CN114019040A - System for detecting gas impurities in sulfur hexafluoride - Google Patents
System for detecting gas impurities in sulfur hexafluoride Download PDFInfo
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- CN114019040A CN114019040A CN202111200474.7A CN202111200474A CN114019040A CN 114019040 A CN114019040 A CN 114019040A CN 202111200474 A CN202111200474 A CN 202111200474A CN 114019040 A CN114019040 A CN 114019040A
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- way valve
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- SFZCNBIFKDRMGX-UHFFFAOYSA-N sulfur hexafluoride Chemical compound FS(F)(F)(F)(F)F SFZCNBIFKDRMGX-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229960000909 sulfur hexafluoride Drugs 0.000 title claims abstract description 63
- 229910018503 SF6 Inorganic materials 0.000 title claims abstract description 60
- 239000012535 impurity Substances 0.000 title claims abstract description 48
- 239000007789 gas Substances 0.000 claims abstract description 90
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 44
- 238000001514 detection method Methods 0.000 claims abstract description 43
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 42
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 34
- QYSGYZVSCZSLHT-UHFFFAOYSA-N octafluoropropane Chemical compound FC(F)(F)C(F)(F)C(F)(F)F QYSGYZVSCZSLHT-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229960004065 perflutren Drugs 0.000 claims abstract description 27
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910002091 carbon monoxide Inorganic materials 0.000 claims abstract description 22
- WMIYKQLTONQJES-UHFFFAOYSA-N hexafluoroethane Chemical compound FC(F)(F)C(F)(F)F WMIYKQLTONQJES-UHFFFAOYSA-N 0.000 claims abstract description 22
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 claims abstract description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000001257 hydrogen Substances 0.000 claims abstract description 20
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 20
- 239000001301 oxygen Substances 0.000 claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 20
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 17
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 230000008569 process Effects 0.000 claims abstract description 16
- 125000004435 hydrogen atom Chemical class [H]* 0.000 claims abstract 5
- 238000000926 separation method Methods 0.000 claims description 30
- 238000002161 passivation Methods 0.000 claims description 10
- 230000006012 detection of carbon dioxide Effects 0.000 claims description 5
- 238000011010 flushing procedure Methods 0.000 claims description 5
- 239000002808 molecular sieve Substances 0.000 claims description 5
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims 1
- 238000004458 analytical method Methods 0.000 abstract description 13
- 230000035945 sensitivity Effects 0.000 abstract description 7
- 150000002431 hydrogen Chemical class 0.000 description 14
- 238000011002 quantification Methods 0.000 description 8
- 239000001307 helium Substances 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 3
- 238000004454 trace mineral analysis Methods 0.000 description 3
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000010891 electric arc Methods 0.000 description 1
- 238000010892 electric spark Methods 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- -1 helium ion Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000126 substance Substances 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
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
-
- 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
- G01N30/60—Construction of the column
- G01N30/6052—Construction of the column body
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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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
- G01N2030/201—Injection using a sampling valve multiport valves, i.e. having more than two ports
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- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The system for detecting the gas impurities in the sulfur hexafluoride selects the enhanced plasma detector 27 and the enhanced plasma detector 28 to detect the gas impurities in the sulfur hexafluoride, the carbon dioxide, the hexafluoroethane and the octafluoropropane detected by the enhanced plasma detector 27 are well separated, the selected analysis flow and analysis conditions are designed to effectively separate the carbon dioxide, the hexafluoroethane and the octafluoropropane which are impurity components, and the detected target objects are not interfered with each other; the total six gases of hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride detected by the enhanced plasma detector 28 are well separated, and the selected analysis process and analysis conditions are designed to effectively separate the impurity components of hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride without mutual interference; the system has the advantages of high sensitivity, low detection limit, wide detection concentration range and the like.
Description
Technical Field
The invention belongs to the technical field of sulfur hexafluoride component impurity content detection, and particularly relates to a system for detecting gas impurities in sulfur hexafluoride.
Background
The sulfur hexafluoride has good insulating and arc extinguishing performance and is widely applied to various high-voltage electrical equipment. However, sulfur hexafluoride is decomposed under the action of corona discharge, electric arc, electric spark and the like during use, the type and content of the decomposition products are closely related to the type of equipment faults, and the influence is caused on the safe operation of electrical equipment, so that the content of gas impurities in the sulfur hexafluoride needs to be accurately detected to judge the operation condition of the sulfur hexafluoride equipment.
At present, gas chromatography is mainly adopted in laboratories for detection, most of the adopted detectors are hydrogen flame ion detectors, thermal conductivity detectors and flame photometric detectors, but the above detectors have low sensitivity, and the detection of trace concentration ranges cannot be guaranteed. The gas chromatograph provided with the helium ion detector can meet the requirement of trace analysis, but the peak shift of high-concentration substances can be caused by the factors such as the column efficiency reduction of the chromatographic column, the interference of impurities and the like in the use process. If a high-concentration sample enters the detector, the detector cannot be recovered to be normal in a short time, and electrode carbon deposition is caused for a long time, so that the sensitivity of the detector is reduced. Therefore, a detection system with high sensitivity and wide detection concentration is needed to meet the detection requirement.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a system for detecting gas impurities in sulfur hexafluoride, which is simple and convenient to operate, short in analysis time and suitable for rapid field detection.
In order to achieve the purpose, the invention provides the following technical scheme: a system for detecting gaseous impurities in sulfur hexafluoride, comprising; a quantification ring 21, a quantification ring 22, a chromatographic column 23, a chromatographic column 24, a chromatographic column 25, a chromatographic column 26, an enhanced plasma detector 27, an enhanced plasma detector 28, a six-way valve 11, a four-way valve 12, and a ten-way valve 13;
the quantitative ring 21 is connected to the six-way valve 11 through a gas path, and the quantitative ring 22 is connected to the ten-way valve 13 through a gas path;
the chromatographic column 23 is connected with the six-way valve 11 and the four-way valve 12 through gas circuits;
the chromatographic column 24 is connected with the four-way valve 12 and an enhanced plasma detector 27 through a gas circuit;
the chromatographic column 25 is connected with the ten-way valve 13 through a gas circuit;
the chromatographic column 26 is connected to the ten-way valve 13 and the enhanced plasma detector 28 through gas paths.
Further, the quantitative ring 21 is a quantitative ring with a volume of 0.5mL treated by a passivation process.
Further, the quantitative ring 22 is a quantitative ring with a volume of 0.5mL treated by a passivation process.
Further, the chromatographic column 23 adopts a PorapakR packed column, and has the following dimensions: the length is 4m and the inner diameter is 2 mm.
Further, the chromatographic column 24 adopts a PorapakQ packed column, and has the following dimensions: the length is 4m and the inner diameter is 2 mm.
Further, the chromatographic column 25 adopts a PorapakR packed column, and has the following dimensions: the length is 4m and the inner diameter is 2 mm.
Further, the chromatographic column 26 adopts a 13X molecular sieve packed column, and has the size: the length is 4m and the inner diameter is 2 mm.
Further, the enhanced plasma detector 27 and the enhanced plasma detector 28 are all four-channel wavelength enhanced plasma detectors.
Further, the detection steps of the system for detecting the gas impurities in the sulfur hexafluoride are as follows:
after a system for detecting gas impurities in sulfur hexafluoride is started, the six-way valve 11, the four-way valve 12 and the ten-way valve 13 are in a closed state, sample gas is respectively filled into the quantitative ring 21 and the quantitative ring 22, then the six-way valve 11 and the four-way valve 12 respectively execute an opening instruction, and gas of the quantitative ring 21 enters a chromatographic column 23 for pre-separation and is separated into a component A containing hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride and a component B containing carbon dioxide, hexafluoroethane, sulfur hexafluoride and octafluoropropane; switching the four-way valve 12 before the component A reaches the four-way valve 12, accurately emptying the component A through an emptying port A when the four-way valve 12 is in an open state, closing the four-way valve 12 after emptying the component A, enabling the component B to enter a chromatographic column 24 for separation, enabling the component B to enter an enhanced plasma detector 27 for detection after separation, then opening the four-way valve 12, emptying sulfur hexafluoride through an emptying outlet A, closing the four-way valve 12, enabling octafluoropropane to enter the enhanced plasma detector 27 through the chromatographic column 24 for detection, and completing detection of carbon dioxide, hexafluoroethane and octafluoropropane;
the gas of the quantitative ring 22 enters a chromatographic column 25 for pre-separation and is separated into a component C containing hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride and a component D containing carbon dioxide, hexafluoroethane, sulfur hexafluoride and octafluoropropane; and after the component C flows out, the ten-way valve 13 is closed, the following component D is subjected to back flushing and is discharged through the evacuation port B, the component C continuously enters the chromatographic column 26 for separation, and the component after secondary separation enters the enhanced plasma detector 28 for detection, so that the detection of hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride can be completed.
The system for detecting the gas impurities in the sulfur hexafluoride selects the enhanced plasma detector 27 and the enhanced plasma detector 28 to detect the gas impurities in the sulfur hexafluoride, has the advantages of high sensitivity, low detection limit, wide detection concentration range and the like, is suitable for trace analysis of gas, and can meet the content detection requirement of the gas impurities in the sulfur hexafluoride for electrical equipment.
The invention relates to a system for detecting gas impurities in sulfur hexafluoride, which selects an enhanced plasma detector 27 and an enhanced plasma detector 28 to detect the gas impurities in the sulfur hexafluoride, wherein the carbon dioxide, hexafluoroethane and octafluoropropane detected by the enhanced plasma detector 27 are well separated, and different signals are provided on four channels, wherein the signals comprise the positive and negative of peaks and the size of the peaks, so that the selected analysis process and analysis conditions are designed to effectively separate the impurity components of carbon dioxide, hexafluoroethane and octafluoropropane, the discharge of sulfur hexafluoride does not cause interference to the detection, the detection target objects do not interfere with each other to detect an actual sample, and the analysis period is about 13 min; the total six gases of hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride detected by the enhanced plasma detector 28 are well separated, and different signals are provided on four channels, the signals are different and comprise the positive and negative of peaks and the size of peaks, so that the selected analysis process and analysis conditions are designed, the impurity components of hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride can be effectively separated, no interference exists among the signals, an actual sample can be detected, and the analysis period is about 9 min; the system has the advantages of high sensitivity, low detection limit, wide detection concentration range and the like.
Drawings
FIG. 1 is a schematic diagram of an initial state gas path structure of a system analysis process valve for detecting gas impurities in sulfur hexafluoride, according to the present invention.
FIG. 2 is a schematic diagram of a gas circuit structure of a system analysis process valve in a back-blowing switching state for detecting gas impurities in sulfur hexafluoride, according to the present invention.
Fig. 3 is a four-channel spectrum of the enhanced plasma detector 27 in the system embodiment 1 for detecting gas impurities in sulfur hexafluoride according to the present invention.
Fig. 4 is a four-channel spectrum of the enhanced plasma detector 28 in embodiment 1 of the system for detecting gas impurities in sulfur hexafluoride in accordance with the present invention.
Detailed Description
The following examples may help one skilled in the art to more fully understand the present invention, but are not intended to limit the invention in any way.
Example 1
A system for detecting gaseous impurities in sulfur hexafluoride, comprising; a quantification ring 21, a quantification ring 22, a chromatographic column 23, a chromatographic column 24, a chromatographic column 25, a chromatographic column 26, an enhanced plasma detector 27, an enhanced plasma detector 28, a six-way valve 11, a four-way valve 12, and a ten-way valve 13;
the quantitative ring 21 is connected to the six-way valve 11 through a gas path, and the quantitative ring 22 is connected to the ten-way valve 13 through a gas path; the quantitative ring 21 is a quantitative ring with the volume of 0.5mL treated by a passivation process, and the quantitative ring 22 is a quantitative ring with the volume of 0.5mL treated by a passivation process;
the chromatographic column 23 is connected with the six-way valve 11 and the four-way valve 12 through gas circuits; the chromatographic column 23 adopts a PorapakR packed column, and has the following dimensions: the length is 4m, and the inner diameter is 2 mm;
the chromatographic column 24 is connected with the four-way valve 12 and an enhanced plasma detector 27 through a gas circuit; the chromatographic column 24 adopts a PorapakQ packed column, and has the following dimensions: the length is 4m, and the inner diameter is 2 mm; the enhanced plasma detector 27 is a four-channel wavelength enhanced plasma detector;
the chromatographic column 25 is connected with the ten-way valve 13 through a gas circuit; the chromatographic column 25 adopts a PorapakR packed column, and has the following dimensions: the length is 4m, and the inner diameter is 2 mm;
the chromatographic column 26 is connected with the ten-way valve 13 and the enhanced plasma detector 28 through gas circuits; the chromatographic column 26 adopts a 13X molecular sieve packed column, and has the following dimensions: the length is 4m, and the inner diameter is 2 mm; the enhanced plasma detector 28 is a four channel wavelength enhanced plasma detector.
The detection steps of the system for detecting the gas impurities in the sulfur hexafluoride are as follows:
after a system for detecting gas impurities in sulfur hexafluoride is started, the six-way valve 11, the four-way valve 12 and the ten-way valve 13 are in a closed state, sample gas is respectively filled into the quantitative ring 21 and the quantitative ring 22, then the six-way valve 11 and the four-way valve 12 respectively execute an opening instruction, and gas of the quantitative ring 21 enters a chromatographic column 23 for pre-separation and is separated into a component A containing hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride and a component B containing carbon dioxide, hexafluoroethane, sulfur hexafluoride and octafluoropropane; switching the four-way valve 12 before the component A reaches the four-way valve 12, accurately emptying the component A through an emptying port A when the four-way valve 12 is in an open state, closing the four-way valve 12 after emptying the component A, enabling the component B to enter a chromatographic column 24 for separation, enabling the component B to enter an enhanced plasma detector 27 for detection after separation, then opening the four-way valve 12, emptying sulfur hexafluoride through an emptying outlet A, closing the four-way valve 12, enabling octafluoropropane to enter the enhanced plasma detector 27 through the chromatographic column 24 for detection, and completing detection of carbon dioxide, hexafluoroethane and octafluoropropane;
the gas of the quantitative ring 22 enters a chromatographic column 25 for pre-separation and is separated into a component C containing hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride and a component D containing carbon dioxide, hexafluoroethane, sulfur hexafluoride and octafluoropropane; and after the component C flows out, the ten-way valve 13 is closed, the following component D is subjected to back flushing and is discharged through the evacuation port B, the component C continuously enters the chromatographic column 26 for separation, and the component after secondary separation enters the enhanced plasma detector 28 for detection, so that the detection of hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride can be completed.
In the embodiment, the sample gas filled into the quantitative rings 21 and 22 is obtained by sampling in the power equipment to be tested; the four channel spectra of the enhanced plasma detector 27 are shown in fig. 3, and the four channel spectra of the enhanced plasma detector 28 are shown in fig. 4.
Example 2
A system for detecting gaseous impurities in sulfur hexafluoride, comprising; a quantification ring 21, a quantification ring 22, a chromatographic column 23, a chromatographic column 24, a chromatographic column 25, a chromatographic column 26, an enhanced plasma detector 27, an enhanced plasma detector 28, a six-way valve 11, a four-way valve 12, and a ten-way valve 13;
the quantitative ring 21 is connected to the six-way valve 11 through a gas path, and the quantitative ring 22 is connected to the ten-way valve 13 through a gas path; the quantitative ring 21 is a quantitative ring with the volume of 0.5mL treated by a passivation process, and the quantitative ring 22 is a quantitative ring with the volume of 0.5mL treated by a passivation process;
the chromatographic column 23 is connected with the six-way valve 11 and the four-way valve 12 through gas circuits; the chromatographic column 23 adopts a PorapakR packed column, and has the following dimensions: the length is 4m, and the inner diameter is 2 mm;
the chromatographic column 24 is connected with the four-way valve 12 and an enhanced plasma detector 27 through a gas circuit; the chromatographic column 24 adopts a PorapakQ packed column, and has the following dimensions: the length is 4m, and the inner diameter is 2 mm; the enhanced plasma detector 27 is a four-channel wavelength enhanced plasma detector;
the chromatographic column 25 is connected with the ten-way valve 13 through a gas circuit; the chromatographic column 25 adopts a PorapakR packed column, and has the following dimensions: the length is 4m, and the inner diameter is 2 mm;
the chromatographic column 26 is connected with the ten-way valve 13 and the enhanced plasma detector 28 through gas circuits; the chromatographic column 26 adopts a 13X molecular sieve packed column, and has the following dimensions: the length is 4m, and the inner diameter is 2 mm; the enhanced plasma detector 28 is a four channel wavelength enhanced plasma detector.
The detection steps of the system for detecting the gas impurities in the sulfur hexafluoride are as follows:
after a system for detecting gas impurities in sulfur hexafluoride is started, the six-way valve 11, the four-way valve 12 and the ten-way valve 13 are in a closed state, sample gas is respectively filled into the quantitative ring 21 and the quantitative ring 22, then the six-way valve 11 and the four-way valve 12 respectively execute an opening instruction, and gas of the quantitative ring 21 enters a chromatographic column 23 for pre-separation and is separated into a component A containing hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride and a component B containing carbon dioxide, hexafluoroethane, sulfur hexafluoride and octafluoropropane; switching the four-way valve 12 before the component A reaches the four-way valve 12, accurately emptying the component A through an emptying port A when the four-way valve 12 is in an open state, closing the four-way valve 12 after emptying the component A, enabling the component B to enter a chromatographic column 24 for separation, enabling the component B to enter an enhanced plasma detector 27 for detection after separation, then opening the four-way valve 12, emptying sulfur hexafluoride through an emptying outlet A, closing the four-way valve 12, enabling octafluoropropane to enter the enhanced plasma detector 27 through the chromatographic column 24 for detection, and completing detection of carbon dioxide, hexafluoroethane and octafluoropropane;
the gas of the quantitative ring 22 enters a chromatographic column 25 for pre-separation and is separated into a component C containing hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride and a component D containing carbon dioxide, hexafluoroethane, sulfur hexafluoride and octafluoropropane; and after the component C flows out, the ten-way valve 13 is closed, the following component D is subjected to back flushing and is discharged through the evacuation port B, the component C continuously enters the chromatographic column 26 for separation, and the component after secondary separation enters the enhanced plasma detector 28 for detection, so that the detection of hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride can be completed.
The specific parameters of the sample gas filled into the quantitative rings 21 and 22 in this embodiment are as follows: 101.22 μmol/mol, oxygen: 99.26. mu. mol/mol, nitrogen: 101.45 μmol/mol, methane: 97.37. mu. mol/mol, carbon monoxide: 99.28. mu. mol/mol, carbon dioxide: 102.56 μmol/mol, carbon tetrafluoride: 98.48. mu. mol/mol, hexafluoroethane: 104.54 μmol/mol, sulfur hexafluoride: 520.61 μmol/mol, octafluoropropane: 99.90 mu mol/mol, helium is used as equilibrium gas; wherein, the helium gas is high-purity helium gas (99.999%).
The measurement results of the peak area corresponding to the standard gas concentration are shown in the following table 1:
TABLE 1
| Serial number | 1 | 2 | 3 | 4 | 5 | 6 | RSD（%） |
| Hydrogen gas | 5007276 | 5031318 | 5097574 | 4965926 | 4841271 | 4981152 | 1.70 |
| Oxygen gas | 1710636 | 1655314 | 1662726 | 1746016 | 1646158 | 1677788 | 2.26 |
| Nitrogen gas | 14725555 | 14784669 | 14640230 | 14792588 | 14602956 | 14765334 | 0.54 |
| Methane | 20972259 | 20800154 | 20360923 | 20513887 | 20859777 | 20829612 | 1.12 |
| Carbon monoxide | 3277611 | 3279405 | 3393890 | 3364155 | 3234759 | 3291781 | 1.80 |
| Carbon tetrafluoride | 1542200 | 1461832 | 1528317 | 1495746 | 1554220 | 1538389 | 2.28 |
| Carbon dioxide | 50629042 | 50147506 | 50163487 | 50911951 | 52613014 | 51139581 | 1.79 |
| Hexafluoroethane | 74035257 | 74542999 | 74291654 | 75300247 | 74477777 | 74659721 | 0.57 |
| Octafluoropropane | 40500608 | 40144993 | 40061547 | 40695103 | 40930749 | 40765332 | 0.86 |
The gas sample to be tested is repeatedly tested for 6 times, the relative standard deviation of the concentration test result of each component is less than 3 percent, and the experimental result is qualified.
Example 3
A system for detecting gaseous impurities in sulfur hexafluoride, comprising; a quantification ring 21, a quantification ring 22, a chromatographic column 23, a chromatographic column 24, a chromatographic column 25, a chromatographic column 26, an enhanced plasma detector 27, an enhanced plasma detector 28, a six-way valve 11, a four-way valve 12, and a ten-way valve 13;
the quantitative ring 21 is connected to the six-way valve 11 through a gas path, and the quantitative ring 22 is connected to the ten-way valve 13 through a gas path; the quantitative ring 21 is a quantitative ring with the volume of 0.5mL treated by a passivation process, and the quantitative ring 22 is a quantitative ring with the volume of 0.5mL treated by a passivation process;
the chromatographic column 23 is connected with the six-way valve 11 and the four-way valve 12 through gas circuits; the chromatographic column 23 adopts a PorapakR packed column, and has the following dimensions: the length is 4m, and the inner diameter is 2 mm;
the chromatographic column 24 is connected with the four-way valve 12 and an enhanced plasma detector 27 through a gas circuit; the chromatographic column 24 adopts a PorapakQ packed column, and has the following dimensions: the length is 4m, and the inner diameter is 2 mm; the enhanced plasma detector 27 is a four-channel wavelength enhanced plasma detector;
the chromatographic column 25 is connected with the ten-way valve 13 through a gas circuit; the chromatographic column 25 adopts a PorapakR packed column, and has the following dimensions: the length is 4m, and the inner diameter is 2 mm;
the chromatographic column 26 is connected with the ten-way valve 13 and the enhanced plasma detector 28 through gas circuits; the chromatographic column 26 adopts a 13X molecular sieve packed column, and has the following dimensions: the length is 4m, and the inner diameter is 2 mm; the enhanced plasma detector 28 is a four channel wavelength enhanced plasma detector.
The detection steps of the system for detecting the gas impurities in the sulfur hexafluoride are as follows:
after a system for detecting gas impurities in sulfur hexafluoride is started, the six-way valve 11, the four-way valve 12 and the ten-way valve 13 are in a closed state, sample gas is respectively filled into the quantitative ring 21 and the quantitative ring 22, then the six-way valve 11 and the four-way valve 12 respectively execute an opening instruction, and gas of the quantitative ring 21 enters a chromatographic column 23 for pre-separation and is separated into a component A containing hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride and a component B containing carbon dioxide, hexafluoroethane, sulfur hexafluoride and octafluoropropane; switching the four-way valve 12 before the component A reaches the four-way valve 12, accurately emptying the component A through an emptying port A when the four-way valve 12 is in an open state, closing the four-way valve 12 after emptying the component A, enabling the component B to enter a chromatographic column 24 for separation, enabling the component B to enter an enhanced plasma detector 27 for detection after separation, then opening the four-way valve 12, emptying sulfur hexafluoride through an emptying outlet A, closing the four-way valve 12, enabling octafluoropropane to enter the enhanced plasma detector 27 through the chromatographic column 24 for detection, and completing detection of carbon dioxide, hexafluoroethane and octafluoropropane;
the gas of the quantitative ring 22 enters a chromatographic column 25 for pre-separation and is separated into a component C containing hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride and a component D containing carbon dioxide, hexafluoroethane, sulfur hexafluoride and octafluoropropane; and after the component C flows out, the ten-way valve 13 is closed, the following component D is subjected to back flushing and is discharged through the evacuation port B, the component C continuously enters the chromatographic column 26 for separation, and the component after secondary separation enters the enhanced plasma detector 28 for detection, so that the detection of hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride can be completed.
In the embodiment, the sample gas filled into the quantitative rings 21 and 22 is obtained by sampling in the power equipment to be tested;
the peak area measurement results for the standard gas concentrations are shown in table 2 below:
TABLE 2
| Serial number | 1 | 2 | 3 | 4 | 5 | 6 | RSD（%） |
| Hydrogen gas | 7235568 | 7355219 | 7440845 | 7261237 | 7194552 | 7235789 | 1.27 |
| Oxygen gas | 3492789 | 3525511 | 3519472 | 3520231 | 3481273 | 3569045 | 0.87 |
| Nitrogen gas | 26167901 | 26913097 | 25689023 | 25828903 | 25309456 | 25526891 | 2.21 |
| Methane | 58987345 | 58679012 | 58708912 | 57308901 | 58200127 | 59008014 | 1.10 |
| Carbon monoxide | 7499172 | 7382890 | 7670934 | 7443031 | 7409235 | 7507530 | 1.38 |
| Carbon tetrafluoride | 3796713 | 3855591 | 3800925 | 3841790 | 3875129 | 3897215 | 1.04 |
| Carbon dioxide | 89156901 | 89460921 | 89995612 | 89360931 | 87468267 | 88064671 | 1.07 |
| Hexafluoroethane | 97230914 | 95539012 | 97032809 | 98933093 | 97130128 | 97536210 | 1.12 |
| Octafluoropropane | 63509012 | 63105097 | 64307128 | 63205190 | 63009037 | 62109021 | 1.13 |
The gas sample to be tested is repeatedly tested for 6 times, the relative standard deviation of the concentration test result of each component is less than 3 percent, and the experimental result is qualified.
The embodiment shows that the system for detecting the gas impurities in the sulfur hexafluoride selects the enhanced plasma detector 27 and the enhanced plasma detector 28 to detect the gas impurities in the sulfur hexafluoride, and the enhanced plasma detector has the advantages of high sensitivity, low detection limit, wide detection concentration range and the like, is suitable for trace analysis of gas, and can meet the content detection requirement of the gas impurities in the sulfur hexafluoride for electrical equipment.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (9)
1. A system for detecting gas impurities in sulfur hexafluoride is characterized by comprising; a quantitative ring (21), a quantitative ring (22), a chromatographic column (23), a chromatographic column (24), a chromatographic column (25), a chromatographic column (26), an enhanced plasma detector (27), an enhanced plasma detector (28), a six-way valve (11), a four-way valve (12) and a ten-way valve (13);
the quantitative ring (21) is connected to the six-way valve (11) through a gas circuit, and the quantitative ring (22) is connected to the ten-way valve (13) through a gas circuit;
the chromatographic column (23) is connected with the six-way valve (11) and the four-way valve (12) through gas circuits;
the chromatographic column (24) is connected with the four-way valve (12) and the enhanced plasma detector (27) through a gas circuit;
the chromatographic column (25) is connected with the ten-way valve (13) through a gas circuit;
the chromatographic column (26) is connected with the ten-way valve (13) and the enhanced plasma detector (28) through gas circuits.
2. The system for detecting gaseous impurities in sulfur hexafluoride as recited in claim 1, wherein said quantitative ring (21) is a passivation process treated quantitative ring having a volume of 0.5 mL.
3. The system for detecting gaseous impurities in sulfur hexafluoride as recited in claim 1, wherein said quantitative ring (22) is a passivation process treated quantitative ring having a volume of 0.5 mL.
4. A system for detecting gaseous impurities in sulphur hexafluoride as claimed in claim 1, characterised in that said chromatographic column (23) is a PorapakR packed column of dimensions: the length is 4m and the inner diameter is 2 mm.
5. A system for detecting gaseous impurities in sulphur hexafluoride as claimed in claim 1, wherein said chromatographic column (24) is a PorapakQ packed column of dimensions: the length is 4m and the inner diameter is 2 mm.
6. A system for detecting gaseous impurities in sulphur hexafluoride as claimed in claim 1, characterised in that said chromatographic column (25) is a PorapakR packed column of dimensions: the length is 4m and the inner diameter is 2 mm.
7. The system for detecting gaseous impurities in sulfur hexafluoride according to claim 1, wherein the chromatographic column (26) is a 13X molecular sieve packed column having the dimensions: the length is 4m and the inner diameter is 2 mm.
8. The system for detecting gaseous impurities in sulfur hexafluoride as recited in claim 1, wherein said enhanced plasma detector (27) and said enhanced plasma detector (28) are four-channel wavelength enhanced plasma detectors.
9. The system for detecting gaseous impurities in sulfur hexafluoride of claim 1, wherein said system for detecting gaseous impurities in sulfur hexafluoride includes the steps of:
after a system for detecting gas impurities in sulfur hexafluoride is started, a six-way valve (11), a four-way valve (12) and a ten-way valve (13) are in a closed state, sample gas is respectively filled into a quantitative ring (21) and a quantitative ring (22), then the six-way valve (11) and the four-way valve (12) respectively execute an opening instruction, and gas of the quantitative ring (21) enters a chromatographic column (23) for pre-separation to be separated into a component A containing hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride and a component B containing carbon dioxide, hexafluoroethane, sulfur hexafluoride and octafluoropropane; switching a four-way valve (12) before the component A reaches the four-way valve (12), accurately emptying the component A through an emptying port A when the four-way valve (12) is in an open state, closing the four-way valve (12) after emptying the component A, enabling the component B to enter a chromatographic column (24) for separation, enabling the component B to enter an enhanced plasma detector (27) for detection after separation, then opening the four-way valve (12), emptying sulfur hexafluoride through an emptying outlet A, closing the four-way valve (12), enabling octafluoropropane to enter the enhanced plasma detector (27) through the chromatographic column (24) for detection, and completing detection of carbon dioxide, hexafluoroethane and octafluoropropane;
the gas of the quantitative ring (22) enters a chromatographic column (25) for pre-separation and is separated into a component C containing hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride and a component D containing carbon dioxide, hexafluoroethane, sulfur hexafluoride and octafluoropropane; and after the component C flows out, closing the ten-way valve (13), carrying out back flushing on the component D, discharging the component D through the evacuation port B, continuously introducing the component C into the chromatographic column (26) for separation, introducing the component subjected to secondary separation into the enhanced plasma detector (28) for detection, and thus completing detection of hydrogen, oxygen, nitrogen, methane, carbon monoxide and carbon tetrafluoride.
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