is a measuring process of the content of the components of carbon monoxide and carbon tetrafluoride: as shown in fig. 5, the fifth carrier gas channel 23 carries the gas sample in the third quantitative loop 5 into the fourth chromatographic column 19, the fourth chromatographic column 19 pre-separates the carbon monoxide and the carbon tetrafluoride component, the pre-separated carbon monoxide and carbon tetrafluoride component flow to 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 pulsed discharge helium ionization detector 31.
Switching the assay system to a fifth state in which the assay system is in a closed 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 heavy components in the fourth chromatographic column 19 are emptied through the second needle valve 21. The process includes the process of evacuating the heavy components such as hexafluoropropylene and octafluoropropane 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 switched to the state of fig. 6, the system is in a closed state, and the system is prevented from permeating air in an analysis state to influence the stability time of the next start-up.
According to the specific embodiment provided by the invention, the invention discloses the following technical effects:
the invention uses multi-path carrier gas multi-chromatographic column multi-detector to separate carbon monoxide (CO) and carbon tetrafluoride (CF)4) Carbon dioxide (CO)2)Tetrafluoroethylene (C)2F4) Hexafluoroethane (C)2F6) Hexafluoropropylene (C)3F6) Octafluoropropane (C)3F8) Trifluoro-acetonitrile (CF)3CN), ethanedinitrile (CNCN), pentafluoropropionitrile (C)2F5CN), dimethyldifluorobutene ((CH)3)2C＝CF2) The components are completely separated, and simultaneously, the carbon monoxide (CO) and the carbon tetrafluoride (CF) are ensured4) Carbon dioxide (CO)2)Tetrafluoroethylene (C)2F4) Hexafluoroethane (C)2F6) Hexafluoropropylene (C)3F6) Octafluoropropane (C)3F8) Trifluoro-acetonitrile (CF)3CN), ethanedinitrile (CNCN), pentafluoropropionitrile (C)2F5CN), dimethyldifluorobutene ((CH)3)2C＝CF2) The accuracy of component detection and the analysis period are short.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other.
The principle and the embodiment of the present invention are explained by applying specific examples, and the above description of the embodiments is only used to help understanding the method and the core idea of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.

Claims (10)

1. A system for measuring a decomposition product in perfluoroisobutyronitrile, characterized by comprising: the device comprises a quantitative sampling device, a carrier gas component, 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 a 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 pulsed 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 pulsed discharge helium ionization detector is used for detecting the content of each component in the second decomposition product;
said third separation means being connected to said pulsed discharge helium ionization detector, said third separation means being for separating a third decomposition product from said 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.
2. The system for measuring a decomposition product in perfluoroisobutyronitrile according to claim 1, wherein the quantitative sampling means comprises a first quantitative ring, a second quantitative ring, and a third quantitative ring connected in this order;
the first quantitative 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 quantitative ring is also respectively connected with the carrier gas component, the third separation device and the tail gas recovery device.
3. The system according to claim 2, wherein the first separation device comprises a first chromatographic column for separating the first decomposition product in the gas sample, the second separation device comprises a second chromatographic column for pre-separating the second decomposition product in the gas sample and a third chromatographic column for secondary separation of 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 carrying out secondary separation on the pre-separated third decomposition product.
4. The system for measuring decomposition products in perfluoroisobutyronitrile according to claim 3, wherein the carrier gas component 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 the 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 second decomposition product pre-separated 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 the 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.
5. The system for measuring decomposition products in perfluoroisobutyronitrile according to claim 4, wherein the 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;
a first port of the automatic switching six-way valve is connected with the gas sample storage device, a second port of the automatic switching six-way valve is connected with a first port of the first automatic switching ten-way valve, a third port and a sixth port of the automatic switching six-way valve are respectively connected with two ends of the first quantitative ring, a fourth port of the automatic switching six-way valve is connected with the first chromatographic column, and a 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 gas carrying 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 gas carrying channel;
a second port of the second automatic switching ten-way valve is connected with the tail gas recovery device, a third port and a tenth port of the second automatic switching ten-way valve are respectively connected with two ends of the third quantitative ring, a fourth port of the second automatic switching ten-way valve is connected with one end of the fifth carrier gas channel, a fifth port of the second automatic switching ten-way valve is connected with one end of the fifth chromatographic column, a sixth port and a ninth port of the second automatic switching ten-way valve are respectively connected with two ends of the fourth chromatographic column, a 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 an 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 the third exhaust channel.
6. The system for measuring a decomposition product in perfluoroisobutyronitrile according to claim 5, further comprising a second automatic switching four-way valve;
a first port of the second automatic switching four-way valve is connected with the carrier gas storage device, and a second port of the second automatic switching four-way valve is connected with 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; a 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 a fourth port of the second automatic switching four-way valve is connected with a third needle valve.
7. The system for determining a decomposition product in perfluoroisobutyronitrile according to claim 6, wherein the system further comprises a first planar tee, a second planar tee, a first planar cross, and a second planar cross;
three ports of the first plane tee joint are respectively connected with a first carrier gas channel, a second carrier gas channel and one port of the first plane tee joint;
the other three ports of the first planar four-way valve are respectively connected with a third gas carrying channel, one port of the second planar three-way valve and a second port of the second automatic switching four-way valve;
the other two ports of the second planar tee joint are respectively connected with a fifth carrier gas channel and a fourth carrier gas channel;
and 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 a third port of the second automatic switching four-way valve.
8. The system according to claim 6, wherein the first exhaust passage, the second exhaust passage, and the third exhaust passage are provided with a first needle valve, a second needle valve, and a fourth needle valve, respectively, and the gas sample storage device and the carrier gas storage device are provided with a first pressure reducing valve and a second pressure reducing valve, respectively, at their outlet positions.
9. A method for measuring a decomposition product in perfluoroisobutyronitrile, which is applied to the measurement system according to any one of claims 1 to 8, the method comprising the steps of:
switching the assay 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 measuring system to a second state, wherein a gas carrier device loads a gas sample in a quantitative sampling device into a first separation device and a second separation device, 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 assay system to a third state in which the second separation device performs a second separation of the pre-separated second decomposition product and the pulsed discharge helium ionization detector detects the content of each component in the second decomposition product;
switching the assay system to a fourth state in which the carrier gas means loads the gas sample in the quantitative sampling means into a third separation means which separates a third decomposition product from the gas sample, the pulsed discharge helium ionization detector detecting the content of each component in the third decomposition product;
switching the assay system to a fifth state in which the assay system is in a closed state.
10. The method according to claim 9, wherein in the first state, the automatically switching six-way valve, the first automatically switching ten-way valve, and the second automatically 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 quantitative ring, the second quantitative ring and the third quantitative 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 rest ports are used as a communication group according to the sequence from the second port to the penultimate 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 component content detection, 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 pre-separated light component is evacuated 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 port at the last end;
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 for component content detection;
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 the fifth chromatographic column for secondary separation, and the second-separated third decomposition product enters a pulse discharge helium ionization detector for component content detection;
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 a fourth chromatographic column are emptied through a second needle valve.
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