CN109507275B - Mass spectrum detection system and method for insulating gas discharge decomposition products in GIS - Google Patents

Mass spectrum detection system and method for insulating gas discharge decomposition products in GIS Download PDF

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Publication number
CN109507275B
CN109507275B CN201811329801.7A CN201811329801A CN109507275B CN 109507275 B CN109507275 B CN 109507275B CN 201811329801 A CN201811329801 A CN 201811329801A CN 109507275 B CN109507275 B CN 109507275B
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discharge
detection system
electrode rod
mass
ionization source
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CN109507275A (en
Inventor
张友鹏
荣命哲
刘庆
马庆
李永林
王小华
赵晓民
杨爱军
韩桂全
刘家霖
韩国辉
傅熊雄
毕迎华
李旭旭
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Xian Jiaotong University
Pinggao Group Co Ltd
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Xian Jiaotong University
Pinggao Group Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N27/00Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/62Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
    • G01N27/64Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode using wave or particle radiation to ionise a gas, e.g. in an ionisation chamber

Abstract

The utility model discloses a mass spectrometry detection system of insulating gas discharge decomposition product in GIS, includes discharge chamber, anion ionization source and mass spectrograph. The disclosure also discloses a method for detecting the discharge decomposition product of the insulating gas in the GIS. The present disclosure is capable of directly detecting the composition of the insulating gas in the GIS without the aid of other tools and techniques.

Description

Mass spectrum detection system and method for insulating gas discharge decomposition products in GIS
Technical Field
The disclosure belongs to the field of gas component detection, and particularly relates to a mass spectrum detection system and method for an insulating gas discharge decomposition product in a GIS.
Background
Gas Insulated metal enclosed switchgear gis (gas Insulated switchgear) is a sealed metal enclosure that encloses the main components of circuit breakers, disconnectors, earthing switches, busbars, transformers, arresters, etc., and is filled with insulating gas as the insulating and arc extinguishing medium. Traditional GIS equipment mainly uses SF6As an insulating and arc-extinguishing medium, the new GIS is also frequently used and SF6The strong electronegative gas with similar properties is used as an insulating and arc extinguishing medium. Since the gas medium in the GIS device undertakes the work of insulation and arc extinction, and may be decomposed into toxic and harmful gases during discharge or affect the insulation and arc extinction performance of the device, it is necessary to study the decomposition condition under the action of current.
At present, the mass spectrometry detection method adopting the commonly used 70eV electron collision has the following problems: (1) the gas molecules to be detected can be bombarded into small fragments by high electron energy, the specific identification capability of different components with similar structures is lacked, and when the detected gas contains a large amount of components with similar chemical compositions and structures, the situation becomes extremely complicated by adopting the traditional mass spectrometry detection method of electron collision, and other tools and technologies are often needed to assist in identifying and analyzing the gas components; (2) SF is commonly used in GIS equipment6The typical electronegative gas is used as an insulating and arc extinguishing medium, and a bulk material of the electronegative gas has strong electronegativity, so that an unstable excited state is formed by adopting a traditional ionization mode, and a stable positively charged ionic group is difficult to form, thereby bringing difficulty to subsequent detection.
Disclosure of Invention
In view of the above disadvantages, the present disclosure aims to provide a mass spectrometry detection system and method for insulation gas discharge decomposition products in a GIS, which can solve the problems of difficult resolution due to similar chemical compositions of different products and positive ion instability due to strong electronegativity after gas decomposition in the existing GIS equipment by simulating various discharge conditions in the GIS equipment, ionizing gas components to be detected by negative ion ionization, deflecting ions with different mass-to-charge ratios under the action of a magnetic field, and detecting.
The purpose of the present disclosure is achieved by the following technical solutions.
A mass spectrometry detection system for dielectric gas discharge decomposition products in a GIS, comprising:
the device comprises a discharge cavity, a negative ion ionization source and a mass spectrometer;
the discharge cavity is sequentially connected with the anion ionization source and the mass spectrometer through a pipeline; wherein the content of the first and second substances,
the discharge cavity is used for discharging and decomposing the insulating gas;
the negative ion ionization source is used for ionizing the decomposed composition of the insulating gas;
the mass spectrometer is used for detecting the mass-to-charge ratio of each component in the plasma generated by the ionization of the composition.
Preferably, the discharge cavity comprises a cavity body, an upper electrode rod and a lower electrode rod; the outer side of the upper electrode rod is wrapped with an upper insulating sleeve, an upper rotary sealing gland is positioned at the top end of the upper insulating sleeve and used for sealing a gap between the upper insulating sleeve and the upper electrode rod, and one end of the upper electrode rod, which extends into the cavity body, is connected with a static contact; the outer side of the lower electrode rod is wrapped by a lower insulating sleeve, a lower rotary sealing gland is located at the bottom end of the lower insulating sleeve and used for sealing a gap between the lower insulating sleeve and the lower electrode rod, one end, extending into the cavity body, of the lower electrode rod is connected with a moving contact, and the contact distance between the moving contact and the fixed contact is controlled through a manual lifting tray.
Preferably, the discharge cavity further comprises observation windows, and the observation windows are arranged on two sides of the cavity body.
Preferably, the material for preparing the upper insulating sleeve and the lower insulating sleeve is thermosetting resin.
Preferably, the thermosetting resin is an epoxy resin.
Preferably, the negative ion ionization source is an electrospray vacuum ultraviolet ionization source.
The present disclosure also provides a method for detecting a decomposition product of an insulating gas in a GIS, comprising the steps of:
s100: vacuumizing the mass spectrum detection system, and injecting insulating gas for GIS equipment into the discharge cavity;
s200: applying external voltage to the discharge cavity to discharge and decompose the insulating gas;
s300: introducing the composition decomposed by the discharge of the insulating gas into a negative ion ionization source for ionization;
s400: and introducing plasma generated by ionizing the composition into a mass spectrometer for mass-to-charge ratio detection.
Preferably, the negative ion ionization source is an electrospray vacuum ultraviolet ionization source.
Compared with the prior art, the beneficial effect that this disclosure brought does:
1. the types and the number of fragment peaks formed in the detection process are greatly reduced, and the gas components in the decomposition products can be identified without other tools and technologies.
2. The present disclosure selects negative ions to generate negative ions, which are more stable than positive ions, and can be directly detected.
Drawings
FIG. 1 is a schematic diagram of a mass spectrometric detection system for dielectric gas discharge decomposition products in a GIS according to the present disclosure;
FIG. 2 is a schematic diagram of the structure of the discharge chamber of FIG. 1;
FIG. 3 is a flow chart of a method for mass spectrometric detection of dielectric gas discharge decomposition products in a GIS according to the present disclosure;
FIG. 4 shows SF detection using prior art methods6Obtaining a mass spectrogram;
FIG. 5 is a diagram of SF detection using the method of FIG. 36The mass spectrum obtained.
Detailed Description
The technical solution of the present disclosure is described in detail below with reference to the accompanying drawings and examples.
Referring to fig. 1, a mass spectrometry detection system for insulation gas discharge decomposition products in a GIS, comprising: the device comprises a discharge cavity, a negative ion ionization source and a mass spectrometer;
the discharge cavity is sequentially connected with the anion ionization source and the mass spectrometer through a pipeline; wherein the content of the first and second substances,
the discharge cavity is used for discharging and decomposing the insulating gas;
the negative ion ionization source is used for ionizing the decomposed composition of the insulating gas;
the mass spectrometer is used for detecting the mass-to-charge ratio of each component in the plasma generated by the ionization of the composition.
The above embodiment constitutes a complete technical scheme of the present disclosure, negative ions are formed by performing negative ion ionization on the discharge decomposition product of the insulating gas to be detected, the negative ions enter the mass spectrometer, are accelerated under the action of an electric field and are deflected under the action of a magnetic field, and the negative ions with different mass-to-charge ratios are separated and then directly detect the components of the insulating gas.
In another embodiment, referring to fig. 2, the discharge chamber includes a chamber body, an upper electrode rod 1, and a lower electrode rod 8; the outer side of the upper electrode rod 1 is wrapped with an upper insulating sleeve 3, an upper rotary sealing gland 2 is positioned at the top end of the upper insulating sleeve 3 and used for sealing a gap between the upper insulating sleeve 3 and the upper electrode rod 1, and one end, extending into the cavity body, of the upper electrode rod 1 is connected with a static contact 4-1; the outer side of the lower electrode rod 8 is wrapped by a lower insulating sleeve 6, a lower rotary sealing gland 7 is located at the bottom end of the lower insulating sleeve 6 and used for sealing a gap between the lower insulating sleeve 6 and the lower electrode rod 8, one end, extending into the cavity body, of the lower electrode rod 8 is connected with a movable contact 4-2, and the contact distance between the movable contact and the fixed contact is controlled through a manual lifting tray 9.
In the embodiment, an experimental power supply is provided by a 0-50 kV voltage-adjustable corona-free test transformer, two poles of the power supply are connected with an upper electrode rod 1 and a lower electrode rod 8 of a discharge cavity after passing through a protective resistor, voltage is applied between a moving contact 4-2 and a static contact 4-1 in the cavity through the two electrode rods, after the voltage between the moving contact 4-2 and the static contact 4-1 exceeds the breakdown voltage of insulating gas in the cavity, the insulating gas is broken down to form an electric arc, and the insulating gas in the cavity starts to decompose under the action of the electric arc.
In another embodiment, the discharge cavity further comprises an observation window 5, and the observation window 5 is disposed on two sides of the cavity body.
In this embodiment, through setting up the observation window 5 in the cavity both sides that discharges, be convenient for observe the inside condition of discharging of cavity.
In another embodiment, the material for preparing the upper insulating sheath 3 and the lower insulating sheath 6 is thermosetting resin.
In this embodiment, the thermosetting resin has excellent electrical insulating properties, and includes phenol resin, urea resin, melamine-formaldehyde resin, epoxy resin, unsaturated resin, polyurethane, polyimide, and the like, and epoxy resin is preferably used in this embodiment.
In another embodiment, the negative ion ionization source is an electrospray vacuum ultraviolet ionization source.
In the embodiment, the insulating gas decomposition product is introduced into the high-vacuum ionization chamber by using electrospray, the decomposition product is ionized by vacuum ultraviolet light with adjustable wavelength in an ionization region, and as the decomposition product is generally polyfluoride and has strong electronegativity, negative ions are directly generated in an electron capture mode.
In another embodiment, referring to fig. 3, the present disclosure further provides a method for detecting an insulation gas discharge decomposition product in a GIS, comprising the steps of:
s100: vacuumizing the mass spectrum detection system, and injecting insulating gas for GIS equipment into the discharge cavity;
s200: applying external voltage to the discharge cavity to discharge and decompose the insulating gas;
s300: introducing the composition decomposed by the discharge of the insulating gas into a negative ion ionization source for ionization;
s400: and introducing plasma generated by ionizing the composition into a mass spectrometer for mass-to-charge ratio detection.
In another embodiment, the negative ion ionization source is an electrospray vacuum ultraviolet ionization source.
FIG. 4 shows SF detection using prior art methods6The mass spectrum obtained. The gas to be measured is pureSF6Gas, detected using conventional mass spectrometry. During the detection process, SF is ionized due to electron bombardment6The molecules are ionized to SF+、SF2 +、SF3 +、SF4 +And SF5 +When a plurality of positive ions exist, a mass spectrogram has a large number of fragment peaks, and the pure SF is difficult to distinguish the composition of the gas to be detected without other means6Whether the gas is a plurality of SFxA mixed gas of gases; at the same time, due to SF6 +Unstable, molecular ion peak SF should appear6 +And the method does not exist, and brings difficulty to detection work.
FIG. 5 is a diagram of SF detection using the detection method designed by this disclosure6The mass spectrum obtained. The measured gas is pure SF6Gas, when the fragment peak appearing on the spectrogram is only SF5 -One, while the conventional scheme produces six fragmentation peaks; meanwhile, the spectrogram obtained by adopting the scheme directly shows the SF corresponding to the SF to be detected6SF of gas6 -Peaks, whereas no SF appears in the mass spectrum of the conventional protocol6 +Peak(s).
Compared with the conventional mass spectrometry detection method, the method for detecting the strong electronegative gas in the GIS has the advantages that the types and the quantity of fragments generated during detection are less, the problem that molecular ions of polyfluoride are unstable and difficult to directly detect is solved, and great convenience is provided for subsequent qualitative analysis of gas components. Therefore, the scheme is a simple and effective method for detecting and analyzing the strong electronegative gas substances in the GIS.
The above description is only a preferred embodiment of the present disclosure and should not be interpreted as limiting the scope of the present disclosure, it should be noted that those skilled in the art can make various changes and modifications without departing from the spirit of the present disclosure, which falls within the protection scope of the present disclosure.

Claims (7)

1. A mass spectrometry detection system for dielectric gas discharge decomposition products in a GIS, comprising: the device comprises a discharge cavity, a negative ion ionization source and a mass spectrometer;
the discharge cavity is sequentially connected with the anion ionization source and the mass spectrometer through a pipeline; wherein the content of the first and second substances,
the discharge cavity is used for discharging and decomposing the insulating gas;
the discharge cavity comprises a cavity body, an upper electrode rod and a lower electrode rod; the outer side of the upper electrode rod is wrapped with an upper insulating sleeve, an upper rotary sealing gland is positioned at the top end of the upper insulating sleeve and used for sealing a gap between the upper insulating sleeve and the upper electrode rod, and one end of the upper electrode rod, which extends into the cavity body, is connected with a static contact; the outer side of the lower electrode rod is wrapped with a lower insulating sleeve, a lower rotary sealing gland is positioned at the bottom end of the lower insulating sleeve and used for sealing a gap between the lower insulating sleeve and the lower electrode rod, one end of the lower electrode rod, which extends into the cavity body, is connected with a movable contact, and the contact distance between the movable contact and the fixed contact is controlled through a manual lifting tray;
the negative ion ionization source is used for ionizing the decomposed composition of the insulating gas;
the mass spectrometer is used for detecting the mass-to-charge ratio of each component in the plasma generated by the ionization of the composition.
2. The mass spectrometry detection system of claim 1, wherein the discharge chamber further comprises observation windows disposed on both sides of the chamber body.
3. The mass spectrometry detection system of claim 1, wherein the upper insulating sleeve and the lower insulating sleeve are made of a thermosetting resin.
4. The mass spectrometry detection system of claim 3, wherein the thermosetting resin is an epoxy resin.
5. The mass spectrometry detection system of claim 1, wherein the negative ion ionization source is an electrospray vacuum ultraviolet ionization source.
6. A method for detecting the decomposition products of the dielectric gas discharge in the GIS by the mass spectrometric detection system of claim 1, comprising the steps of:
s100: vacuumizing the mass spectrum detection system, and injecting insulating gas for GIS equipment into the discharge cavity;
s200: applying external voltage to the discharge cavity to discharge and decompose the insulating gas;
s300: introducing the composition decomposed by the discharge of the insulating gas into a negative ion ionization source for ionization;
s400: and introducing plasma generated by ionizing the composition into a mass spectrometer for mass-to-charge ratio detection.
7. The method of claim 6, wherein the negative ion ionization source is an electrospray vacuum ultraviolet ionization source.
CN201811329801.7A 2018-11-08 2018-11-08 Mass spectrum detection system and method for insulating gas discharge decomposition products in GIS Active CN109507275B (en)

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EP2239574A1 (en) * 2004-03-12 2010-10-13 University Of Virginia Patent Foundation Electron transfer dissociation for biopolymer sequence analysis
CN102221576A (en) * 2010-04-15 2011-10-19 岛津分析技术研发(上海)有限公司 Method and device for generating and analyzing ions
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CN104090054A (en) * 2014-06-18 2014-10-08 广西电网公司电力科学研究院 On-line detection method for SF6 gas in electrical equipment
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EP2239574A1 (en) * 2004-03-12 2010-10-13 University Of Virginia Patent Foundation Electron transfer dissociation for biopolymer sequence analysis
WO2008007105A1 (en) * 2006-07-13 2008-01-17 Micromass Uk Limited Apparatus comprising an ion mobilility spectrometer
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