CN111679025A - Gas chromatography detection system and method for determining gas components of perfluoroisobutyronitrile - Google Patents
Gas chromatography detection system and method for determining gas components of perfluoroisobutyronitrile Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 41
- AASDJASZOZGYMM-UHFFFAOYSA-N 2,3,3,3-tetrafluoro-2-(trifluoromethyl)propanenitrile Chemical compound FC(F)(F)C(F)(C#N)C(F)(F)F AASDJASZOZGYMM-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 238000004817 gas chromatography Methods 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims description 16
- 238000004458 analytical method Methods 0.000 claims abstract description 42
- 239000007789 gas Substances 0.000 claims description 87
- 239000012159 carrier gas Substances 0.000 claims description 40
- 239000012535 impurity Substances 0.000 claims description 31
- 238000004587 chromatography analysis Methods 0.000 claims description 13
- 238000010926 purge Methods 0.000 claims description 13
- 239000000126 substance Substances 0.000 claims description 10
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims description 8
- 238000002347 injection Methods 0.000 claims description 8
- 239000007924 injection Substances 0.000 claims description 8
- 238000000926 separation method Methods 0.000 claims description 7
- 238000011010 flushing procedure Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 238000007664 blowing Methods 0.000 claims description 5
- 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
- 239000000463 material Substances 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims 1
- 238000000354 decomposition reaction Methods 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 229910018503 SF6 Inorganic materials 0.000 description 7
- 238000010586 diagram Methods 0.000 description 6
- QYSGYZVSCZSLHT-UHFFFAOYSA-N octafluoropropane Chemical compound FC(F)(F)C(F)(F)C(F)(F)F QYSGYZVSCZSLHT-UHFFFAOYSA-N 0.000 description 6
- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 description 5
- 229960000909 sulfur hexafluoride Drugs 0.000 description 5
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical group FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 4
- 229960004065 perflutren Drugs 0.000 description 4
- 238000013461 design Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- SFFUEHODRAXXIA-UHFFFAOYSA-N 2,2,2-trifluoroacetonitrile Chemical compound FC(F)(F)C#N SFFUEHODRAXXIA-UHFFFAOYSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- -1 fluorocarbon compound Chemical class 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 238000013022 venting Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/8872—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample impurities
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention provides a gas chromatography detection system and a gas chromatography detection method for detecting gas components of perfluoroisobutyronitrile, wherein the gas chromatography detection system comprises the following steps: a first analysis unit and a second analysis unit; the first analysis unit comprises a first switching valve, a third chromatographic column, a third switching valve and a first detector which are sequentially connected; a first interface on the first switching valve is connected with a gas sample source to be detected; and a second emptying valve is arranged on the third switching valve. The second analysis unit comprises a second switching valve, a first chromatographic column, a second chromatographic column, a fourth switching valve and a second detector which are connected in sequence; a first interface on the second switching valve is connected with a gas sample source to be detected; a third emptying valve is arranged on the second switching valve; and a fourth emptying valve is arranged on the fourth switching valve. The gas chromatography system provided by the invention can realize the C-pair only by one instrument4F7N‑CO2The accurate analysis of all components of the decomposition product of the mixed gas is beneficial to accurately judging the running condition of the electrical equipment; at the same time, the time for analysis is shortened.
Description
Technical Field
The invention relates to the technical field of analytical chemistry, in particular to a gas chromatography detection system and a gas chromatography detection method for detecting gas components of perfluoroisobutyronitrile.
Background
Sulfur hexafluoride (SF) is commonly used in gas-insulated electrical equipment6) Gas as insulating medium, but due to SF6Has strong greenhouse effect and GWP value of about CO223900 times of the power grid, which hinders the green development of the power grid in China and even in the world. Thus, an environmentally friendly SF having an electrical performance equivalent thereto is sought6The alternative gas becomes a hot spot of domestic and foreign research in recent years. In 2014, Alston, France screened a gaseous perfluoroisobutyronitrile (C) named Novec-4710 from the 3M company refrigerant catalog4F7N）。C4F7The insulating property of N is SF under the same condition6More than 2.2 times of the total weight of the sulfur-containing catalyst, and the GWP (global warming potential) is far lower than that of SF6A gas. However, it also suffers from the problem of high liquefaction temperature, and ALSTOM has to mix Novec ™ 4710 with CO2Mixing and using. Can be generally mixed with CO due to higher liquefaction temperature2When the mixed gas is used in a mixed mode, the insulating strength of the mixed gas can still reach SF under the same condition687% -96% of the total weight of the steel. It has been applied to a 145kV GIS by american general companies because it has excellent properties as a good substitute gas.
In the operation process of the electrical equipment, if the equipment fails, partial discharge and other phenomena may occur. Under discharge conditions C4F7N-CO2The mixed gas is decomposed and a large amount of CF may be generated3Radicals, CN radicals, CF radicals, the combination of which can take place in complex chemical reactions, giving, for example, CF3CN and the like, and the operation condition of the equipment can be inferred by detecting the content of the impurities. No C is available on the market at present4F7N-CO2The detection method of the mixed gas system generally utilizes a plurality of instruments for detection, such as TCD (thermal conductivity detector), FTIR and the like, and the detected impurities cannot comprise the characteristic impurities of the decomposition products, the detection limit cannot be satisfactory, and the detection C can be effectively and quickly detected4F7N-CO2Mixing gases is a technical problem.
For detection C4F7The currently reported detection methods include Fourier infrared spectroscopy (FTIR), GC-MS and the like, the detection methods are simple, the impurity types are less, and the chromatography is independently adopted for C4F7Systems and methods for detecting the decomposition products of N have not been reported.
Disclosure of Invention
In view of this, the invention provides a gas chromatography detection system and a gas chromatography detection method for detecting perfluoroisobutyronitrile gas components, and aims to solve the problem of C in the prior art4F7N-CO2The detection efficiency is low when impurity components in the mixed gas are detected.
In one aspect, the present invention provides a gas chromatography detection system for detecting a gas component of perfluoroisobutyronitrile, comprising: a first analysis unit and a second analysis unit; the first analysis unit comprises a first switching valve, a third chromatographic column, a third switching valve and a first detector which are sequentially connected; a first interface on the first switching valve is connected with a gas sample source to be detected; a second emptying valve is arranged on the third switching valve; the second analysis unit comprises a second switching valve, a first chromatographic column, a second chromatographic column, a fourth switching valve and a second detector which are connected in sequence; a first interface on the second switching valve is connected with a gas sample source to be detected; a third emptying valve is arranged on the second switching valve; and a fourth emptying valve is arranged on the fourth switching valve.
Further, in the gas chromatography detection system for detecting the gas component of perfluoroisobutyronitrile, the first carrier gas is connected to the fifth port of the first switching valve; the gas sample inlet to be detected is connected with the first interface of the first switching valve; the second interface of the first switching valve is connected with the first interface of the second switching valve; a first quantitative pipe is arranged on a pipeline connecting the third interface of the first switching valve with the sixth interface of the first switching valve; and the fourth interface of the first switching valve is connected with the first end of the third chromatographic column.
Further, in the above gas chromatography detection system for measuring a perfluoroisobutyronitrile gas component, a fourth carrier gas is connected to the fourth port of the second switching valve, and a third carrier gas is connected to the seventh port of the second switching valve; the third vent valve is connected with an eighth interface of the second switching valve, and a gas sample outlet to be detected is connected with a second interface of the second switching valve; a second quantitative pipe is arranged on a pipeline connecting the third interface of the second switching valve and the tenth interface of the second switching valve; the first chromatographic column is arranged on a pipeline connecting the fifth interface of the second switching valve and the ninth interface of the second switching valve; and the second chromatographic column is arranged on a pipeline connecting the sixth interface of the second switching valve with the sixth interface of the fourth switching valve.
Further, in the above gas chromatography detection system for measuring a perfluoroisobutyronitrile gas component, the second carrier gas is connected to a third port of the third switching valve, the second purge valve is connected to a first port of the third switching valve, and the first detector is connected to a fifth port of the third switching valve; the other end of the third chromatographic column is connected with a sixth interface of the third switching valve; the second port of the third switching valve is connected with the fourth port of the third switching valve.
Further, in the above gas chromatography detection system for measuring a perfluoroisobutyronitrile gas component, the fifth carrier gas is connected to a third port of the fourth switching valve, the fourth purge valve is connected to a first port of the fourth switching valve, and the second detector is connected to a fifth port of the fourth switching valve; the second port of the fourth switching valve is connected with the fourth port of the fourth switching valve.
Further, in the gas chromatography detection system for detecting the gas component of perfluoroisobutyronitrile, the first detector and the second detector are both pulse helium ionization detectors.
Further, in the above gas chromatography detection system for measuring a perfluoroisobutyronitrile gas component, the first switching valve, the third switching valve, and the fourth switching valve are six-way purge pneumatic switching valves, and the second switching valve is a ten-way purge pneumatic switching valve.
Further, in the gas chromatography detection system for detecting the gas component of perfluoroisobutyronitrile, the first chromatographic column is a special analysis pre-column for C4F 7N; the second chromatographic column is a special C4F7N analytical column, and the third chromatographic column is a fluorocarbon analytical capillary column.
In the invention, the C pair can be realized by only one instrument4F7N-CO2The accurate analysis of all components of the decomposition product of the mixed gas is beneficial to accurately judging the running condition of the electrical equipment; meanwhile, the labor force and the testing time are saved, the investment cost of the instrument is also reduced, the use cost is greatly reduced, and the maintenance cost of the instrument is correspondingly reduced; in addition, the sampling amount can be reduced by adopting one instrument for analysis, the use amount of the sample gas and the treatment amount of the used sample are reduced, and the device is safer and more environment-friendly.
In another aspect, the present invention further provides a gas chromatography method for determining a gas component of perfluoroisobutyronitrile, comprising the steps of: step (1), the first switching valve adopts a valve sample introduction mode to introduce samples through a C of a first quantitative pipe4F7N-CO2After most of the fluorocarbon compounds in the mixed gas are separated by the third chromatographic column, the third switching is switchedSwitching the separated fluorocarbon into a first detector by a valve in response to a peak; step (2), the second switching valve is carried out in a back-flushing sample injection mode and passes through the C of the second quantitative pipe4F7N-CO2Pre-separating the mixed gas by a first chromatographic column to obtain Air, CO and CF4、CO2And C2F6The mixture enters a second chromatographic column, and then a second switching valve is switched to perform back flushing pre-separation to obtain other impurity components; switching a fourth switching valve to separate impurity components Air, CO and CF of the second chromatographic column4、CO2And C2F6Respectively switched to respond to peaks in the second detector.
Further, in the method for analyzing the gas component of perfluoroisobutyronitrile, the sample injection step is as follows:
switching the first switching valve, enabling the first carrier gas to carry the gas sample to be detected in the first quantitative tube to enter the third chromatographic column, simultaneously shunting through a tee joint and a first emptying valve, and enabling the third chromatographic column to have a peak at C3F8The previous material is emptied through a second emptying valve; switching the third switching valve so that C3F8And then the impurity components enter a first detector respectively to generate peaks; wait for C2F5After CN finishes the peak, the third switching valve is switched to return to the initial state, and for C4F7N, emptying;
switching the second switching valve and the fourth switching valve, wherein a fourth carrier gas carries the gas sample to be detected in the second quantitative tube to enter the first chromatographic column, and when C in the first chromatographic column2F6And peak at C2F6The former substance enters the second chromatographic column and then the second switching valve is switched to lead the peak to be C2F6The subsequent substances are subjected to back blowing and emptying through a third emptying valve; simultaneously, the third carrier gas carries impurities separated from the second chromatographic column to enter a second detector to finish peak emergence until CF4After the peak is generated, the fourth switching valve is switched to empty through the fourth emptying valve, and when CO is discharged2Cutting after completely emptyingThe fourth switching valve is switched back to the initial state, so that C2F6And (4) peak generation.
The method for analyzing the gas component of the perfluoroisobutyronitrile can complete C by one-time sample injection4F7N-CO2Various impurities in the mixed gas are analyzed, instrument and human errors caused by multiple sample introduction are avoided, the analysis accuracy is improved, the analysis time is short, and related electrical equipment users can timely and accurately judge the running state of the electrical equipment according to the analysis result so as to timely take corresponding safety measures.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a schematic diagram of a connection structure of a gas chromatography detection system for detecting a gas component of perfluoroisobutyronitrile according to an embodiment of the present invention;
FIG. 2 shows an embodiment of the present invention in which the sampling is completed by the first switching valve, the flow is split by the tee and the first vent valve, and CO is vented by the second vent valve2A schematic flow diagram of (a);
FIG. 3 shows a block diagram of a block diagram C according to an embodiment of the present invention3F8Impurities enter the first detector and pass through the third switching valve pair C4F7N is used for emptying;
FIG. 4 shows an embodiment of the present invention in which a fourth carrier gas carries the sample in the second quantitative tube into the first chromatographic column and C is in the first chromatographic column2F6And peak at C2F6The previous substances are all put into a second chromatographic column for separation;
FIG. 5 shows a blow-down reverse blow-off peak at C by the third blow-down valve in the embodiment of the present invention2F6A schematic flow diagram of the following material;
FIG. 6 is a diagram showing a chromatographic analysis of each impurity gas component in the first detector in the embodiment of the present invention;
FIG. 7 is a chromatogram of each impurity gas component in the second detector in the example of the present invention.
In the figure: 1-a first switching valve; 2-a second switching valve; 3-a third switching valve; 4-a fourth switching valve; 5-a first chromatographic column; 6-second chromatography column; 7-third chromatographic column; 8-a first carrier gas; 9-a second carrier gas; 10-a third carrier gas; 11-a fourth carrier gas; 12-a fifth carrier gas; 13-a first dosing tube; 14-a second dosing tube; 15-gas sample inlet to be measured; 16-gas sample outlet to be measured; 17-a first vent valve; 18-a second vent valve; 19-a third vent valve; 20-a fourth vent valve; 21-a tee joint; 22-a first detector; 23-second detector.
Detailed Description
Exemplary embodiments of the present disclosure will be described in more detail below with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art. It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
Referring to fig. 1, a gas chromatography detection system for detecting a gas component of perfluoroisobutyronitrile according to an embodiment of the present invention includes: a first analysis unit and a second analysis unit; wherein, the first analysis unit comprises a first switching valve 1, a third chromatographic column 7, a third switching valve 3 and a first detector 22 which are connected in sequence; a first interface on the first switching valve 1 is connected with a gas sample source to be detected; and a second emptying valve 18 is arranged on the third switching valve 3.
The second analysis unit comprises a second switching valve 2, a first chromatographic column 5, a second chromatographic column 6, a fourth switching valve 4 and a second detector 23 which are connected in sequence; the first interface 201 on the second switching valve 2 is connected with a gas sample source to be detected; a third emptying valve 19 is arranged on the second switching valve 2; and a fourth emptying valve 20 is arranged on the fourth switching valve 4.
Specifically, the gas to be measured in the present invention is C4F7N-CO2Mixed gas, in this example C was determined by means of a first analysis unit4F7N-CO2C in decomposition products of mixed gases3F8(octafluoropropane) C2HF5Cl（R125）、C2H3F3（R143a）、C2H2F4（R134a）、C3F6(Hexafluoropropylene) and C2F5The content of CN; determination of C by means of a second analysis unit4F7N-CO2Air, CO, CF in decomposition products in mixed gas4And C2F6The content of (a). The interfaces and corresponding interfaces of the first switching valve 1, the third chromatographic column 7 and the third switching valve 3 are connected with the first detector 22 through gas pipelines; the interfaces of the second switching valve 2, the first chromatographic column 5, the second chromatographic column 6 and the fourth switching valve 4, and the corresponding interfaces and the second detector 23 are all connected through gas pipelines. The second, third and fourth dump valves 18, 19, 20 may all be needle valves.
Preferably, the first switching valve 1, the third switching valve 3, and the fourth switching valve 4 are six-way purge pneumatic switching valves, and the second switching valve 2 is a ten-way purge pneumatic switching valve. Through reasonably switching the switching valves, the chromatographic analysis process can be effectively simplified, the chromatographic analysis time is shortened, and the chromatographic analysis working efficiency is greatly improved.
Preferably, the first chromatographic column 5 is C4F7N dedicated analytical pre-column, e.g. high polarity molecular column (strong polarity and medium polarity molecular column) can be used to realize air, C2F6Etc. and C4F7Pre-separating N; the second chromatographic column 6 is C4F7The N special analytical column can be, for example, a molecular sieve chromatographic column to realize air, CO and CF4、CO2And C2F6The third chromatographic column 7 is a fluorocarbon compound analysis capillary column, and for C4F7N decomposition product C3F8(octafluoropropane) C2HF5Cl（R125）、C2H3F3（R143a）、C2H2F4（R134a）、C3F6(Hexafluoropropylene) and C2F5And CN is separated. The selection of a proper chromatographic column can separate specific impurity components, and the interference among impurities is avoided.
The first detector 22 and the second detector 23 can be both pulsed helium ionization detectors, which ensures high analytical sensitivity and can limit the detection of all components to 50 ppb.
For flexible control of the first analysis unit, it is preferred that the first carrier gas 8 is connected to the fifth port of the first switching valve 1; a first interface of the first switching valve 1 is connected with a gas sample inlet 15 to be detected; the second port 102 of the first switching valve 1 is connected to the first port 201 of the second switching valve 2, that is, the second switching valve 2 is connected to the gas sample line to be measured through the second port of the first switching valve 1. A first quantitative pipe 13 is arranged on a pipeline connecting the third interface 103 of the first switching valve 1 and the sixth interface 106 of the first switching valve 1; the fourth port 104 of the first switching valve 1 is connected to the first end of the third chromatography column 7.
Preferably, a flow splitting unit is arranged between the first switching valve 1 and the third chromatographic column 7. More specifically, the flow dividing unit includes: a tee 21 and a first vent valve 17; one end of the tee joint is communicated with the second end of the third chromatographic column, and the other end of the tee joint 21 is communicated with the first emptying valve 17. Namely, a tee joint 21 is arranged on a pipeline connecting the first switching valve 1 and the third chromatographic column 7, and the other end of the tee joint 21 is connected with a first emptying valve 17. It should be noted that the first end of the third column 7 may be an inlet end and the second end may be an outlet end.
In this embodiment, the first quantitative tube 13 is disposed on the first switching valve 1, so that the amount of the sample can be accurately controlled, and the amount of the sample can be saved. The first purge valve 17 may be a needle valve.
The specification of the tee joint 21 is matched with the capillary column interface in the third chromatographic column 7, and the special capillary column interface tee joint 21 reduces the dead volume, reduces the noise and effectively avoids air interference. The gas sample to be detected entering the third chromatographic column 7 is prevented from being too high in content by shunting through the tee joint 21 and the first emptying valve 17, so that the service life of the capillary column of the third chromatographic column 7 is prolonged, and the interference problem of main peak tailing in the third chromatographic column 7 is reduced.
The second carrier gas 9 is connected to a third port 33 of the third switching valve 3, the second purge valve 18 is connected to a first port 31 of the third switching valve 3, and the first detector 22 is connected to a fifth port 35 of the third switching valve 3; the other end of the third chromatographic column 7 is connected with a sixth interface 36 of the third switching valve 3; the second connection 32 of the third switching valve 3 is connected to a fourth connection 34 of the third switching valve 3. The design of the flow ensures C4F7N and CO2The emptying of (2) can effectively avoid that the main peak enters the first detector 22 to influence the analysis of the impurity content.
For flexible control of the second analysis unit, it is preferred that the fourth carrier gas 11 is connected to the fourth port 204 of the second switching valve 2, and the third carrier gas 10 is connected to the seventh port 207 of the second switching valve 2; the third vent valve 19 is connected with the eighth interface 208 of the second switching valve 2, and the gas sample outlet 16 to be measured is connected with the second interface 202 of the second switching valve 2; a second quantitative pipe 14 is arranged on a pipeline connecting the third interface 203 of the second switching valve 2 with the tenth interface 210 of the second switching valve 2; the first chromatographic column 5 is arranged on a pipeline connecting the fifth interface 205 of the second switching valve 2 and the ninth interface 209 of the second switching valve 2; the second chromatographic column 6 is arranged on a pipeline connecting the sixth interface 206 of the second switching valve 2 and the sixth interface 46 of the fourth switching valve 4. The design of the back-blowing flow avoids C4F7N enters the second detector 23 and shortens the analysis time. Wherein, in the detection process, in order to realize the flexibility of the back-blowing operation, the advantages areAnd a fourth inlet of the second switching valve 2 is selected as a blowback air inlet. The second quantitative tube 14 is arranged on the second switching valve 2, so that the dosage of the sample can be accurately controlled, and the dosage of the sample can be better saved.
The fifth carrier gas 12 is connected to a third port 43 of the fourth switching valve 4, the fourth purge valve 20 is connected to a first port 41 of the fourth switching valve 4, and the second detector 23 is connected to a fifth port 45 of the fourth switching valve 4; the second connection 42 of the fourth switching valve 4 is connected to a fourth connection 44 of the fourth switching valve 4. This flow design avoids CO2Into the second detector 23. The primary carrier gas 8, secondary carrier gas 9, tertiary carrier gas 10, fourth carrier gas 11 and fifth carrier gas 12 used in this application are 99.999% high purity helium gas.
It can be clearly seen from the above that, the gas chromatography detection system for detecting the gas component of perfluoroisobutyronitrile provided in this embodiment can realize the detection of C only by one instrument4F7N-CO2The accurate analysis of all components of the decomposition product of the mixed gas is beneficial to accurately judging the running condition of the electrical equipment; meanwhile, the labor force and the testing time are saved, the investment cost of the instrument is also reduced, the use cost is greatly reduced, and the maintenance cost of the instrument is correspondingly reduced; in addition, the sampling amount can be reduced by adopting one instrument for analysis, the use amount of the sample gas and the treatment amount of the used sample are reduced, and the device is safer and more environment-friendly.
The method comprises the following steps:
the method for analyzing the gas components of the perfluoroisobutyronitrile provided by the embodiment of the invention comprises the following steps:
step S1, the first switching valve adopts valve sample introduction mode to introduce sample through C of the first quantitative pipe4F7N-CO2After most of the fluorocarbon compounds in the mixed gas are separated by the third chromatographic column, the third switching valve 3 is switched to switch the separated fluorocarbon compounds to the first detector to respond to the peak. Most fluorocarbons herein include C3F8(octafluoropropane) C2HF5Cl（R125）、C2H3F3（R143a）、C2H2F4（R134a）、C3F6(Hexafluoropropylene) and C2F5CN。
The specific sample injection process in the step is as follows:
referring to fig. 2, the first switching valve 1 is switched, the first carrier gas 8 carries the gas sample to be detected in the first quantitative tube 13 to enter the third chromatographic column 7, and is simultaneously split through the tee joint and the first vent valve, so that the peak of the third chromatographic column is at C3F8The previous material is emptied through a second emptying valve. The peak is at C3F8The former substances are mainly CO2. When the first switching valve 1 is switched, the first carrier gas 8 is connected with the fifth interface 105 of the first switching valve, meanwhile, the fifth interface 105, the sixth interface 106, the first quantitative pipe 13, the third interface 103, the fourth interface 104, the tee joint 21, the third chromatographic column 7, the sixth interface 36 and the first interface 31 of the third switching valve 3 are sequentially connected, and the first interface 31 of the third switching valve is connected with one end of the second vent valve 18, so that components (mainly C) which do not need to be analyzed can be conveniently analyzed4F7N) is vented through a second vent valve.
Referring to fig. 3, the third switching valve 3 is switched such that C3F8And impurity components after the peak-off enter the first detector 22 respectively to peak off; wait for C2F5After CN finishes the peak, the third switching valve 3 is switched to return to the initial state, and for C4F7And N, emptying, so far as the analysis work of the first analysis unit is finished. Wherein:
when the third switching valve 3 is switched, the third chromatographic column 7, the sixth interface 36 of the third switching valve 3 and the inlet of the first detector 22 are connected in sequence, so that C3F8And the impurity components having the peak after it enter the first detector 22. The third switching valve 3 is switched back to the initial state, i.e. the sixth port 36 of the third switching valve 3 is connected to the first port 31, the first port 31 is connected to one end of the second blow valve 18, the third port 33 is connected to the second port 32, and the fourth port 34 is connected to the fifth port 35, so as to separate C from the third chromatographic column 74F7And (4) emptying the N. Thus, an analytical spectrum as shown in FIG. 6, in which about 50ppm of C is shown in FIG. 6, can be obtained3F8(octafluoropropane) C2HF5Cl（R125）、C2H3F3（R143a）、C2H2F4（R134a）、C3F6(Hexafluoropropylene) and C2F5And (3) a standard gas spectrum of CN.
Step S2, the second switch valve 2 is operated in a back-blowing sample injection mode and passes through the C of the second quantitative tube4F7N-CO2Pre-separating the mixed gas by a first chromatographic column to obtain Air, CO and CF4、CO2And C2F6The mixture enters a second chromatographic column, and then a second switching valve is switched to perform back flushing pre-separation to obtain other impurity components; switching a fourth switching valve to separate impurity components Air, CO and CF of the second chromatographic column4、CO2And C2F6Respectively switched to respond to peaks in the second detector.
The specific sample injection process in the step is as follows:
referring to fig. 4, the second switching valve 2 and the fourth switching valve 4 are switched, and a fourth carrier gas 11 carries the gas sample to be measured in the second quantitative tube 14 into the first chromatographic column 5, referring to fig. 5, when C is in the first chromatographic column 52F6And peak at C2F6The second switching valve 2 is switched after the former substance enters the second chromatographic column 6, so that the peak is at C2F6The subsequent substances are subjected to back flushing and emptying through a third emptying valve 19; meanwhile, the third carrier gas 10 carries the rest impurities separated from the second chromatographic column 6 into a second detector 23 to finish the peak discharge; referring to FIG. 1, when CF4After the peak discharge is finished, the fourth switching valve 4 is switched to enable CO to be generated2Venting via a fourth vent valve 20, see FIG. 5, when CO is being vented2After the air is completely emptied, the fourth switching valve 4 is switched to ensure that C is2F6And (4) peak generation. The components of the impurity gas analyzed in the second detector 23 are air, CO, CF4And C2F6。
Referring to fig. 4, when the second switching valve 2 is switched for the first time, the fourth carrier gas 11 is connected to the fourth port of the second switching valve 2, and enters the second quantitative tube 14 through the third port 203 of the second switching valve 2, and carries C in the second quantitative tube 144F7N-CO2The mixed gas enters the first chromatographic column 5 through the tenth interface 210 and the ninth interface 209 in sequence for separation, so that the peak is at C2F6The former substance enters the second chromatographic column 6 through the outlet of the first chromatographic column 5, the fifth interface 205 and the sixth interface 206 of the second switching valve 2.
Referring to fig. 5, when the second switching valve 2 is switched for the second time, after the fourth carrier gas 11 is connected to the fourth interface 204 of the second switching valve 2, the fourth carrier gas 11 carries a peak at C2F6The subsequent substances are sequentially discharged through a fifth port 205, the first chromatographic column 5, a ninth port 209, an eighth port 208, and a third discharge valve 19 connected to the eighth port 208. Meanwhile, the third carrier gas 10 is connected to the seventh port of the second switching valve 2, and at the same time, the fourth switching valve 4 is switched so that the outlet of the second chromatography column 6, the sixth port 46 of the fourth switching valve 4, the fifth port 45, and the second detector 23 are sequentially connected to carry the impurity components separated from the first chromatography column 5 into the second chromatography column 6 for separation, and then finally into the second detector 23.
Referring again to FIG. 1, to be CF4After the peak discharge is completed, the fourth switching valve 4 is switched, so that the sixth port of the fourth switching valve 4 is connected with the first port, and the first port is connected with one end of the fourth vent valve 20, so as to connect the CO2Is vented through a fourth vent valve 20. Referring to FIG. 5, wait for CO2After emptying, the fourth switching valve 4 is switched again such that the second chromatography column 6, the sixth interface and the fifth interface of the fourth switching valve 4 are connected with the second detector 23, so that C2F6Peak generation; finally, the fourth switching valve 4 is switched back to the state shown in FIG. 1, and the analysis is finished to obtain the analysis spectrum shown in FIG. 7, wherein FIG. 7 shows 160ppm of air and about 50ppm of CO and CF4And C2F6The standard gas spectrogram.
The steps S1 and S2 can be implemented simultaneouslyOne-time sample introduction is realized, switching valves in all analysis units are reasonably switched, the chromatographic analysis process is simplified, the interference among impurities is effectively avoided, the detection limit of each impurity component can reach 50ppb, and C is realized4F7N-CO2And (4) fully analyzing impurities in the mixed gas.
It can be seen that the invention can complete C by one-time sample injection4F7N-CO2Various impurities in the mixed gas are analyzed, instrument and human errors caused by multiple sample introduction are avoided, the analysis accuracy is improved, the analysis time is short, and related electrical equipment users can timely and accurately judge the running state of the electrical equipment according to the analysis result so as to timely take corresponding safety measures.
It will be apparent to those skilled in the art that various changes and modifications may be made in the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A gas chromatography detection system for determining the gas composition of perfluoroisobutyronitrile, comprising:
the first analysis unit comprises a first switching valve, a third chromatographic column, a third switching valve and a first detector which are sequentially connected; a first interface on the first switching valve is connected with a gas sample source to be detected; a second emptying valve is arranged on the third switching valve;
the second analysis unit comprises a second switching valve, a first chromatographic column, a second chromatographic column, a fourth switching valve and a second detector which are connected in sequence; a first interface on the second switching valve is connected with a gas sample source to be detected; a third emptying valve is arranged on the second switching valve; and a fourth emptying valve is arranged on the fourth switching valve.
2. The gas chromatography detection system for detecting a perfluoroisobutyronitrile gas component according to claim 1, wherein a first carrier gas is connected to the fifth port of the first switching valve; the gas sample inlet to be detected is connected with the first interface of the first switching valve; the second interface of the first switching valve is connected with the first interface of the second switching valve; a first quantitative pipe is arranged on a pipeline connecting the third interface of the first switching valve with the sixth interface of the first switching valve; and the fourth interface of the first switching valve is connected with the first end of the third chromatographic column.
3. The gas chromatography detection system for detecting a perfluoroisobutyronitrile gas component according to claim 1, wherein a fourth carrier gas is connected to a fourth port of the second switching valve, and a third carrier gas is connected to a seventh port of the second switching valve; the third vent valve is connected with an eighth interface of the second switching valve, and a gas sample outlet to be detected is connected with a second interface of the second switching valve; a second quantitative pipe is arranged on a pipeline connecting the third interface of the second switching valve and the tenth interface of the second switching valve; the first chromatographic column is arranged on a pipeline connecting the fifth interface of the second switching valve and the ninth interface of the second switching valve; and the second chromatographic column is arranged on a pipeline connecting the sixth interface of the second switching valve with the sixth interface of the fourth switching valve.
4. The gas chromatography detection system for detecting a perfluoroisobutyronitrile gas component according to claim 1, wherein a second carrier gas is connected to a third port of the third switching valve, the second purge valve is connected to a first port of the third switching valve, and the first detector is connected to a fifth port of the third switching valve; the other end of the third chromatographic column is connected with a sixth interface of the third switching valve; the second port of the third switching valve is connected with the fourth port of the third switching valve.
5. The gas chromatography detection system for detecting a perfluoroisobutyronitrile gas component according to claim 1, wherein the fifth carrier gas is connected to a third port of the fourth switching valve, the fourth purge valve is connected to a first port of the fourth switching valve, and the second detector is connected to a fifth port of the fourth switching valve; the second port of the fourth switching valve is connected with the fourth port of the fourth switching valve.
6. The gas chromatography detection system for detecting the gas composition of perfluoroisobutyronitrile according to claim 1, wherein the first detector and the second detector are both pulsed helium ionization detectors.
7. The gas chromatography detection system for detecting a perfluoroisobutyronitrile gas component according to claim 1, wherein the first switching valve, the third switching valve, and the fourth switching valve are six-way purge pneumatic switching valves, and the second switching valve is a ten-way purge pneumatic switching valve.
8. The gas chromatography detection system for detecting a perfluoroisobutyronitrile gas component according to claim 1, wherein the first chromatography column is C4F7N special analysis pre-column; the second chromatographic column is C4F7And N, a special analysis column, wherein the third chromatographic column is a fluorocarbon analysis capillary column.
9. A method for analyzing a perfluoroisobutyronitrile gas component using the gas chromatography detection system according to any one of claims 1 to 8, comprising the steps of:
step (1), the first switching valve adopts a valve sample introduction mode to introduce samples through a C of a first quantitative pipe4F7N-CO2After most of fluorocarbon compounds in the mixed gas are separated by a third chromatographic column, switching a third switching valve to switch the separated fluorocarbon compounds to a first detector to respond to a peak;
step (2), the second switching valve is carried out in a back-flushing sample injection mode and passes through the C of the second quantitative pipe4F7N-CO2Mixed gas, first introducedThe first chromatographic column realizes the pre-separation of the gas sample to be measured, so that Air, CO and CF are enabled to be obtained4、CO2And C2F6The mixture enters a second chromatographic column, and then a second switching valve is switched to perform back flushing pre-separation to obtain other impurity components; switching a fourth switching valve to separate impurity components Air, CO and CF of the second chromatographic column4、CO2And C2F6Respectively switched to respond to peaks in the second detector.
10. The method of analyzing perfluoroisobutyronitrile gas composition according to claim 9, wherein the feeding step is as follows:
switching the first switching valve, enabling the first carrier gas to carry the gas sample to be detected in the first quantitative tube to enter the third chromatographic column, simultaneously shunting through a tee joint and a first emptying valve, and enabling the third chromatographic column to have a peak at C3F8The previous material is emptied through a second emptying valve; switching the third switching valve so that C3F8And then the impurity components enter a first detector respectively to generate peaks; wait for C2F5After CN finishes the peak, the third switching valve is switched to return to the initial state, and for C4F7N, emptying;
switching the second switching valve and the fourth switching valve, wherein a fourth carrier gas carries the gas sample to be detected in the second quantitative tube to enter the first chromatographic column, and when C in the first chromatographic column2F6And peak at C2F6The former substance enters the second chromatographic column and then the second switching valve is switched to lead the peak to be C2F6The subsequent substances are subjected to back blowing and emptying through a third emptying valve; simultaneously, the third carrier gas carries impurities separated from the second chromatographic column to enter a second detector to finish peak formation until CF4After the peak is generated, the fourth switching valve is switched to empty through the fourth emptying valve, and when CO is discharged2After the air is completely emptied, the fourth switching valve is switched to return to the initial state, so that the air pressure of the air compressor C is controlled to be in the initial state2F6And (4) peak generation.
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