CN109085280B - System for quantitatively detecting sulfur hexafluoride gas component - Google Patents

System for quantitatively detecting sulfur hexafluoride gas component Download PDF

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Publication number
CN109085280B
CN109085280B CN201811203626.7A CN201811203626A CN109085280B CN 109085280 B CN109085280 B CN 109085280B CN 201811203626 A CN201811203626 A CN 201811203626A CN 109085280 B CN109085280 B CN 109085280B
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way valve
port
valve
sulfur
packing column
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CN109085280A (en
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唐念
李丽
樊小鹏
周永言
黄国君
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Guangdong Power Grid Co Ltd
Electric Power Research Institute of Guangdong Power Grid Co Ltd
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Guangdong Power Grid Co Ltd
Electric Power Research Institute of Guangdong Power Grid Co Ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/16Injection
    • G01N30/20Injection using a sampling valve
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/62Detectors specially adapted therefor
    • G01N30/64Electrical detectors

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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)
  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The application discloses a system for quantitatively detecting sulfur hexafluoride gas component, including: the device comprises a first six-way valve, a second six-way valve, a third six-way valve, a PDD detector, a first micro needle valve, a second micro needle valve, a sulfur chromatography packed column, a carbon chromatography packed column and a quantitative ring. The system provided by the application can realize H in the gas sample to be detected 2 、C 3 F 8 、COS、SO 2 F 2 、H 2 S、CS 2 、N 2 、O 2 、CO、SO 2 、CH 4 、CF 4 The sulfur hexafluoride gas component detection system has the advantages of multiple detectable components, simple instrument structure, low price and convenience in market promotion, and solves the technical problems of the existing sulfur hexafluoride gas component detection system which is lack of multiple detectable components, simple structure, low cost and benefit for large-area popularization and application.

Description

System for quantitatively detecting sulfur hexafluoride gas component
Technical Field
The application relates to the technical field of gas detection, in particular to a system for quantitatively detecting sulfur hexafluoride gas components.
Background
Sulfur hexafluoride gas has excellent insulation and arc extinguishing performance, and is widely applied to electrical equipment, and typical application of sulfur hexafluoride gas is gas insulation in high-voltage switch cabinets of power transmission and transformation stations, power plants and the like in power supply departments. When the electrical equipment has defects or fails, sulfur hexafluoride gas can react to generate decomposition products, and detection of the sulfur hexafluoride decomposition products is an important means for diagnosing the insulation state inside the electrical equipment and improving the safe operation level of the equipment.
At present, the method for detecting sulfur hexafluoride gas components comprises the following steps: electrochemical sensor method, gas chromatography, and gas chromatography. The electrochemical sensor method is simple and convenient to use, but few detectable components exist, and serious mutual interference exists among the components; the gas chromatography-mass spectrometry has the advantages of multiple detectable components and high sensitivity, but the system is complex, the instrument is expensive, and the large-area popularization and application are not facilitated; the gas chromatography has a plurality of detectable components, but the system used by the prior art has complex structure and high cost, and is also not beneficial to large-area popularization and application. Therefore, the sulfur hexafluoride gas component detection system which has the advantages of multiple detectable components, simple structure and low cost and is favorable for large-area popularization and application is a technical problem to be solved by the technicians in the field.
Disclosure of Invention
The application provides a system for quantitatively detecting sulfur hexafluoride gas components, which is used for solving the technical problems of the existing sulfur hexafluoride gas component detection system which is lack of a plurality of detectable components, simple in structure, low in cost and beneficial to large-area popularization and application.
The application provides a system for quantitatively detecting sulfur hexafluoride gas components, which comprises: the device comprises a first six-way valve, a second six-way valve, a third six-way valve, a PDD detector, a first micro needle valve, a second micro needle valve, a sulfur chromatographic packing column, a carbon chromatographic packing column and a quantitative ring;
the first end of the first micro needle valve is connected with the first six-way valve, and the second end of the first micro needle valve is connected with the PDD detector;
the second six-way valve is connected with the PDD detector through the third six-way valve;
two ends of the second micro needle valve are respectively connected with two ports of the second six-way valve;
one end of the sulfur chromatographic packing column is connected with the first six-way valve, and the other end of the sulfur chromatographic packing column is connected with the second six-way valve;
one end of the carbon chromatographic packing column is connected with one port of the second six-way valve, and the other end of the carbon chromatographic packing column is connected with the other port of the second six-way valve;
and two ends of the quantitative ring are respectively connected with two ports of the first six-way valve.
Preferably, the system further comprises: a one-way valve;
one end of the one-way valve is connected with the third six-way valve, and the other end of the one-way valve is connected with the PDD detector.
Preferably, the system further comprises: a pressure regulating valve;
one end of the pressure regulating valve is a carrier gas inlet, and the other end of the pressure regulating valve is connected with the third end of the first micro needle valve.
Preferably, the first port of the first six-way valve is connected with the first micro needle valve and the sixth port of the first six-way valve;
the second port of the first six-way valve is connected with the sulfur chromatographic packing column and the third port of the first six-way valve;
the third port of the first six-way valve is connected with the sixth port of the first six-way valve through the dosing ring;
the fifth port of the first six-way valve is a sample inlet, the fourth port of the first six-way valve is a sample outlet, and the fifth port of the first six-way valve is connected with the fourth port of the first six-way valve.
Preferably, one end of the sulfur chromatographic packing column is connected with the second port of the first six-way valve, and the other end is connected with the second port of the second six-way valve.
Preferably, one end of the carbon chromatographic packing column is connected with the first port of the second six-way valve, and the other end of the carbon chromatographic packing column is connected with the sixth port of the second six-way valve;
one end of the second micro needle valve is connected with a third port of the second six-way valve, and the other end of the second micro needle valve is connected with a fourth port of the second six-way valve;
and a fifth port of the second six-way valve is connected with the third six-way valve.
Preferably, the third port, the fourth port and the fifth port of the third six-way valve are all plugged;
the first port of the third six-way valve is connected with the fifth port of the second six-way valve and the second port of the third six-way valve;
the second port of the third six-way valve is also connected with the PDD detector;
and a sixth port of the third six-way valve is an air outlet.
Preferably, the length of the sulfur chromatographic packed column is 1-4 m;
the length of the carbon chromatographic packing column is 1-4 m.
Preferably, the volume of the quantifying ring is 0.05 ml-2 ml.
Preferably, the system further comprises: a controller;
the controller is connected with the first six-way valve, the second six-way valve, the third six-way valve and the PDD detector.
From the above technical scheme, the application has the following advantages:
the system for quantitatively detecting sulfur hexafluoride gas components provided in the application comprises: the device comprises a first six-way valve, a second six-way valve, a third six-way valve, a PDD detector, a first micro needle valve, a second micro needle valve, a sulfur chromatography packed column, a carbon chromatography packed column and a quantitative ring. The system provided by the application comprises a first traceThe first end of the needle valve is connected with the first six-way valve, and the second end of the needle valve is connected with the PDD detector; the second six-way valve is connected with the PDD detector through a third six-way valve; two ends of the second micro needle valve are respectively connected with two ports of the second six-way valve; one end of the sulfur chromatographic packing column is connected with the first six-way valve, and the other end is connected with the second six-way valve; one end of the carbon chromatographic packing column is connected with one port of the second six-way valve, and the other end of the carbon chromatographic packing column is connected with the other port of the second six-way valve; two ends of the quantitative ring are respectively connected with two ports of the first six-way valve; can realize H in a gas sample to be detected 2 、C 3 F 8 、COS、SO 2 F 2 、H 2 S、CS 2 、N 2 、O 2 、CO、SO 2 、CH 4 、CF 4 The sulfur hexafluoride gas component detection system has the advantages of multiple detectable components, simple instrument structure, low price and convenience in market promotion, and solves the technical problems of the existing sulfur hexafluoride gas component detection system which is lack of multiple detectable components, simple structure, low cost and benefit for large-area popularization and application.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort to a person skilled in the art.
Fig. 1 is a schematic structural diagram of a system for quantitatively detecting sulfur hexafluoride gas component according to an embodiment of the present application;
wherein, the reference numerals are as follows:
1. a first six-way valve; 2. a second six-way valve; 3. a third six-way valve; 4. a pressure regulating valve; 5. a first micro needle valve; 6. a dosing ring; 7. sulfur chromatography packed column; 8. a carbon chromatography packed column; 9. a second micro needle valve; 10. a one-way valve; 11. PDD detector.
Detailed Description
The embodiment of the application discloses a system for quantitatively detecting sulfur hexafluoride gas components, which is used for solving the technical problems of the existing sulfur hexafluoride gas component detection system which is lack of a plurality of detectable components, simple in structure, low in cost and beneficial to large-area popularization and application.
Referring to fig. 1, an embodiment of a system for quantitatively detecting sulfur hexafluoride gas component is provided, where the system for quantitatively detecting sulfur hexafluoride gas component provided in the embodiment of the present application includes: a first six-way valve 1, a second six-way valve 2, a third six-way valve 3, a PDD detector 11, a first micro needle valve 5, a second micro needle valve 9, a sulfur chromatography packed column 7, a carbon chromatography packed column 8 and a quantitative ring 6;
the first micro needle valve 5 is connected with the first six-way valve 1 at a first end and connected with the PDD detector 11 at a second end;
the second six-way valve 2 is connected with the PDD detector 11 through the third six-way valve 3;
two ends of the second micro needle valve 9 are respectively connected with two ports of the second six-way valve 2;
one end of the sulfur chromatographic packing column 7 is connected with the first six-way valve 1, and the other end is connected with the second six-way valve 2;
one end of the carbon chromatographic packing column 8 is connected with one port of the second six-way valve 2, and the other end is connected with the other port of the second six-way valve 2;
the two ends of the dosing ring 6 are respectively connected with the two ports of the first six-way valve 1.
In the embodiment of the application, the working temperature of the PDD detector 11 is 90-150 ℃, the temperature of the sulfur chromatographic packing column 7 is 40-100 ℃, the temperature of the carbon chromatographic packing column 8 is 40-100 ℃, the flow rate of the shielding gas of the PDD detector 11 is 7 ml-30 ml/min, and the flow rates of the carrier gas passing through the sulfur chromatographic packing column 7 and the carbon chromatographic packing column 8 are 15-ml ml/min-50 ml/min. The initial states of the first six-way valve, the second six-way valve and the third six-way valve are all in an off state, each six-way valve is in an on state after one valve actuation, and is in an off state after one valve actuation again. In the embodiment of the application, the first micro needle valve reasonably distributes the flow of the protection gas entering the detector and the carrier gas entering the sulfur chromatographic packing column and/or the carbon chromatographic packing column so as to meet the detection requirement. The second micro needle valve is connected between the two ports of the second six-way valve, so that the resistance of the carrier gas passing through the carbon chromatographic packing column can be simulated, and the sulfur chromatographic packing column can keep the pressure and the flow rate of the carrier gas stable in the switching process of the second six-way valve.
The system for quantitatively detecting sulfur hexafluoride gas components provided in the embodiment of the application comprises: a first six-way valve 1, a second six-way valve 2, a third six-way valve 3, a PDD detector 11, a first micro needle valve 5, a second micro needle valve 9, a sulfur chromatography packed column 7, a carbon chromatography packed column 8 and a dosing ring 6. In the system provided by the application, a first end of a first micro needle valve 5 is connected with a first six-way valve 1, and a second end is connected with a PDD detector 11; the second six-way valve 6 is connected with the PDD detector 11 through the third six-way valve 3; two ends of the second micro needle valve 9 are respectively connected with two ports of the second six-way valve 2; one end of the sulfur chromatographic packing column 7 is connected with the first six-way valve 1, and the other end is connected with the second six-way valve 2; one end of the carbon chromatographic packing column 8 is connected with one port of the second six-way valve 2, and the other end is connected with the other port of the second six-way valve 2; two ends of the quantitative ring 6 are respectively connected with two ports of the first six-way valve 1; can realize H in a gas sample to be detected 2 、C 3 F 8 、COS、SO 2 F 2 、H 2 S、CS 2 、N 2 、O 2 、CO、SO 2 、CH 4 、CF 4 The sulfur hexafluoride gas component detection system has the advantages of multiple detectable components, simple instrument structure, low price and convenience in market promotion, and solves the technical problems of the existing sulfur hexafluoride gas component detection system which is lack of multiple detectable components, simple structure, low cost and benefit for large-area popularization and application.
Referring to fig. 1, another embodiment of a system for quantitatively detecting sulfur hexafluoride gas component is provided, where the system for quantitatively detecting sulfur hexafluoride gas component includes: a first six-way valve 1, a second six-way valve 2, a third six-way valve 3, a PDD detector 11, a first micro needle valve 5, a second micro needle valve 9, a sulfur chromatography packed column 7, a carbon chromatography packed column 8 and a quantitative ring 6;
the first micro needle valve 5 is connected with the first six-way valve 1 at a first end and connected with the PDD detector 11 at a second end;
the second six-way valve 2 is connected with the PDD detector 11 through the third six-way valve 3;
two ends of the second micro needle valve 9 are respectively connected with two ports of the second six-way valve 2;
one end of the sulfur chromatographic packing column 7 is connected with the first six-way valve 1, and the other end is connected with the second six-way valve 2;
one end of the carbon chromatographic packing column 8 is connected with one port of the second six-way valve 2, and the other end is connected with the other port of the second six-way valve 2;
the two ends of the dosing ring 6 are respectively connected with the two ports of the first six-way valve 1.
Further, the system further comprises: a one-way valve 10;
one end of the check valve 10 is connected to the third six-way valve 3, and the other end is connected to the PDD detector 11.
The check valve 10 can prevent the shielding gas from back blowing to the sulfur chromatographic packing column 7 and the carbon chromatographic packing column 8, so that the PDD detector 11 does not generate a peak or the peak shape is abnormal, the detection result is affected, and the detection sensitivity is ensured.
Further, the system further comprises: a pressure regulating valve 4;
one end of the pressure regulating valve 4 is a carrier gas inlet, and the other end is connected with a third end of the first micro needle valve 5.
The pressure regulating valve 4 is connected in front of the first micro needle valve 5, so that the stability of the flow rate and pressure of the gas in the valve path can be ensured when the carrier gas enters the valve path system, and the accuracy of the detection result can be ensured.
Further, the first port of the first six-way valve 1 is connected with the first micro needle valve 5 and the sixth port of the first six-way valve 1;
the second port of the first six-way valve 1 is connected with the sulfur chromatographic packing column 7 and the third port of the first six-way valve 1;
the third port of the first six-way valve 1 is connected with the sixth port of the first six-way valve 1 through a dosing ring 6;
the fifth port of the first six-way valve 1 is a sample inlet, the fourth port of the first six-way valve 1 is a sample outlet, and the fifth port of the first six-way valve 1 is connected with the fourth port of the first six-way valve 1.
Further, one end of the sulfur chromatography packing column 7 is connected to the second port of the first six-way valve 1, and the other end is connected to the second port of the second six-way valve.
Further, one end of the carbon chromatographic packing column 8 is connected with the first port of the second six-way valve 2, and the other end is connected with the sixth port of the second six-way valve 2;
one end of the second micro needle valve 9 is connected with a third port of the second six-way valve 2, and the other end is connected with a fourth port of the second six-way valve 2;
the fifth port of the second six-way valve 2 is connected with the third six-way valve 3.
Further, the third port, the fourth port and the fifth port of the third six-way valve 3 are all plugged;
the first port of the third six-way valve 3 is connected with the fifth port of the second six-way valve 2 and the second port of the third six-way valve 3;
the second port of the third six-way valve 3 is also connected with a PDD detector 11;
the sixth port of the third six-way valve 3 is an air outlet.
Further, the length of the sulfur chromatographic packed column 7 is 1-4 m;
the length of the carbon chromatographic packing column 8 is 1-4 m.
It should be noted that, in the embodiment of the present application, in order to ensure the separation degree and sensitivity of the gas sample to be detected and reduce the separation time, the lengths of the sulfur chromatographic packing column 7 and the carbon chromatographic packing column 8 should not be too short or too long, and should be limited to a range of 1m to 4m, in the embodiment of the present application, the lengths of the sulfur chromatographic packing column 7 and the carbon chromatographic packing column 8 are 2m, so that the best separation effect can be obtained.
Further, the volume of the quantifying ring 6 is 0.05ml to 2ml.
The volume of the quantitative ring 6 is 0.05ml to 2ml, and the optimal volume is 1ml.
Further, the system further comprises: a controller;
the controller is connected with the first six-way valve 1, the second six-way valve 2, the third six-way valve 3 and the PDD detector 11.
It should be noted that, the controller in the embodiment of the present application may be a microcomputer or an instrument panel with a liquid crystal display, which may control the valve movements of the first six-way valve 1, the second six-way valve 2 and the third six-way valve 3, and may provide network remote management for the connection device of the system, so as to be beneficial to remote monitoring and management of instruments and data.
In the embodiment of the application, the analysis process of the sulfur hexafluoride gas sample is as follows:
1. helium with purity of more than 99.999% and purified by a helium purifier is used as carrier gas and sequentially passes through a first port of a first six-way valve, a sixth port of the first six-way valve, a quantitative ring, a third port of the first six-way valve, a second port of the first six-way valve, a sulfur chromatographic packing column, a second port of the second six-way valve, a first port of the second six-way valve, a carbon chromatographic packing column, a sixth port of the second six-way valve, a fifth port of the second six-way valve, a first port of a third six-way valve, a second port of the third six-way valve, a one-way valve and a PDD detector.
2. And opening a first six-way valve, and enabling a gas sample to be detected to pass through a fifth port of the first six-way valve, a sixth port of the first six-way valve, the quantitative ring, a third port of the first six-way valve and a fourth port of the first six-way valve in sequence, so as to exhaust gas, wherein the quantitative ring and the sample injection pipeline are fully purged and replaced, and the purging and replacing time is 1-2 min.
3. And a first six-way valve is valve-driven again, and a gas sample to be detected sequentially passes through a sixth port of the first six-way valve, the quantitative ring, a third port of the first six-way valve, a second port of the first six-way valve, a sulfur chromatographic packing column, a second port of the second six-way valve, a first port of the second six-way valve, a carbon chromatographic packing column, a sixth port of the second six-way valve, a fifth port of the second six-way valve, a first port of the third six-way valve, a second port of the third six-way valve and a PDD detector. At this time, the gas sample to be detected is passed through both the sulfur chromatography packed column and the carbon chromatography packed column.
4. And opening the second six-way valve and simultaneously opening the third six-way valve, wherein the gas sample to be detected passes through a second port of the second six-way valve, a third port of the second six-way valve, a second micro needle valve, a fourth port of the second six-way valve, a fifth port of the second six-way valve, a first port of the third six-way valve and a sixth port of the third six-way valve. In the process, the gas sample to be detected enters the gas outlet after passing through the sixth port of the third six-way valve, and the SF is mainly realized 6 Evacuation of the components, preventing SF 6 The detection of other components by a component interferes.
5. And opening the second six-way valve, closing the third six-way valve, and allowing the gas sample to be detected to pass through a second port of the second six-way valve, a third port of the second six-way valve, a second micro needle valve, a fourth port of the second six-way valve, a fifth port of the second six-way valve, a first port of the third six-way valve, a second port of the third six-way valve and a PDD detector. In the process, the gas sample to be detected only passes through the sulfur chromatographic packing column, and the C is mainly realized 3 F 8 、COS、SO 2 F 2 、H 2 S、CS 2 、SO 2 Detecting the components with the peak sequence of C 3 F 8 、COS、SO 2 F 2 、H 2 S、CS 2 、SO 2
6. And (3) valve-driving the second six-way valve again, wherein the gas sample to be detected passes through the second port of the second six-way valve, the first port of the second six-way valve, the carbon chromatographic packing column, the sixth port of the second six-way valve, the fifth port of the second six-way valve, the first port of the third six-way valve, the second port of the third six-way valve and the PDD detector from the sulfur chromatographic packing column. The process of switching the second six-way valve again is mainly realized for H 2 、N 2 、O 2 、CO、CH 4 、CF 4 Detecting the components with the peak sequence of H 2 、N 2 、O 2 、CO、CH 4 、CF 4
7. After one sample injection, the final peak outlet sequence of the sulfur hexafluoride gas component is as follows: c (C) 3 F 8 、COS、SO 2 F 2 、H 2 S、CS 2 、SO 2 、H 2 、N 2 、O 2 、CO、CH 4 、CF 4
In this embodiment of the present application, the analysis process of the sulfur hexafluoride gas sample may further be:
1. helium with purity of more than 99.999% and purified by a helium purifier is used as carrier gas and sequentially passes through a first port of a first six-way valve, a sixth port of the first six-way valve, a quantitative ring, a third port of the first six-way valve, a second port of the first six-way valve, a sulfur chromatographic packing column, a second port of the second six-way valve, a first port of the second six-way valve, a carbon chromatographic packing column, a sixth port of the second six-way valve, a fifth port of the second six-way valve, a first port of a third six-way valve, a second port of the third six-way valve, a one-way valve and a PDD detector.
2. And opening a first six-way valve, and enabling a gas sample to be detected to pass through a fifth port of the first six-way valve, a sixth port of the first six-way valve, the quantitative ring, a third port of the first six-way valve and a fourth port of the first six-way valve in sequence, so as to exhaust gas, wherein the quantitative ring and the sample injection pipeline are fully purged and replaced, and the purging and replacing time is 1-2 min.
3. And a first six-way valve is valve-driven again, and a gas sample to be detected sequentially passes through a sixth port of the first six-way valve, the quantitative ring, a third port of the first six-way valve, a second port of the first six-way valve, a sulfur chromatographic packing column, a second port of the second six-way valve, a first port of the second six-way valve, a carbon chromatographic packing column, a sixth port of the second six-way valve, a fifth port of the second six-way valve, a first port of the third six-way valve, a second port of the third six-way valve and a PDD detector. At this time, the gas sample to be detected is passed through both the sulfur chromatography packed column and the carbon chromatography packed column.
4. Opening a second six-way valve and simultaneously opening a third six-way valve, wherein a gas sample to be detected passes through a second port of the second six-way valve, a third port of the second six-way valve, a second micro needle valve, a fourth port of the second six-way valve, a fifth port of the second six-way valve, a first port of the third six-way valve and a third six-way valveAnd a sixth port of the valve. In the process, the gas sample to be detected enters the gas outlet after passing through the sixth port of the third six-way valve, and the SF is mainly realized 6 Evacuation of the components, preventing SF 6 The detection of other components by a component interferes.
5. And opening the second six-way valve, closing the third six-way valve, and allowing the gas sample to be detected to pass through a second port of the second six-way valve, a third port of the second six-way valve, a second micro needle valve, a fourth port of the second six-way valve, a fifth port of the second six-way valve, a first port of the third six-way valve, a second port of the third six-way valve and a PDD detector. In the process, the gas sample to be detected only passes through the sulfur chromatographic packing column, and the C is mainly realized 3 F 8 、COS、SO 2 F 2 、H 2 S、CS 2 Etc., the peak-out sequence is C in turn 3 F 8 、COS、SO 2 F 2 、H 2 S、CS 2
6. And (3) valve-driving the second six-way valve again, wherein the gas sample to be detected passes through the second port of the second six-way valve, the first port of the second six-way valve, the carbon chromatographic packing column, the sixth port of the second six-way valve, the fifth port of the second six-way valve, the first port of the third six-way valve, the second port of the third six-way valve and the PDD detector from the sulfur chromatographic packing column. The process of switching the second six-way valve again is mainly realized for H 2 、N 2 、O 2 Detection of CO and the like, and the peak-out sequence is H 2 、N 2 、O 2 、CO。
7. And opening the second six-way valve again, and enabling the gas sample to be detected to pass through a second port of the second six-way valve, a third port of the second six-way valve, a second micro needle valve, a fourth port of the second six-way valve, a fifth port of the second six-way valve, a first port of the third six-way valve, a second port of the third six-way valve and a PDD detector. In the process, the gas sample to be detected only passes through the sulfur chromatographic packing column, and the SO is mainly realized 2 Is detected.
8. The second six-way valve is valve-operated again, and the gas sample to be detected passes through the second port of the second six-way valve from the sulfur chromatographic packing column,The device comprises a first port of a second six-way valve, a carbon chromatographic packing column, a sixth port of the second six-way valve, a fifth port of the second six-way valve, a first port of a third six-way valve, a second port of the third six-way valve and a PDD detector. The process of switching the second six-way valve again is mainly realized for CH 4 、CF 4 Etc., the peak-out sequence is CH in turn 4 、CF 4
9. After one sample injection, the final peak outlet sequence of the sulfur hexafluoride gas component is as follows: c (C) 3 F 8 、COS、SO 2 F 2 、H 2 S、CS 2 、H 2 、N 2 、O 2 、CO、SO 2 、CH 4 、CF 4
Through the valve action switching of the second six-way valve, the peak outlet sequence of the sulfur hexafluoride gas component can be changed, and it can be understood that, based on the embodiment of the application, a person skilled in the art can perform corresponding control adjustment according to actual application requirements, and the one-to-one example is not performed here.
The embodiment of the application adopts a three-valve two-column one-detector system, namely a first six-way valve, a second six-way valve, a third six-way valve, a sulfur chromatographic packing column, a carbon chromatographic packing column and a PDD detector, and has the advantages of simple structure, low cost and higher cost performance; the detection operation is convenient, and the determination of more than ten gas components of sulfur hexafluoride can be completed by one sample injection; the two chromatographic columns are filled columns, so that the separation effect is good, and the miniaturization of a column box and the whole chromatograph is facilitated; by controlling the switching of the valve, the sulfur hexafluoride as a main component can be removed, so that the pollution of the sulfur hexafluoride to the PDD detector is avoided, and the influence of the sulfur hexafluoride on the micro-component analysis is greatly reduced.
The above embodiments are only for illustrating the technical solution of the present application, and are not limiting thereof; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the corresponding technical solutions.

Claims (6)

1. A method for quantitatively detecting sulfur hexafluoride gas constituent, the method being practiced with a system for quantitatively detecting sulfur hexafluoride gas constituent, the system comprising: the device comprises a first six-way valve, a second six-way valve, a third six-way valve, a PDD detector, a first micro needle valve, a second micro needle valve, a sulfur chromatographic packing column, a carbon chromatographic packing column and a quantitative ring;
the first end of the first micro needle valve is connected with the first six-way valve, and the second end of the first micro needle valve is connected with the PDD detector;
the second six-way valve is connected with the PDD detector through the third six-way valve;
two ends of the second micro needle valve are respectively connected with two ports of the second six-way valve;
one end of the sulfur chromatographic packing column is connected with the first six-way valve, and the other end of the sulfur chromatographic packing column is connected with the second six-way valve;
one end of the carbon chromatographic packing column is connected with one port of the second six-way valve, and the other end of the carbon chromatographic packing column is connected with the other port of the second six-way valve;
two ends of the quantitative ring are respectively connected with two ports of the first six-way valve;
the first port of the first six-way valve is connected with the first micro needle valve and the sixth port of the first six-way valve;
the second port of the first six-way valve is connected with the sulfur chromatographic packing column and the third port of the first six-way valve;
the third port of the first six-way valve is connected with the sixth port of the first six-way valve through the dosing ring;
the fifth port of the first six-way valve is a sample inlet, the fourth port of the first six-way valve is a sample outlet, and the fifth port of the first six-way valve is connected with the fourth port of the first six-way valve;
one end of the sulfur chromatographic packing column is connected with the second port of the first six-way valve, and the other end of the sulfur chromatographic packing column is connected with the second port of the second six-way valve;
one end of the carbon chromatographic packing column is connected with the first port of the second six-way valve, and the other end of the carbon chromatographic packing column is connected with the sixth port of the second six-way valve;
one end of the second micro needle valve is connected with a third port of the second six-way valve, and the other end of the second micro needle valve is connected with a fourth port of the second six-way valve;
the second port of the second six-way valve is connected with the first port of the second six-way valve;
the fifth port of the second six-way valve is connected with the sixth port of the second six-way valve and the third six-way valve;
the third port, the fourth port and the fifth port of the third six-way valve are all plugged;
the first port of the third six-way valve is connected with the fifth port of the second six-way valve and the second port of the third six-way valve;
the second port of the third six-way valve is also connected with the PDD detector;
a sixth port of the third six-way valve is an air outlet;
the method comprises the following steps:
s1, taking helium with the purity of more than 99.999% and purified by a helium purifier as carrier gas, and sequentially passing through a first port of a first six-way valve, a sixth port of the first six-way valve, a dosing ring, a third port of the first six-way valve, a second port of the first six-way valve, a sulfur chromatographic packed column, a second port of a second six-way valve, a first port of the second six-way valve, a carbon chromatographic packed column, a sixth port of the second six-way valve, a fifth port of the second six-way valve, a first port of a third six-way valve, a second port of the third six-way valve, a one-way valve and a PDD detector;
s2, rotating a first six-way valve, and exhausting gas through a fifth port of the first six-way valve, a sixth port of the first six-way valve, a quantitative ring, a third port of the first six-way valve and a fourth port of the first six-way valve in sequence, wherein the quantitative ring and a sample injection pipeline are fully purged and replaced, and the purging and replacing time is 1-2 min;
s3, rotating the first six-way valve again, and enabling the gas sample to be detected to sequentially pass through a sixth port of the first six-way valve, a quantitative ring, a third port of the first six-way valve, a second port of the first six-way valve, a sulfur chromatograph packing column, a second port of the second six-way valve, a first port of the second six-way valve, a carbon chromatograph packing column, a sixth port of the second six-way valve, a fifth port of the second six-way valve, a first port of the third six-way valve, a second port of the third six-way valve and a PDD detector, wherein the gas sample to be detected passes through the sulfur chromatograph packing column and the carbon chromatograph packing column at the moment;
s4, rotating the second six-way valve and simultaneously rotating the third six-way valve, wherein a gas sample to be detected enters the gas outlet after passing through the second port of the second six-way valve, the third port of the second six-way valve, the second micro needle type valve, the fourth port of the second six-way valve, the fifth port of the second six-way valve, the first port of the third six-way valve and the sixth port of the third six-way valve, and in the process, the gas sample to be detected mainly realizes SF (sulfur hexafluoride) after passing through the sixth port of the third six-way valve 6 Evacuation of the components, preventing SF 6 The detection of other components by the components is interfered;
s5, maintaining a second six-way valve, rotating a third six-way valve, and enabling a gas sample to be detected to pass through a second port of the second six-way valve, a third port of the second six-way valve, a second micro needle type valve, a fourth port of the second six-way valve, a fifth port of the second six-way valve, a first port of the third six-way valve, a second port of the third six-way valve and a PDD detector, wherein in the process, the gas sample to be detected only passes through a sulfur chromatographic packing column, and the C is mainly realized 3 F 8 、COS、SO 2 F 2 、H 2 S、CS 2 、SO 2 Detecting components, wherein the peak sequence is C in sequence 3 F 8 、COS、SO 2 F 2 、H 2 S、CS 2 、SO 2
S6, rotating the second six-way valve again, and enabling the gas sample to be detected to pass through the second port of the second six-way valve, the first port of the second six-way valve, the carbon chromatographic packing column and the second six-way valve from the sulfur chromatographic packing columnThe second six-way valve is switched again at this time, and H is mainly realized 2 、N 2 、O 2 、CO、CH 4 、CF 4 Detecting components, wherein the peak sequence is H 2 、N 2 、O 2 、CO、CH 4 、CF 4
S7, after one sample injection, the final peak outlet sequence of the sulfur hexafluoride gas component is as follows: c (C) 3 F 8 、COS、SO 2 F 2 、H 2 S、CS 2 、SO 2 、H 2 、N 2 、O 2 、CO、CH 4 、CF 4
Or the method comprises the following steps:
s1, taking helium with the purity of more than 99.999% and purified by a helium purifier as carrier gas, and sequentially passing through a first port of a first six-way valve, a sixth port of the first six-way valve, a dosing ring, a third port of the first six-way valve, a second port of the first six-way valve, a sulfur chromatographic packed column, a second port of a second six-way valve, a first port of the second six-way valve, a carbon chromatographic packed column, a sixth port of the second six-way valve, a fifth port of the second six-way valve, a first port of a third six-way valve, a second port of the third six-way valve, a one-way valve and a PDD detector;
s2, rotating a first six-way valve, and exhausting gas through a fifth port of the first six-way valve, a sixth port of the first six-way valve, a quantitative ring, a third port of the first six-way valve and a fourth port of the first six-way valve in sequence, wherein the quantitative ring and a sample injection pipeline are fully purged and replaced, and the purging and replacing time is 1-2 min;
s3, rotating the first six-way valve again, and enabling the gas sample to be detected to sequentially pass through a sixth port of the first six-way valve, a quantitative ring, a third port of the first six-way valve, a second port of the first six-way valve, a sulfur chromatograph packing column, a second port of the second six-way valve, a first port of the second six-way valve, a carbon chromatograph packing column, a sixth port of the second six-way valve, a fifth port of the second six-way valve, a first port of the third six-way valve, a second port of the third six-way valve and a PDD detector, wherein the gas sample to be detected passes through the sulfur chromatograph packing column and the carbon chromatograph packing column at the moment;
s4, rotating the second six-way valve and simultaneously rotating the third six-way valve, wherein a gas sample to be detected enters the gas outlet after passing through the second port of the second six-way valve, the third port of the second six-way valve, the second micro needle type valve, the fourth port of the second six-way valve, the fifth port of the second six-way valve, the first port of the third six-way valve and the sixth port of the third six-way valve, and in the process, the gas sample to be detected enters the gas outlet after passing through the sixth port of the third six-way valve, so that the SF6 component is mainly emptied, and the SF6 component is prevented from interfering with the detection of other components;
s5, maintaining a second six-way valve, rotating a third six-way valve, and enabling a gas sample to be detected to pass through a second port of the second six-way valve, a third port of the second six-way valve, a second micro needle type valve, a fourth port of the second six-way valve, a fifth port of the second six-way valve, a first port of the third six-way valve, a second port of the third six-way valve and a PDD detector, wherein in the process, the gas sample to be detected only passes through a sulfur chromatographic packing column, and the C is mainly realized 3 F 8 、COS、SO 2 F 2 、H 2 S、CS 2 The peak-out sequence is C in turn 3 F 8 、COS、SO 2 F 2 、H 2 S、CS 2
S6, rotating the second six-way valve again, and enabling the gas sample to be detected to pass through the second port of the second six-way valve, the first port of the second six-way valve, the carbon chromatographic packing column, the sixth port of the second six-way valve, the fifth port of the second six-way valve, the first port of the third six-way valve, the second port of the third six-way valve and the PDD detector from the sulfur chromatographic packing column, wherein the process of switching the second six-way valve again is mainly realized for H 2 、N 2 、O 2 Detecting CO, and the peak sequence is H 2 、N 2 、O 2 、CO;
S7, rotating the second six-way valve again, and enabling the gas sample to be detected to pass through a second port and a third port of the second six-way valveThe third port of the two six-way valve, the second micro needle type valve, the fourth port of the second six-way valve, the fifth port of the second six-way valve, the first port of the third six-way valve, the second port of the third six-way valve and the PDD detector, and in the process, the gas sample to be detected only passes through the sulfur chromatographic packing column, and mainly realizes SO (sulfur-doped oxygen) detection 2 Is detected;
s8, rotating the second six-way valve again, enabling the gas sample to be detected to pass through the second port of the second six-way valve, the first port of the second six-way valve, the carbon chromatographic packing column, the sixth port of the second six-way valve, the fifth port of the second six-way valve, the first port of the third six-way valve, the second port of the third six-way valve and the PDD detector from the sulfur chromatographic packing column, and switching the second six-way valve again, wherein the process of switching the second six-way valve again is mainly realized for CH 4 、CF 4 The peak-out sequence is CH in turn 4 、CF 4
S9, after one sample injection, the final peak outlet sequence of the sulfur hexafluoride gas component is as follows: c (C) 3 F 8 、COS、SO 2 F 2 、H 2 S、CS 2 、H 2 、N 2 、O 2 、CO、SO 2 、CH 4 、CF 4
2. The method of claim 1, wherein the system further comprises: a one-way valve;
one end of the one-way valve is connected with the third six-way valve, and the other end of the one-way valve is connected with the PDD detector.
3. The method of claim 1, wherein the system further comprises: a pressure regulating valve;
one end of the pressure regulating valve is a carrier gas inlet, and the other end of the pressure regulating valve is connected with the third end of the first micro needle valve.
4. The method of claim 1, wherein the sulfur chromatography packed column has a length of 1 to 4m;
the length of the carbon chromatographic packing column is 1-4 m.
5. The method of claim 1, wherein the dosing ring has a volume of 0.05ml to 2ml.
6. The method according to any one of claims 1 to 5, wherein the system further comprises: a controller;
the controller is connected with the first six-way valve, the second six-way valve, the third six-way valve and the PDD detector.
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