CN109781868A - A kind of gas chromatography combined with mass spectrometry device for sulfur hexafluoride decomposer detection - Google Patents
A kind of gas chromatography combined with mass spectrometry device for sulfur hexafluoride decomposer detection Download PDFInfo
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- CN109781868A CN109781868A CN201711104972.5A CN201711104972A CN109781868A CN 109781868 A CN109781868 A CN 109781868A CN 201711104972 A CN201711104972 A CN 201711104972A CN 109781868 A CN109781868 A CN 109781868A
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Abstract
A kind of gas chromatography combined with mass spectrometry device for sulfur hexafluoride decomposer detection, is made of gas-chromatography module, four-way switching valve interface and mass spectrum module three parts.Gas-chromatography module includes non-heated valve injection system, column oven, gas chromatographic column；Four-way switching valve interface switches for gas-chromatography and mass spectrum air circuit connection；Mass spectrum module includes ionization source, ionized region, transmission range, repulsion area, accelerating region, Disengagement zone, echo area, detection zone etc..The sulfur hexafluoride background gas of high concentration is largely vented using the present apparatus, do not enter mass spectrum, to improve the mass spectrometry method detection sensitivity of trace sulfur hexafluoride decomposer, gas-chromatography and mass spectrographic two-dimension analysis information are utilized simultaneously, it enormously simplifies and is commercially used for the independent gas phase chromatographic device structure of detection sulfur hexafluoride decomposer detection, with the utility value in industry.
Description
Technical field
The present invention relates to mass spectrum and gas chromatographic technique, specifically a kind of gas phase color for sulfur hexafluoride decomposer detection
Compose mass spectrometry device.
Background technique
Sulfur hexafluoride is a kind of gas material, has good chemical stability, insulating properties and arc-extinguishing, is widely used in
In electrical equipment.Sulfur hexafluoride is best one of the substance of known gaseous material chemical stability, and inertia is considerably beyond nitrogen.
It is not reacted with water, oxygen, ammonia, potassium hydroxide, hydrochloric acid, sulfuric acid etc..Under normal circumstances, sulfur hexafluoride at 150 DEG C or less no
It decomposes.But in electric arc and spark discharge when temperature is more than 200 DEG C of high temperature, sulfur hexafluoride just starts to decompose, and generates one
A little active harmful substances, they influence electrical equipment performance in the electrical equipment of sulfur hexafluoride, and loss can shadow in space
Ring maintenance of electric device personnel health.Therefore, the case where detecting sulfur hexafluoride gas decomposition product in electrical equipment is very
It is necessary.But the influence of the sulfur hexafluoride background gas due to high concentration, the measurement of the sulfur hexafluoride decomposer of trace is deposited
In larger impact.There is commercialized gas chromatograph dedicated for the detection of sulfur hexafluoride decomposer at present, but often all adopts
High concentration sulfur hexafluoride is vented with the switching mode of more valve multicolumns while realizing the fully separating of sulfur hexafluoride decomposer, process is multiple
It is miscellaneous, it is time-consuming and laborious.
Gas chromatographic technique be make in mixture each component two it is alternate be allocated, it is another wherein a phase is stationary phase
It is mutually mobile phase, mobile phase carries mixture and flows through this stationary phase, has an effect with stationary phase, different under same motive force
The time that component is detained in stationary phase is different, successively flows out from stationary phase, also known as chromatography or chromatography.Component is solid
It is fixed mutually constantly to carry out Adsorption and desorption process between mobile phase and be separated from each other, it is detected subsequently into detector.
Mass spectrography is that sample ionization is become gas ion mixture, and by the analytical technology of mass-to-charge ratio separation；Mass spectrum
Instrument is to realize above-mentioned separate analytical technique, to measure the quality of substance and the instrument of content and its structure.Mass spectrometry is
A kind of quickly and efficiently analysis method can carry out isotope analysis conducive to mass spectrograph, compound analysis, gas composition analysis with
And the ultrapure trace analysis of metal or non-metal solid sample.Present Organic Mass Spectrometry can not only carry out point of small molecule
Analysis, and can directly analyze sugar, protein and other.
A kind of gas chromatography combined with mass spectrometry device for sulfur hexafluoride decomposer detection of the invention, will using the present apparatus
The sulfur hexafluoride background gas of high concentration is largely vented, and does not enter mass spectrum, to improve the matter of trace sulfur hexafluoride decomposer
Spectral method detection sensitivity, while gas-chromatography and mass spectrographic two-dimension analysis information are utilized, it enormously simplifies and is commercially used for examining
It surveys sulfur hexafluoride decomposer and detects independent gas phase chromatographic device structure, with the utility value in industry.
Summary of the invention
The object of the present invention is to provide a kind of gas chromatography-mass spectrography devices of sulfur hexafluoride decomposer detection.It utilizes
The sulfur hexafluoride background gas of high concentration is largely vented by the present apparatus, does not enter mass spectrum, to improve the lithium sulphur content of trace
The mass spectrometry method detection sensitivity of object is solved, while utilizing gas-chromatography and mass spectrographic two-dimension analysis information, enormously simplifies business
Change and detect independent gas phase chromatographic device structure for detecting sulfur hexafluoride decomposer, with the utility value in industry.
This device is made of gas-chromatography module, four-way switching valve interface and mass spectrum module three parts.Gas-chromatography mould
Block includes non-heated valve injection system, column oven, gas chromatographic column；Four-way switching valve interface is used for gas-chromatography and mass spectrum gas circuit
Connection switching；Mass spectrum module includes ionization source, ionized region, transmission range, repulsion area, accelerating region, Disengagement zone, echo area, detection zone
Deng.The gas-chromatography module is connect by four-way switching valve interface with mass spectrum module.
Sample gas outlet is connected with No. 3 positions of six-way injection valve in gas-chromatography module；Gas-chromatography quantitative loop entrance with
No. 4 positions of six-way injection valve are connected, outlet is connected with No. 1 position of six-way injection valve；When six-way injection valve is in sample position, sample
Product are followed by No. 3 positions of six-way injection valve, No. 4 positions, gas-chromatography quantitative loop, No. 1 position, No. 2 positions, later by total waste gas outlet
Outflow；
Gas-chromatography carrier gas divides tow channel gas through pressure maintaining valve in gas-chromatography module, wherein all the way gas followed by flowmeter,
No. 4 positions, No. 1 position that four-way valve is flowed into after No. 5 positions of six-way injection valve, No. 6 positions, chromatographic columns, into mass spectrum injection port；Another way
Gas is flowed out by total waste gas outlet later followed by needle valve is flowed into behind flowmeter, No. 2 positions of four-way valve, No. 3 positions；
Sample ions are ionized source and ionize in ionized region in mass spectrum module, and the ion of generation is successively through transmission range, repulsion
Area, accelerating region, Disengagement zone, echo area eventually arrive at detection zone and realize detection.
Detailed description of the invention
It is described in further detail with reference to the accompanying drawing.
Fig. 1 is a kind of gas chromatography combined with mass spectrometry schematic device for sulfur hexafluoride decomposer detection.
In Fig. 1,1 is sample gas；2 be gas-chromatography carrier gas；3 be total waste gas outlet；4 be pressure maintaining valve；5 be flowmeter 1；6
For flowmeter 2；7 be gas-chromatography quantitative loop；8 be six-way injection valve；9 be chromatographic column；10 be four-way valve；11 be needle valve；12
For ionization source；13 be mass spectrum injection port；14 be ionized region；15 be transmission range；16 be repulsion area；17 be detection zone；18 be separation
Area；19 be echo area；20 be accelerating region.
Specific embodiment
A kind of gas chromatography combined with mass spectrometry device for sulfur hexafluoride decomposer detection, by gas-chromatography module, four-way
Switching valve interface and mass spectrum module three parts are constituted.
The outlet of sample gas 1 is connected with No. 3 positions of six-way injection valve 8 in gas-chromatography module；7 entrance of gas-chromatography quantitative loop
It is connected with No. 4 positions of six-way injection valve 8, exports and be connected with No. 1 position of six-way injection valve 8；Six-way injection valve 8 is in sample position
When, sample is followed by No. 3 positions of six-way injection valve 8, No. 4 positions, 7, No. 1 positions of gas-chromatography quantitative loop, No. 2 positions, later by total
Waste gas outlet 3 flows out；
Gas-chromatography carrier gas 2 divides tow channel gas through pressure maintaining valve 5 in gas-chromatography module, wherein gas is all the way followed by flowmeter
6, No. 4 positions, No. 1 position that four-way valve 10 is flowed into after No. 5 positions, No. 6 positions of six-way injection valve 8, chromatographic column 9, into mass spectrum injection port
13；Another way gas is gone out by total exhaust gas later followed by needle valve 11 is flowed into behind flowmeter 5, No. 2 positions of four-way valve 10, No. 3 positions
Mouth 3 flows out；
Sample ions are ionized source 12 and ionize in ionized region 14 in mass spectrum module, and the ion of generation is successively through transmission range
15, repulsion area 16, accelerating region 20, Disengagement zone 18, echo area 19 eventually arrive at detection zone 17 and realize detection.
Firstly, determining the appearance time range of high concentration sulfur hexafluoride.When high-purity lithium containing sulfur hexafluoride decomposer
Sulphur sample gas completes sampling process after being full of gas-chromatography quantitative loop 7, switches six-way injection valve 8 later and is allowed in sample introduction position
It sets, enters mass spectrum after chromatographic column 9 is separated containing the high-purity sulfur hexafluoride sample gas of sulfur hexafluoride decomposer and detected, remembered
Record the appearance time range of lower high concentration sulfur hexafluoride.
Secondly, being completed after being full of gas-chromatography quantitative loop 7 containing the high-purity sulfur hexafluoride sample gas of sulfur hexafluoride decomposer
Sampling process switches six-way injection valve 8 later and is allowed to contain the high-purity sulfur hexafluoride sample of sulfur hexafluoride decomposer in sample introduction position
Product gas is separated through chromatographic column 9.At the beginning of sample flows out the time close to high-purity sulfur hexafluoride appearance of chromatographic column 9 after separation
Begin time point, four-way valve 10 is switched into No. 1 position of four-way valve 10 at this time, No. 2 positions communicate, No. 3 positions, No. 4 positions communicate, i.e., will be big
Emptying is after the high-purity sulfur hexafluoride in part flows through No. 3 positions of four-way valve 10, needle valve 11 to exclude high concentration sulfur hexafluoride to trace
The influence of sulfur hexafluoride decomposer detection；To flow out the time of chromatographic column 9 after separation little over high-purity sulfur hexafluoride when sample
Four-way valve 10 is switched to No. 1 position of four-way valve 10 at this time by the time point that appearance finishes, No. 4 positions communicate, No. 2 positions, No. 3 position phases
Logical, i.e., remaining is continued to bring mass spectrum module into through mass spectrum injection port 13 and be detected by isolated decomposition product.
Claims (8)
1. a kind of gas chromatography combined with mass spectrometry device for sulfur hexafluoride decomposer detection is switched by gas chromatograph, four-way
Valve interface and mass spectrograph three parts are constituted；
Gas chromatograph includes non-heated valve injection system, the gas chromatographic column being placed in column oven；
Four-way switching valve interface switches for gas-chromatography and mass spectrum air circuit connection；
The gas-chromatography module is connect by four-way switching valve interface with mass spectrum module.
2. the apparatus according to claim 1, it is characterised in that:
Mass spectrum module includes ionization source, ionized region, transmission range, repulsion area, accelerating region, Disengagement zone, echo area, detection zone；
Sample gas (1) outlet is connected with No. 3 positions of six-way injection valve (8) in gas-chromatography module；Gas-chromatography quantitative loop (7) enters
Mouthful it is connected with No. 4 positions of six-way injection valve (8), exports and be connected with No. 1 position of six-way injection valve (8)；Six-way injection valve (8) is in
When sample position, sample is followed by No. 3 positions of six-way injection valve (8), No. 4 positions, gas-chromatography quantitative loop (7), No. 1 position, No. 2
Position is flowed out by total waste gas outlet (3) later；
Gas-chromatography carrier gas (2) divides tow channel gas through pressure maintaining valve (4) in gas-chromatography module, wherein gas is all the way followed by flowmeter
1 (5), No. 5 positions of six-way injection valve (8), No. 6 positions, chromatographic column (9) flow into No. 4 positions, No. 1 position of four-way valve (10) afterwards, into matter
It composes injection port (13)；Another way gas is followed by flowing into needle valve behind flowmeter 2 (6), No. 2 positions of four-way valve (10), No. 3 positions
(11), it is flowed out later by total waste gas outlet (3)；
Sample ions are ionized source (12) ionization in ionized region (14) in mass spectrum module, and the ion of generation is successively through transmission range
(15), repulsion area (16), accelerating region (20), Disengagement zone (18), echo area (19) eventually arrive at detection zone (17) and realize detection.
3. a kind of gas chromatography combined with mass spectrometry device for sulfur hexafluoride decomposer detection according to claim 2, special
Sign is: after sampling containing sulfur hexafluoride decomposer or high-purity sulfur hexafluoride sample gas to gas-chromatography quantitative loop (7), switching
Six-way injection valve (8) to sample introduction position, sample is separated through chromatographic column (9), observes the appearance time model of high-purity sulfur hexafluoride
It encloses, determines the whole story time point of high-purity sulfur hexafluoride appearance, when sample flows out time of chromatographic column (9) close to high-purity after separation
The initial time point of sulfur hexafluoride appearance, switches to No. 1 position of four-way valve (10) for four-way valve (10) at this time, No. 2 positions communicate, and 3
Number position, No. 4 positions communicate, i.e., most of high-purity sulfur hexafluoride is flowed through into No. 3 positions of four-way valve (10), needle valve (11) be vented afterwards with
Exclude the influence that high concentration sulfur hexafluoride detects trace sulfur hexafluoride decomposer；To flow out chromatographic column after separation when sample
(9) four-way valve (10) little over the time point that high-purity sulfur hexafluoride appearance finishes, is switched to four-way valve (10) at this time by time
No. 1 position, No. 4 positions communicate, No. 2 positions, No. 3 positions communicate, i.e., remaining is continued by isolated decomposition product through mass spectrum injection port (13)
Mass spectrum module is brought into be detected.
4. a kind of gas chromatography combined with mass spectrometry device for sulfur hexafluoride decomposer detection according to claim 3, special
Sign is: the sulfur hexafluoride decomposer includes CF4、C2F6、C3F8、SO2、H2S、CS2、SOF2、SO2F2It is middle a kind of or two kinds with
On.
5. a kind of gas chromatography combined with mass spectrometry device for sulfur hexafluoride decomposer detection according to claim 1, special
Sign is: using wearing, the six-way injection valve of quantitative loop, positive pressure sampling, sample are full of the non-heated valve injection system at room temperature
Sample introduction is completed in switching valve to sample introduction position after quantitative loop.
6. according to claim 1 or 5 it is described it is a kind of for sulfur hexafluoride decomposer detection gas chromatography combined with mass spectrometry devices,
Be characterized in that: it is 50~1000 μ L that the non-heated valve injection system, which wears quantitative loop volume,；The column oven controllable temperature is
Room temperature~400 DEG C.
7. a kind of gas chromatography combined with mass spectrometry device for sulfur hexafluoride decomposer detection according to claim 1 or claim 2,
Be characterized in that: the gas chromatographic column is the capillary column analyzed suitable for sulfur hexafluoride decomposer, packed column or other are similar
Like pillar, column tube internal diameter is 10~400 μm, and column length is 10~50m, 0~100 μm of inner film thickness.
8. a kind of gas chromatography combined with mass spectrometry device for sulfur hexafluoride decomposer detection according to Claims 2 or 3,
Be characterized in that: the mass spectrograph can be flight time mass spectrum or ion trap mass spectrometry.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711104972.5A CN109781868A (en) | 2017-11-10 | 2017-11-10 | A kind of gas chromatography combined with mass spectrometry device for sulfur hexafluoride decomposer detection |
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| CN201711104972.5A CN109781868A (en) | 2017-11-10 | 2017-11-10 | A kind of gas chromatography combined with mass spectrometry device for sulfur hexafluoride decomposer detection |
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Cited By (1)
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| CN114062475A (en) * | 2021-10-25 | 2022-02-18 | 广西电网有限责任公司电力科学研究院 | Method for on-line monitoring of sulfur hexafluoride concentration and decomposition product concentration |
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| CN114062475A (en) * | 2021-10-25 | 2022-02-18 | 广西电网有限责任公司电力科学研究院 | Method for on-line monitoring of sulfur hexafluoride concentration and decomposition product concentration |
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