CN103336070A - Detection device and method for quantitatively detecting composition of sulfur-containing fault gas in sulfur hexafluoride electrical equipment - Google Patents
Detection device and method for quantitatively detecting composition of sulfur-containing fault gas in sulfur hexafluoride electrical equipment Download PDFInfo
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- 229910018503 SF6 Inorganic materials 0.000 title claims abstract description 120
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 229960000909 sulfur hexafluoride Drugs 0.000 title claims abstract description 111
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 94
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 239000011593 sulfur Substances 0.000 title claims abstract description 92
- 238000001514 detection method Methods 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000000203 mixture Substances 0.000 title claims abstract description 18
- 238000000926 separation method Methods 0.000 claims abstract description 30
- 239000007789 gas Substances 0.000 claims description 149
- 238000004020 luminiscence type Methods 0.000 claims description 35
- 238000004587 chromatography analysis Methods 0.000 claims description 22
- 239000001307 helium Substances 0.000 claims description 19
- 229910052734 helium Inorganic materials 0.000 claims description 19
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 17
- 238000004817 gas chromatography Methods 0.000 claims description 13
- 239000012159 carrier gas Substances 0.000 claims description 12
- 238000012360 testing method Methods 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 4
- 238000010926 purge Methods 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 239000001257 hydrogen Substances 0.000 claims description 3
- 238000005259 measurement Methods 0.000 claims description 3
- 150000002371 helium Chemical class 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 150000002431 hydrogen Chemical class 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 13
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical compound S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 239000012071 phase Substances 0.000 description 8
- 230000004044 response Effects 0.000 description 8
- QGJOPFRUJISHPQ-UHFFFAOYSA-N Carbon disulfide Chemical compound S=C=S QGJOPFRUJISHPQ-UHFFFAOYSA-N 0.000 description 7
- 238000000354 decomposition reaction Methods 0.000 description 7
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- 238000006243 chemical reaction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000003822 preparative gas chromatography Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000004458 analytical method Methods 0.000 description 5
- 238000013459 approach Methods 0.000 description 5
- 230000008901 benefit Effects 0.000 description 5
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 5
- 239000000243 solution Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 3
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000012491 analyte Substances 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
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- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- 238000001819 mass spectrum Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
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- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical compound FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 239000005864 Sulphur Substances 0.000 description 2
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- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
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- 238000009434 installation Methods 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
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- 238000004949 mass spectrometry Methods 0.000 description 1
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Abstract
The invention discloses a detection device for quantitatively detecting the composition of a fault gas in sulfur hexafluoride electrical equipment. The detection device comprises a separation chromatographic column, a thermal conductivity detector and a sulfur chemiluminescence detector, wherein the separation chromatographic column is connected with the thermal conductivity detector which is connected with the sulfur chemiluminescence detector through a six-way valve, the sample outlet end of the thermal conductivity detector is connected with a port 2 of the six-way valve, the sample inlet end of the sulfur chemiluminescence detector is connected with a port 3 of the six-way valve, the six-way valve is controlled to be switched on or off to conduct the connection of the thermal conductivity detector and the sulfur chemiluminescence detector in sample feeding, and when SF6 (Sulfur Hexafluoride) is separated, the thermal conductivity detector and the sulfur chemiluminescence detector are disconnected to discharge the SF6. The invention also discloses a method for quantitatively detecting the composition of the fault gas in the sulfur hexafluoride electrical equipment. According to the detection device and the method, before decomposers of the SF6 are detected, the SF6 is discharged, so that the influence of the SF6 on detection results is reduced, and the sensitivity of the detection of the decomposers of the SF6 is improved.
Description
Technical field
The present invention relates to a kind of pick-up unit of sulfur hexafluoride electrical equipment failure gas, relate in particular to the pick-up unit of sulfur-bearing failure gas component in a kind of quantitative detection sulfur hexafluoride electrical equipment.The invention still further relates to and adopt this device quantitatively to detect the method for sulfur-bearing failure gas component in the sulfur hexafluoride electrical equipment.
Background technology
Sulfur hexafluoride (SF6) is used as the insulating material of high-voltage switch gear, big variable quantity and pressure device, high-tension cable and gas in electrical industry.When these device fails, can discharge, and sulfur hexafluoride gas can issue solution estranged in the high-temperature electric arc effect, its analyte comprises sulfocompound and other compounds etc., sulfocompound comprises vikane (SO
2F
2), cos (COS), sulfuretted hydrogen (H
2S), carbon disulphide (CS
2), sulphuric dioxide (SO
2) etc., so quantitatively detect fault and the defective that these sulfur hexafluoride decomposition products can be used for diagnosing electrical equipment.
At present, the quantitative detecting method of sulfur hexafluoride decomposition product is also very immature, is mainly reflected in: the sulfur hexafluoride decomposition product is formed complicated, and each component often concentration is very low, and the sulfur hexafluoride background value is very high, gives sulfur hexafluoride decomposition product such as vikane (SO
2F
2), cos (COS), sulfuretted hydrogen (H
2S), carbon disulphide (CS
2), sulphuric dioxide (SO
2) separation and the qualitative, quantitative that wait bring great difficulty.
Current, the analytical approach that is applied to the sulfur hexafluoride electrical equipment failure gas mainly contains vapor-phase chromatography, GC-MS(gas chromatography-mass spectrography), infra-red sepectrometry, electrochemical methods, detector tube method etc.
1. detector tube method
The detector tube method mainly is at SO
2Detect SO with HF
2With HF all be the highly acid material, they can react with NaOH, simultaneously SO
2Can impel indicator to change color with iodine generation chemical reaction again, the length of variable color be directly proportional with corresponding material concentration, so its concentration value is read from figure or the marker tape of detector tube easily.Because HF adopts acid-base reaction, SO
2Adopt redox reaction, both reaction mechanism differences are not so these two kinds of materials need to separate.But this method is subjected to the influence of temperature, humidity and resting period easily, and other main decomposition gas is not had detection effect, can not react SF6 discharge decomposed gas component situation comprehensively.
2. gas sensor method
This method mainly is to utilize chemical gas sensitive device to detect gas composition.The chemistry gas sensor is to utilize the shape of tested gas or molecular structure to be had the function (converter function) that the function (receptacle function) that selectivity captures and the chemistry amount that will capture effectively be converted into electric signal to come work.When tested gas was adsorbed to the gas sensory surface, its resistance value can change, thereby obtains the content of this gas.It is fast that the gas sensing method has detection speed, and the efficient height realizes that automatic on-line detects outstanding advantages such as diagnosis thereby can be used with computing machine, detects shortcomings such as gas composition is single but also exist.At present, the gas that can detect with the gas sensor method both at home and abroad mainly is more common gas such as SO
2, HF and H
2S, and to important gas composition SO
2F
2, SOF
2, SF
4, SOF
4And CF
4Then helpless.In addition, it exists interference problem between component as H
2The S sensor can be to SO
2Problems such as effect and HF sensor weak point in serviceable life are arranged.
3. electrochemical process
Utilize electrochemical method, use electrode and electrolytic solution that gas is detected, but only can measure hydrolyzable fluoride and acidity in the cracked gas, can't judge type and the concentration of analyte.And there is zero point drift in instrument, and poor stability influences testing result.
4. infra-red sepectrometry
Infra-red sepectrometry is based on gas to the detection method of the absorption of infrared light.It is qualitative to be according to wave number and the waveform of material to infrared Absorption, and its quantitative foundation is that material is to the degree of infrared Absorption.Except monoatomic molecules and homonuclear molecule, as O
2, N
2, outside the Ne etc., nearly all chemical substance all has absorption in the infrared light district.This method is compared with vapor-phase chromatography and GC-MS(gas chromatography-mass spectrography), and analysis speed soon, does not destroy sample gas, can realize detecting under the normal temperature.But when the analysis of sulfur hexafluoride electrical equipment failure gas component, the infrared absorption peak of sulfur hexafluoride and its decomposition product are as SO
2, F
2, CF
4, SO
2Infrared absorption peak exist overlapping, there is the phase mutual interference, thus the quantivative approach complexity, and also detection limit is also in the ppm level, generally can only reach 5 μ L/L ~ 10 μ L/L, detection sensitivity does not satisfy the detection requirement of sulfur-bearing failure gas component in the sulfur hexafluoride electrical equipment.
5. GC-MS(gas chromatography-mass spectrography)
Mass spectrum is to one of the strongest method of pure material evaluation.GC-MS(gas chromatography-mass spectrography) is to utilize chromatographic process that the sample gas of component complexity is separated and quantitatively, by mass spectrum each component is carried out qualitative analysis again.This method combines advantage and mass spectrum the advantage qualitative on of gas chromatography on quantitatively.But because mass spectrometer system mainly is the analysis at pure material, and its signal value is extremely unstable, needs often to proofread and correct, and it is comparatively loaded down with trivial details to work.
6. vapor-phase chromatography
Vapor-phase chromatography can be analyzed the multicomponent mixture with separate complex, and can with multiple analytical instrument coupling, being a kind of strong analysis means, having bright prospects, also is the popular method of analyzing sulfur-bearing failure gas component in the sulfur hexafluoride electrical equipment at present.
Advantage with gc analysis sulfur hexafluoride electrical equipment failure gas component is that it is that a kind of elder generation separates the method that afterwards detects, and can effectively avoid the intersection of various components to disturb.In addition, gas chromatography can with multiple analytical instrument coupling, as mass spectrometry (GC-MS), gas chromatography and Fourier's infrared spectrum coupling (GC-FTIR), advantage that can comprehensive various analytical instrument is comparatively comprehensively analyzed.
Be applied to the vapor-phase chromatography that sulfur-bearing failure gas component detects in the sulfur hexafluoride electrical equipment, kind according to detecting device is classified, and mainly contains thermal conductance (TCD) method, helium ionization detector (PDD) method and thermal conductance-flame luminosity series connection (TCD-FPD) method etc.
1. thermal conductance (TCD) method: adopt thermal conductivity detector (TCD) (TCD) that the gas chromatography gas separated is detected.Thermal conductivity detector (TCD) almost has response to all substances, and versatility is good, and the range of linearity is wide.Its quantitative principle is based on different material and has different thermal conductivity coefficients, and quantivative approach is simple, mainly is applicable to the detection of the new gas of sulfur hexafluoride.But this detection method sensitivity is lower, particularly to H
2S, SO
2, SO
2F
2Etc. gas detection signals a little less than.And according to present experience, the detection of these several gases all plays an important role for fault or the latency failure judgment of sulfur hexafluoride electrical equipment.
2. thermal conductance-flame luminosity series connection (TCD-FPD): i.e. thermal conductivity detector (TCD) (TCD) and flame photometric detector (FPD) (FPD) are used in series connection.Flame photometric detector (FPD) (FPD) is a kind of phosphorus, sulphur compound to be had high selectivity and highly sensitive mass flow rate sensitive detector.The TCD-FPD method has been introduced FPD, when overcoming simple use TCD to H
2S, SO
2And SO
2F
2The shortcoming that sulfides sensitivity is not high, but for helium ionization detector and sulfur chemistry luminescence detector, its sensitivity is still not high.And the response of FPD is nonlinear response, and quantivative approach is comparatively complicated.
3. helium ionization detector (PDD) method: helium ionization detector (PDD) can be to the overwhelming majority's substance responds, and along with the increase of fixed current is positive to the response of fixed gas, versatility is good.Helium ionization detector has high sensitivity simultaneously, can test in the scope of low ppb level.When measuring the concentration of 5 orders of magnitude of minimum detectable quantity, the result still is linear, and the good range of linearity is arranged.But it is the SO of spirit at quantitative SF6
2F
2, COS and H
2During S, the peak shape of SF6 has a strong impact on the peak shape of these several materials, and its quantitative result allows the people suspect.
In sum, the sensitivity of vapor-phase chromatography thermal conductivity detector (TCD) is not high, and the flame photometric detector (FPD) response is non-linear, and sensitivity can not be satisfied the fault analyte and detect requirement; Helium ionization detector accurately quantitative SF6 is the SO of spirit
2F
2, COS and H
2S gas.
Summary of the invention
One of purpose of the present invention is to provide the pick-up unit of sulfur-bearing failure gas component in a kind of quantitative detection sulfur hexafluoride electrical equipment.This device has separating effect preferably to each the sulfur-bearing failure gas component under sulfur hexafluoride (SF6) background, and can before quantitatively detecting SF6 be discharged, and reduces the sulfur-bearing failure gas of SF6 component, i.e. COS, H
2S, SO
2F
2, CS
2, SO
2And the influence of the testing result of other sulfur component, the detection sensitivity of raising sulfur-bearing failure gas component.
Two of purpose of the present invention is to provide the method that adopts said apparatus quantitatively to detect sulfur-bearing failure gas component in the sulfur hexafluoride electrical equipment.This method can be accurately quantitative COS, the H in the sulfur-bearing failure gas
2S, SO
2F
2, CS
2, SO
2And other sulfur component.
First purpose of the present invention is achieved through the following technical solutions: the pick-up unit of sulfur-bearing failure gas component in a kind of quantitative detection sulfur hexafluoride electrical equipment, it comprises the separation chromatography post, thermal conductivity detector (TCD) and sulfur chemistry luminescence detector, described separation chromatography post links to each other with thermal conductivity detector (TCD), thermal conductivity detector (TCD) is connected with the sulfur chemistry luminescence detector by a six-way valve, the sample outlet end of described thermal conductivity detector (TCD) is connected with the port 2 of six-way valve, the test entrance point of described sulfur chemistry luminescence detector is connected with six-way valve port 3, the switch of control six-way valve makes its port 2 and port 3 connections when sample introduction, the conducting thermal conductivity detector (TCD) is connected with the sulfur chemistry luminescence detector, disconnecting thermal conductivity detector (TCD) when separating SF6 is connected with the sulfur chemistry luminescence detector, port 2, port 1, port 5 and port 6 are communicated with formation SF6 discharge-channel, discharging SF6 successively.
Refer in the sulfur hexafluoride electrical equipment failure gas sample introduction process during sample introduction of the present invention and sulfur-bearing failure gas component during to sulfur chemistry luminescence detector sample introduction.When referring to SF6 to be separated during described separation SF6, when namely discharging SF6.
The sulfur chemistry luminescence detector (SCD) that the present invention uses is not subjected to the interference of most sample substrate to mole linear responses (corresponding to sulphur atom) such as sulfide are, has higher sensitivity (＜0.5 pg S/sec) and surpasses 1 * 10
4Linear.It comprises ozone generator, low pressure reaction pond, double plasma controller, double plasma firing chamber and gas chromatography detector, products of combustion is drawn into a low pressure reaction pond, add excessive ozone herein, the light that subsequent reactions sends is detected by the quick photomultiplier of indigo plant by optical filter and amplifies, and shows then or exports to data handling system.The chemiluminescence reaction that its principle sulfur monoxide (SO) that burning produces based on sulfocompound and ozone react and takes place:
The present invention also comprises carrier gas source, is used for the carrier gas supply, and described carrier gas source is connected with the port 4 of six-way valve.
The present invention also comprises helium gas source, and this helium gas source is connected with the separation chromatography post by the six-way valve injector, and gas sample to be determined and helium enter the separation chromatography post through the six-way valve injector to carry out gas and separate.
Separation chromatography post of the present invention adopts the at present existing separation chromatography post that the sulfur hexafluoride electrical equipment failure gas separates that can be used for, and comprises capillary column.As one embodiment of the present of invention, it is bore 0.32 mm that described separation chromatography post adopts chromatographic column, and length is the gas-pro capillary column of 60 m, as J﹠amp; W113-4362.
Second purpose of the present invention is to be achieved through the following technical solutions: the method for sulfur-bearing failure gas component in a kind of quantitative detection sulfur hexafluoride electrical equipment may further comprise the steps:
(1)
The divided gas flow component:Sulfur hexafluoride electrical equipment failure gas to be measured is fed the separation chromatography post, is the phase that flows with helium, gas composition is carried out gas chromatography separate;
(2)
Discharge sulfur hexafluoride:Separated gas enters in the thermal conductivity detector (TCD) and detects, appearance time and appearance time zone with the sulfur hexafluoride standard items are for referencial use, when arriving or during near the appearance time of sulfur hexafluoride, open six-way valve, port 2 disconnects with port 3 and being connected, port 2, port 1, port 5 and port 6 are communicated with successively, discharge sulfur hexafluoride;
(3)
The quantitative measurement of sulfur-bearing failure gas component:When arriving or going out the peak during concluding time near sulfur hexafluoride, close six-way valve, port 2 and port 3 are communicated with, the conducting thermal conductivity detector (TCD) is connected with the sulfur chemistry luminescence detector, residual gas in the described thermal conductivity detector (TCD) feeds in the sulfur chemistry luminescence detector and quantitatively detects, and then obtains each sulfur-bearing failure gas components contents.
The sulfur hexafluoride electrical equipment failure gas that will be substrate with SF6 feeds in the separation chromatography post SF6, COS, H
2S, SO
2F
2, CS
2And SO
2Carry out the gas chromatography separation etc. gas composition.And in component, therefore the appearance time of SF6 can change the path of gas by the switch six-way valve the earliest, emits SF6 gas, residual gas is fed in the sulfur chemistry luminescence detector (SCD) and detects.Because before entering SCD, complete or most of removal with SF6 gas, make the background value of SF6 drop to relatively low level to the influence of the signal value of other gas compositions, guaranteed the accuracy of sulfur chemistry luminescence detector (SCD) to the quantitative testing result of each sulfur-bearing failure gas component.The impulse force that produces when closing six-way valve makes separation of C OS, H
2S, SO
2F
2, CS
2, SO
2And the retention time of sulfur-bearing failure gas component such as other sulfur component delays, and further guaranteed the background value of SF6 and separating of each sulfur-bearing failure gas component peak shape, improved the accuracy of the quantitative testing result of each sulfur-bearing failure gas component greatly.
The chromatographic condition of gas chromatographic column adopts present existing chromatographic condition for separating of the gas composition in the sulfur hexafluoride electrical equipment failure gas to get final product in the step of the present invention (1).Separating effect for the gas composition that improves the sulfur hexafluoride electrical equipment failure gas, as one embodiment of the present of invention, the chromatographic condition of described separation chromatography post is: injector temperature: 200 ℃, pressure: 25 psi, total flow: 41.498 ml/min, dottle pin purge flow rate: 3 ml/min, shunt mode: shunting 10:1, chromatographic column: J﹠W113-4362:260 ℃: 60 m * 320 μ m * 0 μ m, post oven temperature, degree: initial temperature is 60 ℃, keeps 6 min; Speed with 10 ℃/min rises to 150 ℃, keeps 2 min.
The running parameter of thermal conductivity detector (TCD) adopts the running parameter of the gas composition in the known detection sulfur hexafluoride electrical equipment failure gas to get final product in the step of the present invention (2).As one embodiment of the present of invention, the detected temperatures of described thermal conductivity detector (TCD) is 200 ℃.
The running parameter of step of the present invention (3) sulfur chemistry luminescence detector adopts the running parameter of the gas composition in the known detection sulfur hexafluoride electrical equipment failure gas to get final product.As one embodiment of the present of invention, the detected temperatures of described sulfur chemistry luminescence detector is 225 ℃, 800 ℃ of SCD gas ions burner temperature wherein, hydrogen 45 ml/min, air 63 ml/min.
The present invention also comprises the step of measuring sulfur hexafluoride and each sulfur-bearing failure gas component appearance time zone, concrete operations are: the standard items of getting sulfur hexafluoride and each sulfur-bearing failure gas component are made into mixed gas, carry out gas chromatographic detection then, thereby obtain the appearance time zone of sulfur hexafluoride and each sulfur-bearing failure gas component, as the reference of subsequent step.The chromatographic condition of gas chromatography is identical with described step (1) chromatographic condition in this step.
The present invention compared with prior art has following beneficial effect:
(1) detection accuracy height
Pick-up unit provided by the invention has separating effect preferably to each the sulfur-bearing failure gas component under sulfur hexafluoride (SF6) background.And thermal conductivity detector (TCD) is connected with the sulfur chemistry luminescence detector by six-way valve in the device, and gas passage between the two can be changed.Because the time that SF6 gas occurs is the earliest, can it be discharged by changing the gas passage, reduce it to COS, H
2S, SO
2F
2, CS
2, SO
2Reach the influence of the peak shape of other sulfur component, improved the accuracy of quantitative testing result widely.
(2) detection sensitivity height
The present invention further adopt the sulfur chemistry luminescence detector to detect, and the sensitivity of sulfur chemistry luminescence detector is the ppb rank, the minimum 0.01 μ L/L that reaches of detection limit behind thermal conductivity detector (TCD).And before entering the sulfur chemistry luminescence detector, SF6 gas has been removed or most of the removal, has not had the interference of SF6 gas, more can improve detection sensitivity greatly.
(3) linear response
It all is linear responses that the present invention adopts sulfur chemistry luminescence detector and thermal conductivity detector (TCD), and the range of linearity is wide.
Description of drawings
Fig. 1 is installation drawing of the present invention.
Fig. 2 is the opening synoptic diagram of the valve of six-way valve 2.
Fig. 3 is the closed condition synoptic diagram of the valve of six-way valve 2.
Fig. 4 is that the TCD of each gas composition in the sulfur hexafluoride electrical equipment failure gas detects spectrogram.
Fig. 5 is that the SCD of each sulfur-bearing failure gas component detects spectrogram (after removing sulfur hexafluoride).
Embodiment
The present invention will be described to enumerate a part of instantiation below, is necessary to be pointed out that at this following specific embodiment only for the invention will be further described, does not represent limiting the scope of the invention.Some nonessential modifications that other people make according to the present invention and adjustment still belong to protection scope of the present invention.
Embodiment one: pick-up unit
The pick-up unit of sulfur-bearing failure gas component is one embodiment of the present of invention in a kind of quantitative detection sulfur hexafluoride electrical equipment as shown in Figure 1, comprises six-way valve injector 13, separation chromatography post 18, six-way valve 16, thermal conductivity detector (TCD) 15 and sulfur chemistry luminescence detector 14.The port 1 of six-way valve injector 13 ' be injection port, port 2 ' waste gas outlet, port 5 ' be phase import of flowing.Port 4 ' be connected with the sample introduction end of separation chromatography post 18, port 5 ' then be connected with mobile phase transfer pipeline 19, the air intake opening of the phase transfer pipeline 19 that flows is used for being connected with helium gas source, and this pipeline is provided with electronic pressure controller 12.The sample outlet end of separation chromatography post 18 is connected with thermal conductivity detector (TCD) 15, and 15 of thermal conductivity detector (TCD)s pass through six-way valve 16 and sulfur chemistry luminescence detector 14.Wherein, the port 2 of six-way valve 16 is injection port, and port 3 is outlet, and port 4 is carrier gas inlet, and port 6 is gas discharge outlet.The sample outlet end of thermal conductivity detector (TCD) 15 is connected with port 2, and port 3 is connected with the sample introduction end of sulfur chemistry luminescence detector 14, and port 4 is connected with gas-carrier pipeline 17, and gas-carrier pipeline 10 inlet ends are established the interface that is connected for carrier gas source.
As shown in Figure 2, when port 1 and port 2, port 3 and port 4 and port 5 and port 6 are communicated with respectively, port 2 disconnects with port 3 and being connected, six-way valve 16 is in opening, port 2, port 1, port 5 and port 6 are communicated with successively, constitute the SF6 discharge-channel, and gas-carrier pipeline 17 is communicated with sulfur chemistry luminescence detector 14.As shown in Figure 3, port 2 is communicated with respectively with port 1 with port 5, port 6 with port 3, port 4, and six-way valve 16 is in closed condition, and thermal conductivity detector (TCD) 15 is connected with sulfur chemistry luminescence detector 14, port 4, port 5, port 1 and port 6 are communicated with successively, constitute the carrier gas discharge-channel.
In the present embodiment, it is bore 0.32 mm that the separation chromatography post adopts chromatographic column, and length is the gas-pro capillary column of 60 m, specifically adopts J﹠W113-4362:260 ℃: 60 m * 320 μ m * 0 μ m.
Present embodiment also can comprise carrier gas source, and carrier gas source is connected with the interface of gas-carrier pipeline 17.
Present embodiment also can comprise helium gas source, helium gas source and port 5 ' then be connected with mobile phase transfer pipeline 19.
Embodiment two: detection method
1. determine appearance time and the appearance time zone of sulfur hexafluoride and each sulfur-bearing failure gas component
The standard items of getting sulfur hexafluoride (SF6) and part sulfur-bearing failure gas component are mixed into mixed gas, and wherein part sulfur-bearing failure gas component comprises vikane (SO
2F
2), cos (COS), sulfuretted hydrogen (H
2S), carbon disulphide (CS
2) and sulphuric dioxide (SO
2), wherein SF6 is balanced gas, SO
2F
2: COS:H
2S:CS
2: SO
2=20:10; 9.65:3.78:10, get 0.1ml then and detect, obtain SF6, SO
2F
2, COS, H
2S, CS
2And SO
2Appearance time and appearance time zone.As seen from Figure 4, SF6 is the gas composition that occurs the earliest, and its appearance time goes out the peak concluding time about 4min about 3.2min, the appearance time zone between 3.0 ~ 4.2min, SO
2F
2, COS, H
2S, CS
2And SO
2Appearance time be respectively 4.598 min, 5.003 min, 5.087 min, 9.007 min and 10.675 min.
The chromatographic condition of gas chromatography is: injector temperature: 200 ℃, pressure: 25 psi, total flow: 41.498 ml/min, dottle pin purge flow rate: 3 ml/min, shunt mode: shunting 10:1, chromatographic column: J﹠W113-4362:260 ℃: 60 m * 320 μ m * 0 μ m, post oven temperature, degree: initial temperature is 60 ℃, keeps 6 min; Speed with 10 ℃/min rises to 150 ℃, keeps 2 min.
The detected temperatures of thermal conductivity detector (TCD) 15 is 200 ℃.
Gas composition in the sulfur hexafluoride electrical equipment failure gas to be measured quantitatively detects
(1)
The divided gas flow component:Sulfur hexafluoride electrical equipment failure gas to be measured is fed the separation chromatography post, is the phase that flows with helium, and sulfur hexafluoride and each sulfur-bearing failure gas component are carried out the gas chromatography separation.
Through the port 5 of six-way valve injector 13 ' go into helium, as mobile phase, through the port 1 ' injection sulfur hexafluoride electrical equipment failure gas of six-way valve injector 13, sample size is 0.1ml.
The chromatographic condition of gas chromatography is: injector temperature: 200 ℃, pressure: 25 psi, total flow: 41.498 ml/min, dottle pin purge flow rate: 3 ml/min, shunt mode: shunting 10:1, chromatographic column: J﹠W113-4362:260 ℃: 60 m * 320 μ m * 0 μ m, post oven temperature, degree: initial temperature is 60 ℃, keeps 6 min; Speed with 10 ℃/min rises to 150 ℃, keeps 2 min.
(2)
Discharge sulfur hexafluoride:Separated gas enters in the thermal conductivity detector (TCD) and detects, the detected temperatures of thermal conductivity detector (TCD) 15 is 200 ℃, appearance time zone with the sulfur hexafluoride standard items is for referencial use, when arriving or during near the appearance time of sulfur hexafluoride, namely approach or when arriving 3.0min, open six-way valve, port 1 and port 2, port 3 and port 4 and port 5 and port 6 are communicated with respectively, port 2 disconnects with port 3 and being connected, port 2, port 1, port 5 and port 6 are communicated with formation SF6 discharge-channel successively, sample gas passes through separation chromatography post 18 in proper order, thermal conductivity detector (TCD) 15, port 2, port 1, port 5, port 6 is discharged, by emptying, do not enter in the sulfur chemistry luminescence detector and detect at last.
(3)
The quantitative measurement of sulfur-bearing failure gas component:When arriving or going out the peak during concluding time near sulfur hexafluoride, namely arrive or during near 4.2min, close six-way valve, port 1 and port 6, port 2 and port 3 and port 3 and port 5 are communicated with respectively, port 2 and port 3 are communicated with, the conducting thermal conductivity detector (TCD) is connected with the sulfur chemistry luminescence detector, and port 4, port 5, port 1 and port 6 are communicated with formation carrier gas discharge-channel successively.At this moment, make separation of C OS, H owing to close impulse force that six-way valve 16 produces
2S, SO
2F
2, CS2, SO
2In the retention time of portion gas delay, at 4.595 min COS appears, H appears in 5.003 min
2SO appears in S, 5.067 min
2F
2, CS appears in 9.007 min
2SO appears with 10.675 min
2Sample gas separates by chromatographic column, through thermal conductivity detector (TCD) 15, enters into sulfur chemistry luminescence detector 14 and detects, testing conditions is: 225 ℃ of detector temperatures, 800 ℃ of double plasma chamber temperatures, hydrogen 45 ml/min, air 63 ml/min, the result as shown in Figure 5.And the typical curve of the part SF6 decomposition components of setting up, its parameter is as shown in the table:
The present invention can summarize with other the concrete form without prejudice to spirit of the present invention or principal character.The above embodiment of the present invention and test example all can only be thought explanation of the present invention rather than restriction, therefore every foundation essence technology of the present invention all belongs in the scope of technical solution of the present invention any trickle modification, equivalent variations and modification that above embodiment does.
Claims (10)
1. pick-up unit that quantitatively detects sulfur-bearing failure gas component in the sulfur hexafluoride electrical equipment, it is characterized in that, comprise the separation chromatography post, thermal conductivity detector (TCD) and sulfur chemistry luminescence detector, described separation chromatography post links to each other with thermal conductivity detector (TCD), thermal conductivity detector (TCD) is connected with the sulfur chemistry luminescence detector by a six-way valve, the sample outlet end of described thermal conductivity detector (TCD) is connected with the port 2 of six-way valve, the test entrance point of described sulfur chemistry luminescence detector is connected with six-way valve port 3, the switch of control six-way valve makes its port 2 and port 3 connections when sample introduction, the conducting thermal conductivity detector (TCD) is connected with the sulfur chemistry luminescence detector, when separating SF6, disconnecting thermal conductivity detector (TCD) is connected with the sulfur chemistry luminescence detector, port 2, port 1, port 5 and port 6 are communicated with formation SF6 discharge-channel, discharging SF6 successively.
2. according to the pick-up unit of sulfur-bearing failure gas component in the described quantitative detection sulfur hexafluoride electrical equipment of claim 1, it is characterized in that, also comprise carrier gas source, be used for the carrier gas supply, described carrier gas source is connected with flowing valve port 4.
3. according to the pick-up unit of sulfur-bearing failure gas component in the described quantitative detection sulfur hexafluoride electrical equipment of claim 1, it is characterized in that, also comprise helium gas source, this helium gas source is connected with the separation chromatography post by the six-way valve injector, and sulfur hexafluoride electrical equipment failure gas to be measured and helium enter the separation chromatography post through the six-way valve injector to carry out gas and separate.
4. according to the pick-up unit of sulfur-bearing failure gas component in the described quantitative detection sulfur hexafluoride electrical equipment of claim 1, it is characterized in that described separation chromatography post adopts capillary chromatographic column.
5. according to the pick-up unit of sulfur-bearing failure gas component in the described quantitative detection sulfur hexafluoride electrical equipment of claim 4, it is characterized in that described capillary chromatographic column is bore 0.32 mm, length is the gas-pro capillary chromatographic column of 60 m.
6. a method that adopts each described pick-up unit of claim 1 ~ 5 quantitatively to detect sulfur-bearing failure gas component in the sulfur hexafluoride electrical equipment is characterized in that, may further comprise the steps:
(1)
The divided gas flow component:Sulfur hexafluoride electrical equipment failure gas to be measured is fed the separation chromatography post, is the phase that flows with helium, gas composition is carried out gas chromatography separate;
(2)
Discharge sulfur hexafluoride:Separated gas enters in the thermal conductivity detector (TCD) and detects, appearance time and appearance time zone with the sulfur hexafluoride standard items are for referencial use, when arriving or during near the appearance time of sulfur hexafluoride, open six-way valve, port 2 disconnects with port 3 and being connected, port 2, port 1, port 5 and port 6 are communicated with successively, discharge sulfur hexafluoride;
(3)
The quantitative measurement of sulfur-bearing failure gas component:When arriving or going out the peak during concluding time near sulfur hexafluoride, close six-way valve, port 2 and port 3 are communicated with, the conducting thermal conductivity detector (TCD) is connected with the sulfur chemistry luminescence detector, residual gas in the described thermal conductivity detector (TCD) feeds in the sulfur chemistry luminescence detector and quantitatively detects, and then obtains each sulfur-bearing failure gas components contents.
7. the method for sulfur-bearing failure gas component in the quantitative detection sulfur hexafluoride electrical equipment according to claim 6, it is characterized in that, chromatographic condition is in the described step (1): injector temperature: 200 ℃, pressure: 25 psi, total flow: 41.498 ml/min, dottle pin purge flow rate: 3 ml/min, shunt mode: shunting 10:1, chromatographic column: J﹠W113-4362:260 ℃: 60 m * 320 μ m * 0 μ m, post oven temperature, degree: initial temperature is 60 ℃, keeps 6 min; Speed with 10 ℃/min rises to 150 ℃, keeps 2 min.
8. the method for sulfur-bearing failure gas component in the quantitative detection sulfur hexafluoride electrical equipment according to claim 6 is characterized in that the detected temperatures of thermal conductivity detector (TCD) is 200 ℃ described in the described step (2).
9. the method for sulfur-bearing failure gas component in the quantitative detection sulfur hexafluoride electrical equipment according to claim 6, it is characterized in that, the detected temperatures of described step (3) sulfur chemistry luminescence detector is 225 ℃, 800 ℃ of SCD gas ions burner temperature wherein, hydrogen 45 ml/min, air 63 ml/min.
10. the method for sulfur-bearing failure gas component in the quantitative detection sulfur hexafluoride electrical equipment according to claim 6, it is characterized in that, also comprise the step of measuring sulfur hexafluoride and each sulfur-bearing failure gas component appearance time zone, concrete operations are: the standard items of getting sulfur hexafluoride and each sulfur-bearing failure gas component are made into mixed gas, carry out gas chromatographic detection then, thereby obtain the appearance time zone of sulfur hexafluoride and each sulfur-bearing failure gas component, as the reference of subsequent step, the chromatographic condition of gas chromatography is identical with described step (1) chromatographic condition in this step.
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Address after: 510080 Dongfeng East Road, Dongfeng, Guangdong, Guangzhou, Zhejiang Province, No. 8 Patentee after: ELECTRIC POWER RESEARCH INSTITUTE, GUANGDONG POWER GRID CO., LTD. Address before: Guangzhou City, Guangdong province Yuexiu District 510080 Dongfeng East Road, No. 8 building water Kong Guangdong Patentee before: Electrical Power Research Institute of Guangdong Power Grid Corporation |