CN103105441B - Qualitative and quantitative analysis method for sulfur hexafluoride (SF6) gas discharge decomposition product - Google Patents
Qualitative and quantitative analysis method for sulfur hexafluoride (SF6) gas discharge decomposition product Download PDFInfo
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- CN103105441B CN103105441B CN201310014509.7A CN201310014509A CN103105441B CN 103105441 B CN103105441 B CN 103105441B CN 201310014509 A CN201310014509 A CN 201310014509A CN 103105441 B CN103105441 B CN 103105441B
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- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000004445 quantitative analysis Methods 0.000 title claims abstract description 20
- 238000004451 qualitative analysis Methods 0.000 title claims abstract description 16
- 229910018503 SF6 Inorganic materials 0.000 title abstract 5
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 title abstract 5
- 229960000909 sulfur hexafluoride Drugs 0.000 title abstract 5
- 150000001875 compounds Chemical class 0.000 claims abstract description 19
- 238000001514 detection method Methods 0.000 claims abstract description 13
- 238000005070 sampling Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 35
- 230000014759 maintenance of location Effects 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 8
- 238000010926 purge Methods 0.000 claims description 5
- 239000012159 carrier gas Substances 0.000 claims description 4
- 238000010812 external standard method Methods 0.000 claims description 3
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims description 3
- 238000002798 spectrophotometry method Methods 0.000 claims description 2
- 238000007599 discharging Methods 0.000 claims 1
- 101000856246 Arabidopsis thaliana Cleavage stimulation factor subunit 77 Proteins 0.000 abstract 1
- OBTWBSRJZRCYQV-UHFFFAOYSA-N sulfuryl difluoride Chemical compound FS(F)(=O)=O OBTWBSRJZRCYQV-UHFFFAOYSA-N 0.000 abstract 1
- DUGWRBKBGKTKOX-UHFFFAOYSA-N tetrafluoro(oxo)-$l^{6}-sulfane Chemical compound FS(F)(F)(F)=O DUGWRBKBGKTKOX-UHFFFAOYSA-N 0.000 abstract 1
- LSJNBGSOIVSBBR-UHFFFAOYSA-N thionyl fluoride Chemical compound FS(F)=O LSJNBGSOIVSBBR-UHFFFAOYSA-N 0.000 abstract 1
- 238000013459 approach Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 238000009413 insulation Methods 0.000 description 5
- 238000003822 preparative gas chromatography Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000012113 quantitative test Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 206010000372 Accident at work Diseases 0.000 description 1
- 208000033962 Fontaine progeroid syndrome Diseases 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 230000008033 biological extinction Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000012790 confirmation Methods 0.000 description 1
- 239000012611 container material Substances 0.000 description 1
- 238000012937 correction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229920002620 polyvinyl fluoride Polymers 0.000 description 1
- 238000011002 quantification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
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Abstract
The invention discloses a qualitative and quantitative analysis method for a sulfur hexafluoride (SF6) gas discharge decomposition product. The method comprises the following steps of: sampling; performing qualitative and quantitative analysis on a sample by a gas chromatograph-mass spectrograph, wherein a quadrupole rod quality detector is adopted, and a chromatographic column is a CP-Sil 5 CB capillary column. Compared with the prior art, the method can be used for detecting decomposition components comprehensively, detecting eight components including CF4, C2F6, CO2, SO2F2, SOF4, SOF2, SO2 and H2S synchronously, and performing fast recognition and accurate quantitative analysis on the compound. The detection on the SF6 decomposition product assists in an operator to know the insulating state inside electrical equipment so as to judge failure causes accurately.
Description
Technical field
The invention belongs to analysis detection field, be specifically related to a kind of qualitative and quantitative analysis SF
6the method of gas discharge decomposition product.
Background technology
SF
6gas has the good feature of stable chemical nature, safety non-toxic, insulation and arc extinction performance at normal temperatures, makes it be widely deployed in various electrical equipment as a kind of excellent insulating medium.But, along with the electric equipment operation time increases, various insulation fault problem will be there is, be characterized in before not puncturing, shelf depreciation occurring at device interior insulating medium.
SF
6generation, under the effect of shelf depreciation, is decomposed and is produced subfluoride, the O in these sub-stable materials and equipment by gas
2or H
2o reacts further and generates SO
2f
2, SOF
4, SOF
2, SO
2, H
2s, S
2f
10o, HF, CF
4deng product.Wherein, acidic materials SO
2, H
2s, HF have corrosive attack, destroy material and cause dielectric strength to decline, and then cause industrial accident.
For shelf depreciation, traditional detection method is as serious by on-the-spot electromagnetic interference (EMI) in electrical measuring method, ultrasonic method, and impact judges.By analyzing SF
6the kind of electric discharge decomposition product and concentration, can understand device interior state of insulation, for fault diagnosis provides an effective foundation.At present, research both domestic and external shows, the shelf depreciation that different insulative defect causes, SF
6difference is there is in electric discharge decomposition product in kind and generating rate.Therefore, need to find a kind of effective qualitative and quantitative analysis method, identification SF as much as possible
6electric discharge decomposition product, this is to accurately judging that insulation fault is significant.
At present, SF is analyzed
6the common method of gas discharge decomposition product is vapor-phase chromatography, infra-red sepectrometry.But there are the following problems in actual applications for these methods:
1) analysis result is not comprehensive.Utilize vapor-phase chromatography to SF
6the detection of electric discharge decomposition product, the selection of chromatographic column is even more important, and it determines follow-up qualitative and quantitative analysis to effective separation of target compound.In IEC60480-2004 standard, suggestion adopts Porapak Q packed column to be separated, but as can be seen from (Fig. 1) in feature spectrogram, SO
2f
2retention time and SF
6close, both go out peak simultaneously, can not realize being separated completely.Meanwhile, this pillar can not detect other decomposition products as SOF
4and H
2s.And if request for utilization number is 201010134902.6 " a kind of SF analyzed in electrical equipment
6the method of decomposition product " the Gas Pro chromatographic column of recommending in patent, although can SO be realized
2f
2with SF
6be separated, but SOF
2easily SO is changed in pillar
2and cannot detect, and it is to SOF
4detection also helpless.
2) to be accurately qualitatively not easy.Adopt vapor-phase chromatography to analyze unknown sample, qualitative progress needs retention time and known substance calibrating gas to compare, thus determines unknown sample composition.If jointly go out peak without calibrating gas or some composition, then can cause difficulty to accurately qualitative.
3) quantitatively there is interference mutually.Vapor-phase chromatography can only carry out integral and calculating to complete separation peak shape, and each target compound is separated as failed by testing process completely, and peak shape partial stack overlaps even completely then cannot accurate quantitative analysis, there is interference each other.
4) detection limit is not enough.Infra-red sepectrometry detects SF
6electric discharge decomposition product, although without the need to being separated various component, its detection limit is higher than vapor-phase chromatography, cannot detect the product of lower concentration.
Summary of the invention
Having the object of this invention is to provide one can multianalysis and accurate qualitative, quantitative SF
6the combined gas chromatography mass spectrometry analytical approach of gas discharge decomposition product.
To achieve these goals, technical scheme of the present invention is: provide a kind of qualitative and quantitative analysis SF
6the method of gas discharge decomposition product, key step comprises:
1) sample;
2) utilize gas chromatography-GC-MS to carry out qualitative and quantitative analysis to sample, detecting device is quadrupole rod mass detector, and chromatographic column adopts CP-Sil 5 CB capillary column.
Described step 2) the CP-Sil 5 CB chromatographic column selected, its parameter is: length is 60m, and thickness is 8 μm, and internal diameter is 0.32mm.
Preferably, described step 2) analytical approach, analysis condition is as follows, carrier gas: high-purity He gas (99.9999%); Post case temperature: initial 40 DEG C-60 DEG C, final 150
dEG C-220
dEG C; Heating rate: 5
dEG C/min-20 DEG C/min; Post flow: 0.9mL/min-1.2 mL/min; Purge flow rate: 3 mL/min.
Described step 2) analytical approach, analyze SF
6gas discharge decomposition product, its setting parameter is:
1. chromatographiccondition is as follows:
Carrier gas: high-purity He gas (99.9999%),
Sampling volume: 300 μ L,
Post case temperature: 40
dEG C constant temperature keeps 7min, with 15
dEG C/min ramp to 220
dEG C, keep 1min,
Injector temperature: 200
dEG C,
Sample introduction pattern: shunting,
Split ratio: 10,
Flow control mode: constant linear velocity,
Pressure: 56.1kPa,
Post flow: 1.2mL/min,
Purge flow rate: 3.0mL/min;
2. mass spectrophotometry condition is as follows:
Ion source temperature: 200 DEG C,
Interface temperature: 250
dEG C,
The detector switch time: after starting detection, open at time 2.9min, close at time 4.02min, open at time 4.26min, close at time 7min,
Detecting device acquisition mode: SIM,
Gather quasi-molecular ions: comprise the quasi-molecular ions that mass-to-charge ratio is 69,50,119,44,83,102,105,86,67,48,34,33,64,66.
Described step 2) analytical approach, synchronously utilize retention time and with reference to ion identification target compound, setting retention time deviation range ± 0.069min, setting with reference to Ion Phase to strength variance value 80%.
Described step 2) SF
6the analysis of electric discharge analyte detects and comprises: sample introduction; After starting detection, at SF
6before going out peak, analyze CF
4, C
2f
6(time period 2.9min-4.02min); Treat SF
6go out peak complete, reopen detecting device, Analysis for CO
2, SO
2f
2, SOF
4, SOF
2, H
2s, SO
2(time period 4.26min-7min).
Described step 2) analytical approach, the quantitative employing external standard method of target compound, sets up the typical curve that " concentration-peak area " is corresponding, optional zero crossing in typical curve linear fitting procedure, calculate peak area according to integrating meter, then calculate target compound concentration value by typical curve.For the C that cannot purchase calibrating gas
2f
6, adopt relative C
3f
8correction factor is that 1.0 modes carry out sxemiquantitative.
Described step 2) analytical approach, the quantitative test Monitoring lower-cut of various target compound is as follows:
Table 1 SF
6gas discharge decomposition product quantitative analysis method Monitoring lower-cut
| Gas composition | CF 4 | CO 2 | SO 2F 2 | SOF 4 | SOF 2 | H 2S |
| Minimum inspection limit (μ l/l) | 0.6 | 0.1 | 0.3 | 0.4 | 0.2 | 0.6 |
Note: adopt semiquantitative C
2f
6, and detect the SO by chromatographic column remaining influence
2, Monitoring lower-cut cannot be determined.
After the present invention adopts technique scheme, mainly contain following advantage:
1) detected components kind is comprehensive.Single injected sampling, adopts SF
6electric discharge decomposition product analytical approach, can detect CF
4, C
2f
6, CO
2, SO
2f
2, SOF
4, SOF
2, SO
2, H
28 kinds of components such as S.Testing process only needs to complete for 20 minutes, increases work efficiency, and reduces energy consumption.Detect material comprehensive, contribute to fully understanding inside electric appliance state of insulation, accurate failure judgement.
2) to unknown sample fast qualitative.Without the need to buying calibrating gas, utilize the known compound in the ion maps that detects and standard spectrum storehouse to compare can to realize qualitative.Utilize retention time and reference ion relative intensity, in accurate judgement sample, whether target compound exists simultaneously.
3) accurate quantitative analysis.For treating quantification compound, selected good object ion peak, after qualitative confirmation, only needs to carry out integration to collected specific objective quasi-molecular ions, can calculate concentration from typical curve.Even if two kinds even retention time of multiple compounds are close, as long as select different object ion peaks to carry out integral and calculating to different compound, accurate quantitative analysis can be carried out equally.Compared with gas chromatography, eliminate overlap of peaks cause cannot be quantitative impact.
Accompanying drawing explanation
Fig. 1 adopts the Porapak Q packed column of advising in existing IEC60480-2004 standard, carries out the typical color spectrogram that gas chromatographic detection obtains.
Fig. 2 is SF of the present invention in embodiment
6the testing result of gas discharge decomposition product analysis method.
Embodiment
Analysis SF described in the present embodiment
6the gas chromatography-mass spectrography method of gas discharge decomposition product, comprises the following steps:
1) sample.In order to avoid sampling container material is to the absorption detecting sample, the sampler bag that Tedlar material can be adopted to make gathers gaseous sample.During collection, the material of connecting line adopts teflon or stainless steel as far as possible.Before each sampling, utilize vacuum pump to be vacuumized by sampler bag, remove other gaseous impuritieies; Connecting line can carry out purging and vacuumizing with tested gas.The present embodiment adopts certain domestic SF
6the sample gas of gas after 96h shelf depreciation, and people is for adding a certain amount of CF
4, H
2s, with the validity of verification method.
2) Shimadzu gas chromatograph-mass spectrometer (GCMS) (GCMS-QP2010) is adopted to detect sample.Select CP-Sil 5 CB chromatographic column, its parameter is: length is 60m, and thickness is 8 μm, and internal diameter is 0.32mm.If chromatogram column length is short, separating effect is bad.Use high-purity He gas as carrier gas; Pin sample introduction, sampling volume is 300 μ L.
1. chromatographic condition is set:
Post case temperature: 40 DEG C of constant temperature keep 7min, with 15
dEG C/min ramp to 220 DEG C, keep 1min; Injector temperature: 200
dEG C; Sample introduction pattern: shunting, split ratio is 10; Flow control mode: constant linear velocity; Pressure: 56.1kPa; Post flow: 1.2mL/min; Purge flow rate: 3.0mL/min.
2. Mass Spectrometry Conditions is set:
Ion source temperature: 200
dEG C; Interface temperature: 250
dEG C; The detector switch time: after starting detection, open at time 2.9min, close at time 4.02min, open at time 4.26min, close at time 7min, select SIM type collection; Gather quasi-molecular ions: comprise the quasi-molecular ions that mass-to-charge ratio (m/z) is 69,50,119,44,83,102,105,86,67,48,34,33,64,66.
3) qualitative analysis, adopts retention time and with reference to ion identification compound, setting retention time band ± 0.069min, setting reference Ion Phase is to strength variance value 80%.
4) quantitative test, to the characteristic ion peak integration of target compound, substitutes into the peak area obtained " concentration-peak area " typical curve that external standard method draws gained, target compound concentration in calculation sample.
Fig. 2 detects SF for utilizing said method
6the result of gas discharge decomposition product.In figure, the corresponding compound of each quasi-molecular ions is followed successively by CF
4, C
2f
6, CO
2, SO
2f
2, SOF
4, SOF
2, H
2s, SO
2, each content is:
Above disclosedly be only preferred embodiment of the present invention, certainly can not limit the interest field of the present invention with this, therefore according to the equivalent variations that the claims in the present invention are done, still belong to the scope that the present invention is contained.
Claims (5)
1. a qualitative and quantitative analysis SF
6the method of gas discharge decomposition product, is characterized in that:
Utilize gas chromatography-GC-MS to 8 kinds of SF
6discharging product CF
4, C
2f
6, CO
2, SO
2f
2, SOF
2, SOF
4, H
2s, SO
2carry out qualitative and quantitative analysis, wherein, detecting device is quadrupole rod mass detector, and chromatographic column adopts CP-Sil 5CB capillary column, and chromatographiccondition is as follows:
Carrier gas: 99.9999% high-purity He gas;
Sampling volume: 300 μ L;
Post case temperature: 40 DEG C of constant temperature keep 7min, with 15 DEG C/min ramp to 220 DEG C, keeps 1min;
Injector temperature: 200 DEG C;
Sample introduction pattern: shunting;
Split ratio: 10;
Flow control mode: constant linear velocity;
Pressure: 56.1kPa;
Post flow: 1.2mL/min;
Purge flow rate: 3.0mL/min.
2. qualitative and quantitative analysis SF as claimed in claim 1
6the method of gas discharge decomposition product, is characterized in that:
Mass spectrophotometry condition is as follows:
Ion source temperature: 200 DEG C;
Interface temperature: 250 DEG C;
The detector switch time: after starting detection, open at time 2.9min, close at time 4.02min; Open at time 4.26min, close at time 7min;
Detecting device acquisition mode: SIM;
Gather quasi-molecular ions: comprise the quasi-molecular ions that mass-to-charge ratio is 69,50,119,44,83,102,105,86,67,48,34,33,64,66.
3. qualitative and quantitative analysis SF as claimed in claim 2
6the method of gas discharge decomposition product, is characterized in that: synchronously utilize retention time and with reference to ion identification target compound, set retention time deviation range ± 0.069min, and setting reference Ion Phase is to strength variance value 80%.
4. qualitative and quantitative analysis SF as claimed in claim 2
6the method of gas discharge decomposition product, is characterized in that: sample introduction, after starting detection, at SF
6before going out peak, at time period 2.9min-4.02min, analyze CF
4, C
2f
6; Treat SF
6go out peak complete, at time period 4.26min-7min, Analysis for CO
2, SO
2f
2, SOF
4, SOF
2, H
2s, SO
2.
5. qualitative and quantitative analysis SF as claimed in claim 2
6the method of gas discharge decomposition product, it is characterized in that: the quantitative employing external standard method of target compound, set up the typical curve that " concentration-peak area " is corresponding, optional zero crossing in typical curve linear fitting procedure, calculate peak area according to integrating meter, then calculate target compound concentration value by typical curve.
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