CN101799458A - Method for analyzing decomposition products of SF6 in electrical device - Google Patents
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Abstract
The invention discloses a method for analyzing decomposition products of SF6 in electric equipment. The method comprises the following steps: sampling; and analyzing and detecting a sample with a chromatograph, wherein the detection part of the chromatograph comprises a thermal conductivity detector (TCD) and fission-product detector (FPD) which are in serial connection, the chromatographic column adopts capillary column GS GasPro, and all the pipelines of the chromatograph must be passivated. By using the invention, the decomposition products such as SO2F2 in SF6 can be accurately analyzed; and by analyzing the decomposition impurities such as SO2F2, the internal operating condition of the SF6 gas isolating device can be effectively judged and the electric equipment failure can be successfully judged.
Description
Technical field
The invention belongs to the analyzing and testing field, relate to a kind of method of analyzing the decomposition product of the SF6 in the electrical equipment particularly.
Background technology
Sulfur hexafluoride (SF
6) be at normal temperatures and pressures a kind of colourless, tasteless, nontoxic, do not fire, the forming gas of chemical property stabilizer pole.SF
6Molecule be the symmetrical structure of single sulphur polyfluoro, have extremely strong electronegativity, give its excellent electric insulation and arc extinction performance.At present, SF
6As the insulating medium of a new generation, be widely used in high pressure, the electric equipment of UHV (ultra-high voltage).Fill SF
6The electrical equipment floor area few, running noises is little, no fire hazard has greatly improved the safe reliability of electric equipment operation.
SF
6Gas can decompose under the effect of overheated, electric arc, electric spark and corona discharge, and its decomposition product also can react with micro-moisture, electrode and the solid insulating material in the equipment, and its product more complicated has gaseous impurities, as carbon tetrafluoride (CF
4), fluoridize sulfonyl (SO
2F
2), fluoridize thionyl (SOF
2), sulphuric dioxide (SO
2), ten fluorine, one oxidation, two sulphur (S
2OF
10) etc., also have some solid impurities, as aluminum fluoride (AlF
3), tungsten fluoride (WF
6) etc., specifically decomposition approach sees the following form.
For operating electrical equipment, judge its device interior running status difficulty relatively, by analyzing and testing SF
6The decomposition product of gas is to judge SF
6Strong means of air insulating device internal operation situation.In recent years, Guangdong Province is by detecting SF
6CF in the gas
4And SO
2Content Deng decomposition product has successfully been judged a lot of electrical equipment malfunctions.According to former studies experience and real work, pass through SF
6The decomposition product SO of gas
2F
2Also can effectively judge SF
6Air insulating device internal operation situation is strong means successfully judging electrical equipment malfunction.
At present, analyze SF
6The common method of decomposition product is utilized the gc analysis SF6 decomposition product CF that is equipped with thermal conductivity detectors (TCD) for being equipped with the vapor-phase chromatography of thermal conductivity detectors (TCD)
4, SOF
2Realize easily, but to SO
2F
2And SO
2Quantitative measurement is difficulty very.Because SF
6In except that above-mentioned impurity, also have fluorocarbons class material, as perfluoroethane (C
2F
6), octafluoropropane (C
3F
8), ten fluorine butane (C
4F
10) etc., the same SO of these impurity
2F
2Can overflow altogether, can not make a distinction.Under the condition of some chromatographic column, SO
2F
2Even can not be from its background SF
6In separately, and and SF
6Overflow altogether, (Fig. 1 provides typical SF among the IEC60480-2004 to see Fig. 1 for details
6The decomposition product gas chromatogram).
Summary of the invention
Technical matters to be solved by this invention provides a kind of SF that analyzes in the electrical equipment
6The method of decomposition product.This method can effectively solve the prior art means can not accurately analyze SF
6Middle decomposition product SO
2F
2Problem, thereby accurately judge SF
6Air insulating device internal operation situation ensures the electrical equipment safe operation.
A kind of SF that analyzes in the electrical equipment
6The method of decomposition product may further comprise the steps:
Sampling;
Adopt gas chromatograph that sample is carried out analyzing and testing, described chromatographic test section is connected in series by thermal conductivity detectors (TCD) and two detecting devices of flame photometric detector (FPD) (FPD), chromatographic column adopting capillary column GS GasPro, described chromatographic whole pipelines must passivation.
Preferably, analyzing and testing parameter of the present invention is: adopt He gas as carrier gas; 50-80 ℃ of column oven initial temperature, finishing temperature 120-200 ℃, rate of heat addition 12-20 ℃/min.More preferably, adopt He gas as carrier gas, 50 ℃ of column oven initial temperatures, 1 ℃/min rises to 55 ℃, and 15 ℃/min rises to 180 ℃, and the tail wind drift amount of detecting device is 8-10ml/min.
Through a large amount of experiments, optimized parameter combinations is: adopt He gas as carrier gas; 50 ℃ of injector temperatures, pressure 11.6psi, flow 18.5ml/min, dottle pin purge flow rate 3ml/min, split sampling, split ratio is 5; Chromatographic column is by flow control, flow 2.577ml/min, aux. pressure 4.35psi; 50 ℃ of column oven initial temperatures, 1 ℃/min rises to 55 ℃, and 15 ℃/min rises to 180 ℃; 200 ℃ of TCD detector temperatures, reference flow 30ml/min, tail wind drift amount 8ml/min; 230 ℃ of FPD detector oven and auxiliary transmission line temperature, H
2Airshed 75ml/min, air mass flow 100ml/min, tail wind drift amount 10ml/min.
The described analyzing and testing of described step (2) comprising: sample introduction, testing sample by the FPD detecting device, are not mainly analyzed air, CF by the TCD detecting device
4, C
2F
6And SF
6
Work as SF
6Substantially go out and (promptly work as SF after the peak finishes
6After analysis finishes), testing sample is both by the TCD detecting device, and also by the FPD detecting device, the TCD detecting device is mainly analyzed C
3F
8, C
4F
10, the FPD detecting device is mainly analyzed SO
2F
2, SOF
2, S
2OF
10, SO
2
The SF that the present invention will adopt back
6The sample utilization is equipped with the gc analysis of TCD and FDP polyphone detecting device, utilizes the TCD detecting device to analyze SF
6Decomposition product CF
4, C
2F
6, C
3F
8, C
4F
10Deng, utilize the FPD detecting device to analyze SF
6Decomposition product SOF
2, SO
2F
2, S
2OF
10Deng.Described method is being utilized gc analysis SF
6During decomposition product, all the gas sample all enters the analysis of TCD detecting device, and SF is only arranged
6Each component after the component just enters the FPD detecting device, because the SF that adopts back
6The overwhelming majority is SF in the sample
6If, the SF that these are excessive
6All enter the FPD detecting device, can pollute the FPD detecting device, influence subsequent measurements.This method not only can accurately be measured CF
4, C
2F
6, C
3F
8, C4F
10Deng impurity, can also accurately measure SOF
2, SO
2F
2, S
2OF
10Deng impurity, make SF
6The analysis of decomposition product is more accurate, thereby can more effective judgement electrical equipment malfunction.
Description of drawings
Fig. 1 is the vapor-phase chromatography SF that uses thermal conductivity detectors in the prior art
6The decomposition product gas chromatogram;
Fig. 2-4 is respectively among the embodiment 1, the chromatograph structural drawing of being made up of two detecting devices polyphones of TCD and FPD under the different conditions;
Fig. 5 is a TCD detecting device analysis result synoptic diagram in the prior art among the embodiment 1;
Fig. 6 is the method for the invention analysis result synoptic diagram among the embodiment 1;
Fig. 7 is a TCD detecting device analysis result synoptic diagram in the prior art among the embodiment 2;
Fig. 8 is the method for the invention analysis result synoptic diagram among the embodiment 2.
Embodiment
Below by embodiment the present invention is carried out concrete description, only be used for the present invention is further specified, can not be interpreted as qualification protection domain of the present invention.
SF in the described analysis electrical equipment of present embodiment
6The method of decomposition product may further comprise the steps:
(1) sampling: each technical scheme of spot sampling part is all identical with prior art, the sulfur hexafluoride sample of gathering from hold-up vessel must be representative, sample should be taken from liquid sulfur hexafluoride, if there is not liquid sulfur hexafluoride in hold-up vessel, the sample of being gathered can only be represented the sulfur hexafluoride of gaseous state so.Before sampling from hold-up vessel, storage tank and analytical equipment or all should vacuumize by vacuum pump with all coupling parts of sulfur hexafluoride gas gas production bottle.If thief hatch is to use long and narrow pipe to link in the main gas tank of hold-up vessel, then the gas purging in the hold-up vessel should be used in the pipeline coupling part, and is representative with the sulfur hexafluoride gas sample of guaranteeing to gather from hold-up vessel.During sampling, connect material and should select stainless steel or other that material of chemical reaction does not take place as far as possible, to reduce reaction and the pollution in the sampling process.Analytic sample can not pass through filtrator (molecular sieve, aluminium oxide), otherwise can change the composition of gas.For guaranteeing that sample is not subjected to the pollution of dust, can use dust filter unit.In order to reduce the discharging of sulfur hexafluoride gas to atmosphere, limit of the harm of poisonous analyte simultaneously to human body, can use collecting bag, or similarly install.Gas in the collecting bag also should reclaim.
(2) employing is chromatographic carries out analyzing and testing to sample:
(A) chromatographic analyzing and testing part must can be realized by TCD and two detecting device polyphones of FPD.Concrete detecting device connection layout can be referring to Fig. 2-4, and as shown in the figure, chromatograph mainly comprises flow control system 1 and auxiliary flow control system 2, chromatogram injection port 3, chromatographic column 4, TCD detecting device 5 and FPD detecting device 6, six-way valve 7 and six-way valve 8.
(B) chromatographic column adopting capillary column GS GasPro (J﹠amp; W, 60 meters * 0.32 millimeter), this chromatographic column can realize SO
2F
2With the separation fully of background SF6, and adopt other chromatographic column then not reach requirement as former used conventional post (stainless-steel tube, interior dress porous polymer type porapak Q, 3-4 rice x3 millimeter);
(C) the necessary passivation of chromatographic whole pipeline is because part SF
6Decomposition product such as SO
2F
2And SO
2Have severe corrosive,, can influence SO as the not passivation of equipment pipeline
2F
2And SO
2Quantitative test.Experimental results show that: chromatograph is during without transpassivation, SF
6The sample introduction number of times of sample to reach 5 times and more than, just can obtain stablizing constant chromatogram;
(D) detected parameters is set, and concrete chromatographic parameter is as follows: adopt He gas as carrier gas; 50 ℃ of injector temperatures, pressure 11.6psi, flow 18.5ml/min, dottle pin purge flow rate 3ml/min, split sampling, split ratio is 5; Chromatographic column is by flow control, flow 2.577ml/min, aux. pressure 4.35psi; 50 ℃ of column oven initial temperatures, 1 ℃/min rises to 55 ℃, and 15 ℃/min rises to 180 ℃; 200 ℃ of TCD detector temperatures, reference flow 30ml/min, tail wind drift amount 8ml/min; 230 ℃ of FPD detector oven and auxiliary transmission line temperature, H
2Airshed 75ml/min, air mass flow 100ml/min, (this tail wind drift amount is generally bigger when using the FPD detecting device separately for tail wind drift amount 10ml/min, about 30ml/min, but when TCD and FPD detecting device polyphone use, because TCD carrier gas or auxiliary gas also enter the FPD detecting device, be provided with excessively as tail wind drift amount, make the FPD fray-out of flame easily).
(E), stratographic analysis concrete steps:
(1) flushing quantity tube, preparation sample introduction: by repeatedly flushing, testing sample is by the injection port of six-way valve, enter quantity tube, prepare to analyze, this moment instrument connection layout as shown in Figure 2, six-way valve 7 cuts out in two six-way valves, six-way valve 8 is opened, sample rests on quantity tube, does not enter instrument analysis by the chromatogram injection port;
(2) sample introduction: this moment, six-way valve 7 became opening (about 0.01 minute time action) by closed condition, carrier gas is blown into the chromatogram injection port with the gas to be measured in the quantity tube, enter chromatographic column analysis, six-way valve 8 states are constant, the connection layout of instrument as shown in Figure 3, testing sample is by the TCD detecting device, and by the FPD detecting device, this stage can not analyzed air, CF
4, C
2F
6And SF
6Deng material;
(3) sample analysis: treat SF
6Substantially after going out the peak and finishing, six-way valve 8 becomes closed condition (about 3 minutes time action) by opening, and six-way valve 7 states are constant, the connection layout of instrument as shown in Figure 4, this moment, testing sample both passed through the TCD detecting device, and also by the FPD detecting device, this stage can not only be analyzed C by TCD
3F
8, C
4F
10Deng the fluorocarbons material, can also analyze SO by FPD
2F
2, SOF
2, S
2OF
10, SO
2Deng sulfur-containing impurities;
(4) quantitative test: adopt external standard method to carry out quantitative test, each content of material goes out the peak area linear dependence at peak with it in the TCD detecting device, and the content of each material goes out the peak area correlation of indices at peak with it in the FPD detecting device.
Specifically see Fig. 5 and Fig. 6, Fig. 5 is the result who analyzes with the independent TCD detecting device of the same sample of present embodiment in the prior art, and five impurity peaks among the figure are followed successively by air, CF
4, C
2F
6, C
3F
8, SO
2F
2, as seen from the figure, C
3F
8And SO
2F
2Can not separate fully, particularly work as C
3F
8Content is far above SO
2F
2The time, SO
2F
2Can not accurately measure; Fig. 6 is the result that present embodiment FPD detecting device is analyzed, and the impurity peaks among the figure is SO
2F
2, this shows, analyze SF by the FPD detecting device
6Decomposition product SO
2F
2The time not disturbed by other impurity, relatively accurately.In electrical equipment, do not have generally can not have SO in the air chamber of fault
2F
2If have SO through the collected specimens analyzing and testing in certain air chamber
2F
2, then must fully pay close attention to, if SO in this air chamber
2F
2The content sustained growth, then the possibility of this air chamber fault is very big.
SF in the described analysis electrical equipment of present embodiment
6The method of decomposition product, step is substantially the same manner as Example 1, and different is: the analyzing and testing parameter is specially: He gas is as carrier gas; 80 ℃ of column oven initial temperatures, 200 ℃ of finishing temperatures, 20 ℃/min of the rate of heat addition, concrete See Figure.Wherein, Fig. 7 is the result who analyzes with the independent TCD detecting device of the same sample of present embodiment in the prior art, and three impurity peaks among the figure are followed successively by air, CF
4, C
3F
8And SO
2F
2Overflow the peak altogether, as seen from the figure, C
3F
8And SO
2F
2Overflow altogether, can not separate; Fig. 8 is the result that present embodiment FPD detecting device is analyzed, and the impurity peaks among the figure is SO
2F
2, this shows, analyze SF by the FPD detecting device
6Decomposition product SO
2F
2The time not disturbed by other impurity, relatively accurately.In electrical equipment, do not have generally can not have SO in the air chamber of fault
2F
2If have SO through the collected specimens analyzing and testing in certain air chamber
2F
2, then must fully pay close attention to, if SO in this air chamber
2F
2The content sustained growth, then the possibility of this air chamber fault is very big.
Claims (5)
1. SF who analyzes in the electrical equipment
6The method of decomposition product is characterized in that, mainly may further comprise the steps:
(1) sampling;
(2) adopt gas chromatograph that sample is carried out analyzing and testing, the test section of described gas chromatograph is connected in series by thermal conductivity detectors and flame photometric detector (FPD), chromatographic column adopting capillary column GS GasPro, whole pipeline passivation of described gas chromatograph.
2. analytical approach according to claim 1 is characterized in that, the analyzing and testing parameter is: adopt He gas as carrier gas; 50-80 ℃ of column oven initial temperature, finishing temperature 120-200 ℃, rate of heat addition 12-20 ℃/min, the tail wind drift amount of detecting device is 8-10ml/min.
3. analytical approach according to claim 2 is characterized in that, described column oven initial temperature is 50 ℃, and 1 ℃/min rises to 55 ℃, and 15 ℃/min rises to 180 ℃.
4. analytical approach according to claim 3 is characterized in that, the analyzing and testing parameter is: adopt He gas as carrier gas; 50 ℃ of injector temperatures, pressure 11.6psi, flow 18.5ml/min, dottle pin purge flow rate 3ml/min, split sampling, split ratio is 5; Chromatographic column is by flow control, flow 2.577ml/min, aux. pressure 4.35psi; 50 ℃ of column oven initial temperatures, 1 ℃/min rises to 55 ℃, and 15 ℃/min rises to 180 ℃; 200 ℃ of thermal conductivity detectors temperature, reference flow 30ml/min, tail wind drift amount 8ml/min; 230 ℃ of flame photometric detector (FPD) well heater and auxiliary transmission line temperature, H
2Airshed 75ml/min, air mass flow 100ml/min, tail wind drift amount 10ml/min.
5. according to each described analytical approach of claim 1-4, it is characterized in that the described analyzing and testing of step (2) comprising: sample introduction, testing sample by flame photometric detector (FPD), are not mainly analyzed air, CF by thermal conductivity detectors
4, C
2F
6And SF
6
Work as SF
6Substantially after going out the peak and finishing, testing sample is both by thermal conductivity detectors, and also by flame photometric detector (FPD), thermal conductivity detectors is mainly analyzed C
3F
8, C
4F
10, flame photometric detector (FPD) is mainly analyzed SO
2F
2, SOF
2, S
2OF
10, SO
2
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