CN208383820U - A kind of SF6/CF4Mixed gas decomposition product detection device - Google Patents
A kind of SF6/CF4Mixed gas decomposition product detection device Download PDFInfo
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- CN208383820U CN208383820U CN201820837581.8U CN201820837581U CN208383820U CN 208383820 U CN208383820 U CN 208383820U CN 201820837581 U CN201820837581 U CN 201820837581U CN 208383820 U CN208383820 U CN 208383820U
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- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 52
- 238000001514 detection method Methods 0.000 title claims abstract description 49
- 239000007789 gas Substances 0.000 claims abstract description 107
- 239000012159 carrier gas Substances 0.000 claims abstract description 79
- 238000012546 transfer Methods 0.000 claims abstract description 34
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- 238000004458 analytical method Methods 0.000 claims abstract description 24
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 20
- 238000004587 chromatography analysis Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 14
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical compound FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 7
- 230000000694 effects Effects 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 230000005526 G1 to G0 transition Effects 0.000 claims description 3
- 230000004907 flux Effects 0.000 claims description 3
- 238000007689 inspection Methods 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 2
- 238000002438 flame photometric detection Methods 0.000 claims 3
- 238000009413 insulation Methods 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 2
- 239000000523 sample Substances 0.000 description 56
- 229910018503 SF6 Inorganic materials 0.000 description 44
- WRQGPGZATPOHHX-UHFFFAOYSA-N ethyl 2-oxohexanoate Chemical compound CCCCC(=O)C(=O)OCC WRQGPGZATPOHHX-UHFFFAOYSA-N 0.000 description 26
- 229910002092 carbon dioxide Inorganic materials 0.000 description 21
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 19
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 18
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 17
- 239000001569 carbon dioxide Substances 0.000 description 17
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 10
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 9
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 8
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 8
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- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 2
- 229960000909 sulfur hexafluoride Drugs 0.000 description 2
- BVPWJMCABCPUQY-UHFFFAOYSA-N 4-amino-5-chloro-2-methoxy-N-[1-(phenylmethyl)-4-piperidinyl]benzamide Chemical compound COC1=CC(N)=C(Cl)C=C1C(=O)NC1CCN(CC=2C=CC=CC=2)CC1 BVPWJMCABCPUQY-UHFFFAOYSA-N 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
A kind of SF6/CF4Mixed gas decomposition product detection device, belongs to high voltage and insulation technology field.The device are as follows: sample introduction equipment is connected with analysis circuit, the analysis circuit detection device connection in parallel by automatic transfer valve and two；Analysis circuit is provided with three carrier gas roads and a sample road；It is provided with pressure stabilizing flow valve, flowmeter, six-way valve and chromatograph in first carrier gas road and Article 3 carrier gas road, each equipment is sequentially connected；Article 2 carrier gas road includes pressure stabilizing flow valve and flowmeter, is connect with automatic transfer valve；Sample road is divided into the first valve and the second valve, and the branch of the first valve connects the first six-way valve, the second six-way valve of piping connection of the second valve；The device can effectively detect SF6/CF4Feature decomposition product of the mixed gas under arcing ensures that the safe operation of switchgear provides effective technological means to be the operating status of accurate judgement inside electric appliance.
Description
Technical field
The utility model belongs to high voltage and insulation technology field, and in particular to a kind of SF6/CF4Mixed gas, which is decomposed, to be produced
Analyte detection device.
Background technique
Sulfur hexafluoride (SF6) it is that one kind is colourless, tasteless, nontoxic, non-ignitable, chemical property is extremely stable at normal temperatures and pressures
Synthetic gas, SF6Molecule be single sulphur polyfluoro symmetrical structure, there is extremely strong electronegativity, thus with excellent insulation and
Arc extinction performance, and be widely used exhausted in Cubicle Gas-Insulated Switchgear (GIS), gas circuit breaker (GCB), gas
In edge transformer, gas transmission of electricity pipeline (GIL).
However, SF6There is also some shortcomingss in practical applications: SF6Gas is larger in pressure, and environment temperature is too low
In the case where be easy liquefaction；SF6A large amount of use of gas can have an impact the greenhouse effects in the whole world, in Kyoto Protocol
In, SF6One of restricted six kinds of greenhouse gases are listed in, global warming coefficient (GWP) is CO223900 times of gas.For
Reduction SF6Influence to greenhouse effects, for a long time, domestic and foreign scholars are to find SF6Substitution gas largely grind
Study carefully, but not yet finds that one kind can substitute SF completely in terms of insulation performance and arc extinction performance6Gas, solve SF in short term6Greenhouse
The method of effect is the dosage for reducing it in the power system, such as uses SF6/N2、SF6/CF4Mixed gas etc..Subtract from source
Few SF6The greenhouse effects of discharge.
From the point of view of current every research and application, SF6/CF4Mixed gas insulation and blow-out performance are preferable, have very
Good application potential.Although SF6/CF4Mixed gas in physicochemical characteristics with high-purity SF6It is similar, but make in switching arc
With the decomposition product and pure SF of lower mixed gas6There are very big differences, if still using pure SF6The detection method of gas, Wu Fazhun
The operating status of true reactive switches equipment.
SF6/CF4Mixed gas can generate decomposition, decomposition product and moisture micro in equipment, electrode under arcing
And solid insulating material reacts, and generates more complicated mixture, and such as: carbon monoxide (CO), carbon dioxide
(CO2), methane (CH4), hydrogen (H2), carbon tetrafluoride (CF4), fluorination sulfonyl (SO2F2), fluorination thionyl (SOF2), octafluoro third
Alkane (C3F8), hydrogen sulfide (H2S), sulfur dioxide (SO2) etc., shown in main decomposition approach See Figure:
Utility model content
The purpose of this utility model is to provide a kind of SF6/CF4Mixed gas decomposition product detection device.The device can be with
Effective detection SF6/CF4Feature decomposition product of the mixed gas under arcing be such as: CO, CO2、CH4、CF4、CO2、SOF2、
SO2F2、C3F8、H2S、SO2Deng to ensure the safety fortune of switchgear for the operating status of accurate judgement inside electric appliance
Row provides effective technological means.
The technical solution of the utility model is:
A kind of SF6/CF4Mixed gas decomposition product detection device, comprising: sample introduction equipment, analysis circuit and detection device；
Wherein, sample introduction equipment is connected with analysis circuit, and analysis circuit is connected by automatic transfer valve with detection device；
The analysis circuit is provided with three carrier gas roads and a sample road；
Wherein, first carrier gas road includes the first pressure stabilizing flow valve, first flowmeter, the first six-way valve and the first chromatography
Instrument, each equipment are sequentially connected；Wherein, the first six-way valve is connected with the first quantity tube, and the first chromatograph is equipped with the first chromatography
Column；First pressure stabilizing flow valve is connected by carrier gas drying tube with carrier gas supply line, and the first chromatographic column is connected with automatic transfer valve；
Article 2 carrier gas road includes the second pressure stabilizing flow valve and second flowmeter；Second pressure stabilizing flow valve is dry by carrier gas
Pipe is connected with carrier gas supply line, and second flowmeter is connected with automatic transfer valve；
Article 3 carrier gas road includes third pressure stabilizing flow valve, third flowmeter, the second six-way valve, the second chromatograph and third
Six-way valve, each equipment are sequentially connected；Wherein, the second six-way valve is connected with the second quantity tube, and the second chromatograph is equipped with second
Chromatographic column, third six-way valve are connected with isolating valve and third chromatograph；Third chromatograph is equipped with third chromatographic column, third pressure stabilizing
Flow valve is connected by carrier gas drying tube with carrier gas supply line, and third six-way valve is connected with automatic transfer valve；
One sample road include the first valve and the second valve, sample air pipe after sample gas drying tube,
It is separately connected the first valve and the second valve, is divided into two branches, the first six-way valve is connected by the branch of the first valve, passes through
The branch of second valve connects the second six-way valve；
Second six-way valve and third six-way valve is arranged at Article 3 carrier gas road, and is used in series, wherein
Second six-way valve is used to sample introduction, and the switching for the isolating valve that third six-way valve is used to be isolated, and is arranged by third six-way valve is made
Passed through or with can choose sample not by third chromatographic column, hence into detection device.
The detection device includes thermal conductivity detector (TCD) (TCD) and flame photometric detector (FPD), wherein Thermal Conductivity
Two detectors of device (TCD) and flame photometric detector (FPD) compose in parallel；Detection device and analysis circuit by cutting automatically
Valve connection is changed, automatic transfer valve allows hand over different detectors, to detect SF6/CF4Mixed gas decomposition product.
The flame photometric detector (FPD) is using hydrogen D generator and air C generator as gas source.
According to the difference of the gas of chromatography post detection, corresponding detector is selected, specifically:
The polytetrafluoroethylene (PTFE) packed column that first chromatographic column is mainly TDX-01 with stationary phase, bridge stream 90-150mA, column temperature 80
~120 DEG C, pressure is 0.1psi before column；Using the first chromatographic column mainly for separating of SF6/CF4In mixed gas decomposition product
CO、CO2、CH4, measured using TCD；Using the first chromatography post separation SF6/CF4SOF in mixed gas decomposition product2、
SO2F2, measured using FPD；
Second chromatographic column mainly uses PorapakQ packed column, and being suitble to granularity mesh is 40-60, and column length is 10~40m, column internal diameter
3mm, pressure is 15psi-25psi before column；Using the second chromatographic column mainly for separating of SF6/CF4In mixed gas decomposition product
Air, CO2、CF4、C3F8、SF6, measured using TCD；
Third chromatographic column mainly uses GasPro series capillary column, column length 30-50m, column internal diameter 0.3mm, and pressure is before column
10psi-20psi；Using third chromatographic column mainly for separating of SF6/CF4SO in mixed gas decomposition product2、H2S is used
FPD measurement；
It is carrier gas, carrier gas stream 10mL/min-15mL/min that the carrier gas selection purity, which is 99.99wt.% helium,.
The sample introduction equipment avoids sample gas dirty using hand gun sample introduction or sample introduction bag sample introduction during sample introduction
Dye.
In the detection device of the utility model, the hydrogen source gas purity of flame photometric detector reach 99.9999wt.% with
On, hydrogen D flow velocity is 35~45mL/min, and air C flow velocity is 130~150mL/min.
The analysis circuit of the utility model has the function of volume and flow control.
The carrier gas stream that each chromatographic column passes through is controlled by pressure stabilizing flow valve and flowmeter, carrier gas flux 2.577mL/
Min, aux. pressure 4.35psi, pressure is 15psi-25psi before chromatographic column column, chromatographic column gas outlet pressure is 10psi-
20psi, chromatographic column should be led to carrier gas Passivation Treatment 4h at 120 DEG C before use, be done once after Passivation Treatment using temperature programming
Blank assay guarantees the accuracy of experiment.
The TCD detector temperature is 60 DEG C, and bridge electric current is 80mA, flow rate of carrier gas 10mL/min-15mL/min.
The FPD detector temperature is 150 DEG C, flow rate of carrier gas 10mL/min-15mL/min.
The SF of the utility model6/CF4The detection process of mixed gas decomposition product are as follows: by controlling the first valve and second
Valve, control sample to be tested pass through the first chromatographic column or the second chromatographic column；
It is controlled by automatic transfer valve and TCD detector, Analysis for CO, CO is entered by the sample to be tested of the first chromatographic column2、
CH4；SOF is detected by FPD detector2、SO2F2, switch the second valve, so that sample to be tested passes through the second chromatographic column and third
Chromatographic column detects CF by automatically switching Vavle switching TCD detector4、CO2、C3F8、SF6Gas, FPD detector detect H2S、
SO2。
A kind of SF of the utility model6/CF4The detection device of mixed gas decomposition product, the beneficial effect is that:
1. the measure loop of the utility model, by the SF of sample introduction6/CF4Mixed gas, be equipped with gas chromatograph and TCD and
FDP is in detector, by automatically switching decomposition product CO, the CO of Vavle switching realization to mixed gas under arcing2、CH4、
CF4、CO2、SOF2、SO2F2、C3F8、H2S、SO2Etc. being detected.Since mixed gas decomposition product is more complicated, if all
Into detector not only can contaminated equipment, damage chromatographic column, can also since detector is to the difference of different component detection sensitivity,
So that testing result is inaccurate.The utility model use three root chromatogram columns, using the first chromatographic column in mixed gas CO,
CO2、CH4It is detected using TCD detector, to SOF2、SO2F2It is detected using FPD detector；Pass through cutting for automatic transfer valve
It changes, by CF4、CO2、C3F8、、SF6By the second chromatography post separation, detected by TCD detector, H2S、 SO2By third chromatographic column point
From being detected by FPD detector, accurately and effectively measured to realize decomposition product, judge that mixed gas electrical equipment is former
Barrier provides more accurate judgment method.
2. this method is by selecting different chromatographic columns to utilize gas chromatograph (GC) to mixed gas under arcing
Decomposition product analyzed, acted on by the switching of six-way valve and automatic switching valve, utilize thermal conductivity detector (TCD) (TCD) and flame
Photometric detector (FPD) detection unit detects the gas component in decomposition product.By selecting chromatographic column appropriate, take
Build SF6/CF4The measure loop of decomposition product under mixed gas arcing, to decomposition product of the mixed gas under arcing
It is tested and analyzed.
Detailed description of the invention
Fig. 1 is the utility model embodiment SF6/CF4Mixed gas decomposition product detection device connection schematic diagram；
Fig. 2 is that the second chromatography post separation sample gas enters TCD detector connection schematic diagram；
Fig. 3 is that the first chromatographic column and the second chromatography post separation sample gas enter TCD and FPD detector connection schematic diagram；
Fig. 4 is that third chromatography post separation sample gas enters FPD detector connection schematic diagram；
Fig. 5 is the first chromatography post detection CO, CO2Standard chromatogram；
Fig. 6 is detection SF6The standard chromatogram of decomposition product.
Wherein, in figure, 1 is carrier gas drying tube, and 2 be the first pressure stabilizing flow valve, and 3 be first flowmeter, and 4 is logical for the one or six
Valve, 5 be the first quantity tube, and 6 be the first chromatographic column, and 7 be the second pressure stabilizing flow valve, and 8 be second flowmeter, and 9 be third pressure stabilizing stream
Valve is measured, 10 be third flowmeter, and 11 be the second six-way valve, and 12 be the second quantity tube, and 13 be the second chromatographic column, and 14 is logical for the three or six
Valve, 15 be third chromatographic column, and 16 be isolating valve, and 17 be automatic transfer valve, and 18 be TCD detector, and 19 be FPD detector, and 20 are
Sample gas drying tube, 21 be the first valve, and 22 be the second valve.
A is carrier gas, and B is sample gas, and C is air, and D is hydrogen.
Specific embodiment
It elaborates with reference to the accompanying drawing to specific embodiment of the present utility model.
In following embodiment, G4600-64006 gas chromatograph that the gas chromatograph used produces for agilent company.
In following embodiment, hydrogen source gas system is the hydrogen source gas system of Parker (Parker) company production.
In following embodiment, used chromatographic column is intended to be passivated processing before testing, and column bleed is detected in color
After composing aging of column process, make primary blank test (not sample introduction) using temperature programming.Usually with 10 DEG C/min from 50 DEG C
Maximum operation (service) temperature is risen to, keeps 10min after reaching maximum operation (service) temperature.Obtain a loss figure.These numerical value may be to the present
The solution for comparing test and experiment problem afterwards is helpful.In the chromatogram of blank test, there should not be chromatographic peak appearance.Such as
There is chromatographic peak in fruit, usually may be from injection port bring pollutant.If under normal use state, chromatographic column
Performance is begun to decline, and the signal value of baseline can increase.In addition, if at quite low temperatures, baseline signal value is significantly greater than
Initial value, then it is possible that being that chromatographic column and GC system have pollution.Old chromatographic column during installation cuts the both ends of chromatographic column
A part is gone, guarantees that the clast of no sample introduction pad remains in column.
Embodiment
A kind of SF6/CF4Mixed gas decomposition product detection device, comprising: sample introduction equipment, analysis circuit and detection device；
Wherein, sample introduction equipment is connected with analysis circuit, and analysis circuit is connected by automatic transfer valve 17 with detection device；Its
Attachment structure schematic diagram is shown in Fig. 1.
The analysis circuit is provided with three carrier gas roads and a sample road；
Wherein, first carrier gas road includes the first pressure stabilizing flow valve 2, first flowmeter 3, the first six-way valve 4 and the first color
Spectrometer, each equipment are sequentially connected；Wherein, the first six-way valve 4 is connected with the first quantity tube 5, and the first chromatograph is equipped with first
Chromatographic column 6；First pressure stabilizing flow valve 2 connect with carrier gas supply line by carrier gas drying tube 1, the first chromatographic column 6 with cut automatically
Change the connection of valve 17；
Article 2 carrier gas road includes the second pressure stabilizing flow valve 7 and second flowmeter 8；Second pressure stabilizing flow valve 7 passes through carrier gas
Drying tube 1 is connected with carrier gas supply line, and second flowmeter 8 and automatic transfer valve 17 connect；
Article 3 carrier gas road includes third pressure stabilizing flow valve 9, third flowmeter 10, the second six-way valve 11, the second chromatograph
With third six-way valve 14, each equipment is sequentially connected；Wherein, the second six-way valve 11 is connected with the second quantity tube 12, the second chromatography
Instrument is equipped with the second chromatographic column 13, and third six-way valve 14 is connected with isolating valve 16 and third chromatograph；Third chromatograph is equipped with
Third chromatographic column 15, third pressure stabilizing flow valve 9 are connected by carrier gas drying tube 1 with carrier gas supply line, 14 He of third six-way valve
Automatic transfer valve 17 connects；
One sample road includes the first valve 21 and the second valve 22, and sample air pipe passes through sample gas drying tube
After 20, it is separately connected the first valve 21 and the second valve 22, is divided into two branches, connects first by the branch of the first valve 21
Six-way valve 4 connects the second six-way valve 11 by the branch of the second valve 22；
Second six-way valve 11 and third six-way valve 14 are arranged at Article 3 carrier gas road, and are used in series,
Wherein, the second six-way valve 11 is used to sample introduction, and third six-way valve 14 is used to the isolation be isolated, and be arranged by third six-way valve 14
The switching effect of valve 16 can choose sample and pass through or not pass through third chromatographic column 15, hence into detection device.
The detection device includes thermal conductivity detector (TCD) (TCD detector 18) and flame photometric detector (FPD detector
19), wherein two detector parallel connection groups of thermal conductivity detector (TCD) (TCD detector 18) and flame photometric detector (FPD detector 19)
At；Detection device is connected with analysis circuit by automatic transfer valve, and automatic transfer valve 17 allows hand over different detectors, thus
Detect SF6/CF4Mixed gas decomposition product.
According to the difference of the gas of chromatography post detection, corresponding detector is selected, specifically:
The polytetrafluoroethylene (PTFE) packed column that first chromatographic column 6 is mainly TDX-01 with stationary phase, bridge stream 90-150mA, column temperature
110 DEG C, pressure is 0.1psi before column；Using the first chromatographic column mainly for separating of SF6/CF4CO in mixed gas decomposition product,
CO2、 CH4, measured using TCD；Using the first chromatography post separation SF6/CF4SOF in mixed gas decomposition product2、SO2F2, adopt
It is measured with FPD；
Second chromatographic column 13 mainly uses PorapakQ packed column, and granularity mesh is suitble to be 40-60, and column length is 10~40m, in column
Diameter 3mm, pressure is 15psi-25psi before column；Using the second chromatographic column mainly for separating of SF6/CF4In mixed gas decomposition product
Air, CO2、CF4、C3F8、SOF2, measured using TCD；
Third chromatographic column 15 mainly uses GasPro series capillary column, and column length 30-50m, column internal diameter 0.3mm, pressure is before column
10psi-20psi；Using third chromatographic column mainly for separating of SF6/CF4SO in mixed gas decomposition product2、H2S、SO2F2,
It is measured using FPD；
The carrier gas A selection purity is that 99.99wt.% helium is carrier gas, and carrier gas A air-flow is 10mL/min-15mL/
min。
The sample introduction equipment avoids sample gas dirty using hand gun sample introduction or sample introduction bag sample introduction during sample introduction
Dye.
In the detection device of the utility model, the hydrogen D gas source purity of flame photometric detector reaches 99.9999wt.%
More than, hydrogen D flow velocity is 35~45mL/min, and air C flow velocity is 130~150mL/min.
The analysis circuit of the utility model has the function of volume and flow control.
The carrier gas stream that each chromatographic column passes through is controlled by pressure stabilizing flow valve and flowmeter, carrier gas flux 2.577mL/
Min, aux. pressure 4.35psi, pressure is respectively 15psi-25psi, 10psi-20psi before chromatographic column column, and chromatographic column is using
Before should lead to carrier gas Passivation Treatment 4h at 120 DEG C, do primary blank experiment using temperature programming after Passivation Treatment, guarantee experiment
Accuracy.
The TCD detector temperature is 60 DEG C, and bridge electric current is 80mA, flow rate of carrier gas 10mL/min-15mL/min；
The FPD detector temperature is 150 DEG C, flow rate of carrier gas 10mL/min-15mL/min；
The SF of the utility model6/CF4The detection process of mixed gas decomposition product are as follows: by controlling the first valve and second
Valve, control sample to be tested pass through the first chromatographic column or the second chromatographic column；
It is controlled by automatic transfer valve and TCD detector, Analysis for CO, CO is entered by the sample to be tested of the first chromatographic column2、
CH4；SOF is detected by FPD detector2、SO2F2, switch the second valve, so that sample to be tested passes through the second chromatographic column and third
Chromatographic column detects CF by automatically switching Vavle switching TCD detector4、CO2、C3F8、SF6Gas, FPD detector detect H2S、
SO2。
A kind of SF6/CF4The detection method of mixed gas decomposition product, using above-mentioned apparatus, comprising the following steps:
(1) carrier gas and sampling: it is carrier gas, carrier gas stream 10mL/min-15mL/ that selection purity, which is 99.99% helium,
Min excludes influence of micro- micro- oxygen of water to experiment in gas by carrier gas drying tube 1, passes through three pressure maintaining valves and three flowmeters
Control carrier gas stream.Using hand gun sample introduction or sampler bag sample introduction, to reduce the reaction and pollution during sample introduction.
(2) analysis detection, the specific steps of chromatography are carried out to sample using gas chromatograph are as follows:
1) quantity tube, sampling are rinsed:
When initial position, 1 in automatic transfer valve and 2,3 and 4,5 and 6 are connected, and carrier gas A is passed through by automatic transfer valve
TCD detector 18 is repeatedly rinsed, by Article 2 carrier gas road, by 3 and 4 in automatic transfer valve, repeatedly in first carrier gas road
FPD detector 19 is rinsed, to drain remaining gas in pipeline.
Valve 1 and valve 2 are in opening state, and sample gas B enters the first quantity tube 5 by the first valve 21, meanwhile,
Sample gas B enters the second quantity tube 12 by the second valve 22, repeatedly rinses quantity tube, drains remaining gas in pipeline, to
Sample is entered by injection port to be prepared to analyze in quantity tube, and the connection of instrument at this time is as shown in Figure 1, the first six-way valve 4, second
11 route of six-way valve is closed, and sample rests in quantity tube, is not through chromatography column feed materials mouth and is entered instrument and is analyzed；
2) as shown in Fig. 2, the second six-way valve 11 is opened, the second quantity tube 12 sample introduction: is connected to Article 3 carrier gas road
In, third six-way valve 14 is closed, and isolating valve 16 is connected in Article 3 carrier gas road, will be in the second quantity tube 12 by carrier gas A
Gas is blown into the second chromatographic column 13, and the communication port 5 and 2,3 and 4 in automatic transfer valve 17,1 and 6 are respectively turned on, and second is quantitative
Sample to be tested in pipe 12 measures air, the CF in sample gas by TCD detector4、CO2And SF6Gas；
3) it tests and analyzes: as shown in figure 3, to SF in the second chromatographic column 126Appearance finishes, and the first six-way valve 4 is in and is opened
State is opened, the first quantity tube 5 is connected into first carrier gas road, and the sample to be tested in the first quantity tube 5 is blown into the first color by carrier gas A
It composes in column 6, the second valve 22 is in close state, and automatic transfer valve 17 acts, at this point, the communication port 1 in automatic transfer valve 17
With 2,3 and 4,5 are separately connected with 6, CO, CO that the first chromatographic column 6 is isolated2、CH4Into being detected in TCD detector；Its
In, the first chromatographic column 6 detects CO, CO2Standard chromatogram see Fig. 5；
To CO, CO in the first chromatographic column 62After gas appearance is complete, switch automatic transfer valve 17, at this point, automatic transfer valve
Communication port 1 and 4,3 and 2 in 17,5 are separately connected with 6, the SOF that the first chromatographic column 6 is isolated2、SO2F2It is sent to FPD inspection
It surveys in device 19, waits SO2F2After appearance, the first valve 21 is closed；
Second valve 22 is opened, and the second six-way valve 11 work, the second quantity tube 12 is connected in Article 3 carrier gas road, third
Six-way valve 14 is closed, and isolating valve 16 is connected in Article 3 carrier gas road, at this point, carrier gas A is by the sample gas B in the second quantity tube 12
It is blown into the second chromatographic column 13 and is analyzed, the CF that the second chromatographic column 13 is isolated4、CO2、C3F8Gas by isolating valve by
Automatic transfer valve 17 (communication port 2 and 5,1 and 6 of automatic transfer valve 17 at this time, 3 and 4 are respectively turned on) is sent to TCD detector
In, at this point, to the CF in sample gas B4、CO2、C3F8Gas is detected.
As shown in figure 4, to the CF in the second chromatographic column 134、CO2、C3F8After gas appearance is complete, third six-way valve 14 is opened
It opens, third chromatographic column 15 is connected in Article 3 carrier gas road, at this time the communication port 5 and 4,1 and 2 of automatic transfer valve 17,3 and 6
It is respectively turned on, the H that third chromatographic column 15 is isolated2S、SO2It is switched into FPD detector and is detected by automatic transfer valve 17.
Detect SF6The standard chromatogram of decomposition product is shown in Fig. 6.
1) quantitative analysis: quantitative analysis is carried out using external standard method, peak face of each content of material with appearance in TCD detector 18
Product is linearly related, and the content of each substance passes through the peak area correlation of indices of appearance in FPD detector 19.
2) it resets: being finished to all peak appearances, the first six-way valve 4 and the second six-way valve 11 are reset to sample position, automatically
Switching valve 17 is measured to initial position.It repeats the above steps, is measured in parallel sample gas and records chromatography response at least twice,
Until the adjacent response relative deviation measured twice is not more than 10%.
The analysis method of the utility model can detect simultaneously it can be seen from the typical chromatography that the utility model measures
SF6/CF4Decomposition product CO, the CO of mixed gas under arcing2、CH4、CF4、CO2、SOF2、SO2F2、C3F8、H2S、 SO2
Etc. foreign gases, separative efficiency it is high, can be to judge that mixed gas breaker gas chamber failure provides judgment basis.
Claims (9)
1. a kind of SF6/CF4Mixed gas decomposition product detection device, which is characterized in that the SF6/CF4Mixed gas decomposition product
Detection device includes: sample introduction equipment, analysis circuit and detection device；
Wherein, sample introduction equipment is connected with analysis circuit, and analysis circuit is connected by automatic transfer valve with detection device；
The analysis circuit is provided with three carrier gas roads and a sample road；
Wherein, first carrier gas road includes the first pressure stabilizing flow valve, first flowmeter, the first six-way valve and the first chromatograph, respectively
A equipment is sequentially connected；Wherein, the first six-way valve is connected with the first quantity tube, and the first chromatograph is equipped with the first chromatographic column；The
One pressure stabilizing flow valve is connected by carrier gas drying tube with carrier gas supply line, and the first chromatographic column is connected with automatic transfer valve；
Article 2 carrier gas road includes the second pressure stabilizing flow valve and second flowmeter；Second pressure stabilizing flow valve by carrier gas drying tube and
The connection of carrier gas supply line, second flowmeter are connected with automatic transfer valve；
Article 3 carrier gas road includes that third pressure stabilizing flow valve, third flowmeter, the second six-way valve, the second chromatograph and the three or six are logical
Valve, each equipment are sequentially connected；Wherein, the second six-way valve is connected with the second quantity tube, and the second chromatograph is equipped with the second chromatography
Column, third six-way valve are connected with isolating valve and third chromatograph；Third chromatograph is equipped with third chromatographic column, third pressure stabilizing flow
Valve is connected by carrier gas drying tube with carrier gas supply line, and third six-way valve is connected with automatic transfer valve；
One sample road includes the first valve and the second valve, and sample air pipe is after sample gas drying tube, respectively
The first valve and the second valve are connected, two branches are divided into, the first six-way valve is connected by the branch of the first valve, by second
The branch of valve connects the second six-way valve；
Second six-way valve and third six-way valve is arranged at Article 3 carrier gas road, and is used in series, wherein second
Six-way valve is used to sample introduction, and the switching effect for the isolating valve that third six-way valve is used to be isolated, and be arranged by third six-way valve can
To select sample to pass through or not by third chromatographic column, hence into detection device；
The detection device includes thermal conductivity detector (TCD) and flame photometric detector, wherein thermal conductivity detector (TCD) and flame luminosity inspection
Two detectors of device are surveyed to compose in parallel；Detection device is connected with analysis circuit by automatic transfer valve, and automatic transfer valve can be cut
Different detectors is changed, to detect SF6/CF4Mixed gas decomposition product.
2. SF as described in claim 16/CF4Mixed gas decomposition product detection device, which is characterized in that the flame light
Detector is spent using hydrogen generator and air generator as gas source.
3. SF as described in claim 16/CF4Mixed gas decomposition product detection device, which is characterized in that the sample introduction is set
It is standby, using hand gun sample introduction or sample introduction bag sample introduction.
4. SF as described in claim 16/CF4Mixed gas decomposition product detection device, which is characterized in that examined according to chromatographic column
The difference of the gas of survey selects corresponding detector, specifically:
The polytetrafluoroethylene (PTFE) packed column that first chromatographic column is mainly TDX-01 with stationary phase, bridge stream 90-150mA, column temperature 80~120
DEG C, pressure is 0.1psi before column；Using the first chromatographic column mainly for separating of SF6/CF4CO, CO in mixed gas decomposition product2、
CH4, measured using TCD；Using the first chromatography post separation SF6/CF4SOF in mixed gas decomposition product2、SO2F2, using FPD
Measurement；
Second chromatographic column mainly uses PorapakQ packed column, be suitble to granularity mesh be 40-60, column length be 10~40m, column internal diameter 3mm,
Pressure is 15psi-25psi before column；Using the second chromatographic column mainly for separating of SF6/CF4Air in mixed gas decomposition product,
CO2、CF4、C3F8、SF6, measured using TCD；
Third chromatographic column mainly uses GasPro series capillary column, column length 30-50m, column internal diameter 0.3mm, and pressure is 10psi- before column
20psi；Using third chromatographic column mainly for separating of SF6/CF4SO in mixed gas decomposition product2、H2S is surveyed using FPD
It is fixed.
5. SF as described in claim 16/CF4Mixed gas decomposition product detection device, which is characterized in that carrier gas is that purity is
99.99wt.% helium is carrier gas, carrier gas stream 10mL/min-15mL/min.
6. SF as described in claim 16/CF4Mixed gas decomposition product detection device, which is characterized in that flame photometric detection
The hydrogen source gas purity of device reaches 99.9999wt.% or more, and hydrogen flow rate is 35~45mL/min, and air velocity is 130~
150mL/min。
7. SF as described in claim 16/CF4Mixed gas decomposition product detection device, which is characterized in that each chromatographic column is logical
The carrier gas stream crossed is controlled by pressure stabilizing flow valve and flowmeter, carrier gas flux 2.577mL/min, and aux. pressure is
4.35psi, pressure is 15psi-25psi before chromatographic column column, and chromatographic column gas outlet pressure is 10psi-20psi.
8. SF as described in claim 16/CF4Mixed gas decomposition product detection device, which is characterized in that the thermal conductivity inspection
Device is surveyed, temperature is 60 DEG C, and bridge electric current is 80mA, flow rate of carrier gas 10mL/min-15mL/min.
9. SF as described in claim 16/CF4Mixed gas decomposition product detection device, which is characterized in that the flame light
Detector is spent, temperature is 150 DEG C, flow rate of carrier gas 10mL/min-15mL/min.
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| CN110108813A (en) * | 2019-05-23 | 2019-08-09 | 沈阳工业大学 | Detect the device and method of perfluor isobutyronitrile and carbon dioxide gas mixture decomposition product |
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2018
- 2018-05-31 CN CN201820837581.8U patent/CN208383820U/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110108813A (en) * | 2019-05-23 | 2019-08-09 | 沈阳工业大学 | Detect the device and method of perfluor isobutyronitrile and carbon dioxide gas mixture decomposition product |
| CN110108813B (en) * | 2019-05-23 | 2024-02-13 | 沈阳工业大学 | Device and method for detecting mixed gas decomposition product of perfluoroisobutyronitrile and carbon dioxide |
| CN110954655A (en) * | 2019-11-18 | 2020-04-03 | 核工业北京化工冶金研究院 | Dynamic increase and decrease measuring device and method for inspection device of integrated control room of in-situ leaching uranium mine |
| CN112362766A (en) * | 2020-10-13 | 2021-02-12 | 广西电网有限责任公司电力科学研究院 | System for detecting gas components in sulfur hexafluoride electrical equipment |
| CN112858553A (en) * | 2020-12-30 | 2021-05-28 | 四川红华实业有限公司 | Corrosive gas analysis chromatograph and analysis method |
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