CN104198638A - Chromatographic analysis system and method for detecting sulfur hexafluoride decomposition products - Google Patents
Chromatographic analysis system and method for detecting sulfur hexafluoride decomposition products Download PDFInfo
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- CN104198638A CN104198638A CN201410413157.7A CN201410413157A CN104198638A CN 104198638 A CN104198638 A CN 104198638A CN 201410413157 A CN201410413157 A CN 201410413157A CN 104198638 A CN104198638 A CN 104198638A
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Abstract
The invention discloses a chromatographic analysis system and method for detecting sulfur hexafluoride decomposition products. A sample injection valve connector I is connected with a sample injection valve connector IV; a sample injection valve connector II is communicated with a sample injection pipe; a sample injection valve connector III is connected with an emptying valve I; a sample injection valve connector V is connected with a first chromatographic column; the sample injection valve connector IV is connected with sample injection valve carrier gas; a connector I of a detector switching valve is communicated with the first chromatographic column, a connector II of the detector switching valve is connected with a first detector, a connector III of the detector switching valve is connected with detector switching valve carrier gas, a connector IV of the detector switching valve is connected with a shunt, and the shunt is connected with a second chromatographic column; a connector I of a four-way switching valve is connected with an emptying valve IV, a connector II of the four-way switching valve is connected with the second chromatographic column, a connector III of the four-way switching valve is connected with a second detector, and a connector IV of the four-way switching valve is connected with four-way valve carrier gas. The system and the method can be used for detecting all the components of the decomposition products such as CF4, CO, CO2, SF2O2, SF2O and H2S, and simultaneously, the conditions of peak broadening and SF6 trailing caused by series connection of the detectors can be avoided.
Description
Technical field
The present invention relates to a kind of chromatographic analysis systems and method, be particularly useful for the stratographic analysis of sulfur hexafluoride decomposition product.
Background technology
The stratographic analysis flow process of the sulfur hexafluoride decomposition product of comparative maturity is all to adopt dual-detector detecting pattern, the general universal thermal conductivity detector (TCD) of TCD of installing, for example, with sulfide detecting device (FPD sulfide detecting device), the former is for the carbon tetrafluoride (CF to sulfur hexafluoride decomposition product
4), CO (carbon monoxide), CO
2materials such as (carbon dioxide) detects, and the latter is used for fluoridizing sulfonyl (SF
2o
2), fluoridize thionyl (SF
2o), sulfuretted hydrogen (H
2s), sulphuric dioxide (SO
2) etc. sulfocompound detect.At present, the general detecting device series connection analysis process that adopts, be that carrier gas enters successively two detecting devices and detects after chromatographic column with sample, but this flow process has two main shortcomings to be: first, the hangover situation of sulfur hexafluoride is very serious, even sometimes can cover its small concentration component below, for example, fluoridize sulfonyl; Second, under same test condition, after appearance time more leans on, go out peak-to-peak type wider, more difficult detection, owing to being that detecting device adopts series system, sample enters sulfide detecting device again and can cause the component peaks type that goes out peak on sulfide detecting device to be widened after high temperature TCD detecting device (temperature of general TCD detecting device reaches more than 250 DEG C), quantitative error is larger, is unfavorable for carrying out trace analysis; The 3rd, SF
6the highest SF beyond doubt of content in decomposition product
6if, SF
6component detects in sulfide detecting device, and its peak height is for example, by the very high detecting device ultimate value (FPD detecting device) that even exceedes, thereby causes whole spectrogram to be difficult for little content component to carry out integration, and the utmost point is not attractive in appearance.
Summary of the invention
In order to address the above problem, the present invention proposes a kind of chromatographic analysis system that detects sulfur hexafluoride decomposition product.
The technical solution adopted in the present invention is:
Detect a chromatographic analysis system for sulfur hexafluoride decomposition product, comprise sample feeding pipe, sampling valve, the first root chromatogram column, detecting device transfer valve, the second root chromatogram column and four-way switching valve; Wherein, described sampling valve interface I is connected with interface IV, and interface II is communicated with sample feeding pipe, and interface III is connected with atmospheric valve I, and interface V is connected with the first root chromatogram column, and interface VI is connected with sampling valve carrier gas; The interface I of described detecting device transfer valve is communicated with the first root chromatogram column, and interface II connects the first detecting device, the carrier gas of interface III connection detector transfer valve, and interface IV connects a shunt, and described shunt is connected with the second chromatographic column; The interface I of described four-way switching valve connects atmospheric valve IV, and interface II connects the second chromatographic column; Interface III connects the second detecting device, and interface VI connects four-way valve carrier gas.
Between sampling valve interface I and interface IV, be connected with quantity tube.
The first described detecting device is PPD helium ion detector or TCD thermal conductivity detector (TCD).
The second described detecting device is PPD helium ion detector or FPD sulfide detecting device,
Described carrier gas be helium.
The first described chromatographic column is Porapak Q packed column, and the second chromatographic column is Gaspro capillary column, and the first chromatographic column is main separation chromatography post, and the second chromatographic column is that auxiliary separating is from chromatographic column.
Described shunt one end is connected with an air damping, and the other end connects the second chromatographic column, and described air damping can root
According to requiring to reconcile damping size.
The first described detecting device is PPD helium ion detector or TCD thermal conductivity detector (TCD).
The second described detecting device is PPD helium ion detector or FPD sulfide detecting device.
Carrier gas used is helium.
Detect a chromatogram analysis method for sulfur hexafluoride decomposition product, as follows:
Before sampling valve does not switch, sample enters quantity tube by sampling valve interface II and sampling valve interface I, and finally emptying via sampling valve interface IV and sampling valve interface III, after switching, carrier gas enters quantity tube and enters the first chromatographic column with sample wherein by sampling valve interface V via sampling valve interface VI and sampling valve interface I and separates for the first time;
Sample after separating for the first time directly enters the first detecting device by detecting device transfer valve interface I and detecting device transfer valve interface II 1 and detects, the gas having detected is discharged by atmospheric valve II, treat first detecting device detect component detect after switch detector transfer valve, the component that goes out peak evening enters shunt by detecting device transfer valve interface I and detecting device transfer valve interface IV in the situation that not entering the first detecting device, sample flow enters the second chromatographic column after being reduced according to the ratio of setting by shunt, separates for the second time;
Sample after secondary separation enters four-way switching valve by four-way switching valve interface II and is discharged and carried out emptying by four-way switching valve interface I again, treats SF
6component emptying is complete, switches four-way switching valve, makes sample enter the second detecting device by four-way switching valve interface II and four-way switching valve interface III and detects, and the gas having detected is discharged from atmospheric valve V.
The invention has the beneficial effects as follows,
Detecting device transfer valve is arranged on after the first chromatographic column, the sample that carrier gas is carried is switched to detecting device and shunt on request, to all switch into the first detecting device from the first chromatographic column sample out or all switch to shunt, make the sample separating for the second time without the first detecting device, in case the first detector temperature too high cause late go out peak component peaks type widen.
Four-way switching valve is arranged between the second detecting device and the second chromatographic column, the sample that when initial, the second chromatographic column is come is in emptying state, do not enter the second detecting device, after switching, sample enters the second detecting device, so just can control the peak that goes out of SF66, and does not allow SF6 component enter the second detecting device and detects, thereby reduce, on the impact of component thereafter, also to make spectrogram more attractive in appearance.
The present invention is by sampling valve, detecting device transfer valve, and four-way switching valve realizes the switching to sample trend, shunt and air damping are realized the sample size of the second root chromatogram column are controlled, and finally realize the first detecting device and detect CF
4, CO, CO
2, the second detecting device detects SF
2o
2, SF
2o, H
2s, SO
2etc. component, by the second root chromatogram column, not segregative component is carried out to secondary separation, main SF
6background gas carries out emptying processing by four-way switching valve.
Brief description of the drawings
Fig. 1 stratographic analysis flowage structure of the present invention figure;
In Fig. 1: 1. sample feeding pipe; 2. quantity tube; 3. carrier gas; 4. sampling valve; 5. sampling valve interface I; 6. sampling valve interface II; 7. sampling valve interface III; 8. sampling valve interface IV; 9. sampling valve interface V; 10. sampling valve interface VI; 11. atmospheric valve I; 12. first chromatographic columns; 13. connecting lines; 14. detecting device transfer valves; 15. detecting device transfer valve interface I; 16. detecting device transfer valve interface II; 17. detecting device transfer valve interface III; 18. detecting device transfer valve interface IV; 19. first detecting devices; 20. atmospheric valve II; 21. shunts; 22. air-flow dampings; 23. atmospheric valve III; 24. second chromatographic columns; 25. four-way switching valves; 26. four-way switching valve interface I; 27. four-way switching valve interface II; 28. four-way switching valve interface III; 29. four-way switching valve interface IV; 30. atmospheric valve IV; 31. four-way valve carrier gas; 32. second detecting devices; 33. atmospheric valve V; 34. detecting device transfer valve carrier gas.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in detail:
Sample feeding pipe 1 is connected with sampling valve interface II 6, one end of quantity tube 2 is connected with sampling valve interface I 5, the other end is connected with sampling valve interface IV 8, carrier gas 3 is connected with sampling valve interface VI 10, sampling valve interface V 9 is connected with the first chromatographic column 12 sample introduction ends, detecting device transfer valve interface I 15 is connected with the first chromatographic column 12 sample outlet ends by connecting line 13, the first detecting device 19 is connected with detecting device transfer valve interface II 16, detecting device transfer valve carrier gas 34 is connected with detecting device transfer valve interface III 17, shunt 21 is connected with detecting device transfer valve interface IV 18 by connecting line 13, air damping 22 is arranged on a branch road of shunt 21, the sample introduction end of the second chromatographic column 24 is connected with another branch road of shunt 21, the sample outlet end of the second chromatographic column 24 is connected with four-way switching valve interface II 27, the second detecting device 32 is connected with four-way switching valve interface III 28, four-way valve carrier gas 31 is connected with four-way switching valve interface IV 29, atmospheric valve I 11, atmospheric valve II 20, atmospheric valve III 23, atmospheric valve IV 30, atmospheric valve V 33 respectively with sampling valve interface III 7, the first detecting device 19, air-flow damping 22, four-way switching valve interface I 26, the second detecting device 32 is connected.
Before sampling valve 4 does not switch, sample enters quantity tube 2 by sampling valve interface II 6 and sampling valve interface I 5, and finally emptying via sampling valve interface IV 8 and sampling valve interface III 7, after switching, carrier gas 3 enters quantity tube 2 and enters the first chromatographic column 12 with sample wherein by sampling valve interface V 9 via sampling valve interface VI 10 and sampling valve interface I 5 and separates for the first time, this time mainly separates CF
4, CO, CO
2, initial gross separation SF
6, F
2sO
2, F2SO, H
2s etc., sample after separating for the first time directly enters the first detecting device 19 by detecting device transfer valve interface I and detecting device transfer valve interface II 16 and detects, the gas having detected is discharged by atmospheric valve II 20, treat component that the first detecting device 19 detects detect after switch detector transfer valve 14, the component that goes out peak evening just enters shunt 21 by detecting device transfer valve interface I 15 and detecting device transfer valve interface IV 18 in the situation that having little time to enter the first detecting device 19, sample flow enters the second chromatographic column 24 after being reduced according to certain ratio by shunt 21, separate for the second time, separate and contribute to SF for the second time
6the component that later goes out peak is avoided SF
6impact, the sample after secondary separation enters four-way switching valve 25 by four-way switching valve interface II 27 and is discharged and carried out emptying by four-way switching valve interface I 26 again, treats SF
6component emptying is complete, switches four-way switching valve 25, is that sample enters the second detecting device 32 by four-way switching valve interface II 27 and four-way switching valve interface III 28 and detects, and the gas having detected is discharged from atmospheric valve V 33.
The first detecting device is PPD helium ion detector or TCD thermal conductivity detector (TCD).
The second detecting device is PPD helium ion detector or FPD sulfide detecting device,
Carrier gas is helium.
The first chromatographic column is Porapak Q packed column, and the second chromatographic column is Gaspro capillary column, and the first chromatographic column is main separation chromatography post, and the second chromatographic column is that auxiliary separating is from chromatographic column.
Shunt one end is connected with an air damping, and the other end connects the second chromatographic column, and air damping can be reconciled damping size as requested.
The first detecting device can be PPD helium ion detector, can be also TCD thermal conductivity detector (TCD).The second detecting device can be PPD
Helium ion detector, can be also FPD sulfide detecting device, and carrier gas used is helium.
The present invention realizes CF
4, CO, CO2, SF
2o
2, SF
2o, H
2the full constituent of the decomposition products such as S detects, and in can detecting full constituent, has both avoided widening because of the detecting device peak type causing of connect, passes through again the second chromatographic column secondary separation and SF
6the mode of background gas emptying has solved SF
6the situation of hangover.
Claims (9)
1. a chromatographic analysis system that detects sulfur hexafluoride decomposition product, is characterized in that: comprise sample feeding pipe, sampling valve, the first root chromatogram column, detecting device transfer valve, the second root chromatogram column and four-way switching valve; Wherein, described sampling valve interface I is connected with interface IV, and interface II is communicated with sample feeding pipe, and interface III is connected with atmospheric valve I, and interface V is connected with the first root chromatogram column, and interface VI is connected with sampling valve carrier gas; The interface I of described detecting device transfer valve is communicated with the first root chromatogram column, and interface II connects the first detecting device, the carrier gas of interface III connection detector transfer valve, and interface IV connects a shunt, and described shunt is connected with the second chromatographic column; The interface I of described four-way switching valve connects atmospheric valve IV, and interface II connects the second chromatographic column; Interface III connects the second detecting device, and interface VI connects four-way valve carrier gas.
2. the chromatographic analysis system of detection sulfur hexafluoride decomposition product as claimed in claim 1, is characterized in that: between sampling valve interface I and interface IV, be connected with quantity tube.
3. the chromatographic analysis system of detection sulfur hexafluoride decomposition product as claimed in claim 1, is characterized in that: the first described detecting device is PPD helium ion detector or TCD thermal conductivity detector (TCD).
4. the chromatographic analysis system of detection sulfur hexafluoride decomposition product as claimed in claim 1, is characterized in that: the second described detecting device is PPD helium ion detector or FPD sulfide detecting device.
5. the chromatographic analysis system of detection sulfur hexafluoride decomposition product as claimed in claim 1, is characterized in that: described carrier gas is helium.
6. the chromatographic analysis system of detection sulfur hexafluoride decomposition product as claimed in claim 1, it is characterized in that: the first described chromatographic column is Porapak Q packed column, the second chromatographic column is Gaspro capillary column, and the first chromatographic column is main separation chromatography post, the second chromatographic column is that auxiliary separating is from chromatographic column.
7. the chromatographic analysis system of detection sulfur hexafluoride decomposition product as claimed in claim 1, is characterized in that: the first described detecting device is PPD helium ion detector or TCD thermal conductivity detector (TCD).
8. the chromatographic analysis system of detection sulfur hexafluoride decomposition product as claimed in claim 1, is characterized in that: the second described detecting device is PPD helium ion detector or FPD sulfide detecting device.
9. the analytical approach of the chromatographic analysis system as described in claim as arbitrary in claim 1-8, is characterized in that, as follows:
Before sampling valve does not switch, sample enters quantity tube by sampling valve interface II and sampling valve interface I, and finally emptying via sampling valve interface IV and sampling valve interface III, after switching, carrier gas enters quantity tube and enters the first chromatographic column with sample wherein by sampling valve interface V via sampling valve interface VI and sampling valve interface I and separates for the first time;
Sample after separating for the first time directly enters the first detecting device by detecting device transfer valve interface I and detecting device transfer valve interface II 1 and detects, the gas having detected is discharged by atmospheric valve II, treat first detecting device detect component detect after switch detector transfer valve, the component that goes out peak evening enters shunt by detecting device transfer valve interface I and detecting device transfer valve interface IV in the situation that not entering the first detecting device, sample flow enters the second chromatographic column after being reduced according to the ratio of setting by shunt, separates for the second time;
Sample after secondary separation enters four-way switching valve by four-way switching valve interface II and is discharged and carried out emptying by four-way switching valve interface I again, treats SF
6component emptying is complete, switches four-way switching valve, makes sample enter the second detecting device by four-way switching valve interface II and four-way switching valve interface III and detects, and the gas having detected is discharged from atmospheric valve V.
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| CN104198638B CN104198638B (en) | 2015-11-18 |
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| CN106124670A (en) * | 2016-09-06 | 2016-11-16 | 嘉必优生物技术（武汉）股份有限公司 | A kind of method detecting lycopene |
| CN109085280A (en) * | 2018-10-16 | 2018-12-25 | 广东电网有限责任公司 | A kind of system of quantitative detection sulfur hexafluoride gas ingredient |
| CN109459511A (en) * | 2018-11-14 | 2019-03-12 | 中国南方电网有限责任公司超高压输电公司检修试验中心 | Helium ion detector and subject breaker decomposition product mixed gas separation method |
| CN109633423A (en) * | 2018-11-14 | 2019-04-16 | 中国南方电网有限责任公司超高压输电公司检修试验中心 | A kind of nozzle of circuit breaker ablation status assessing system |
| CN109781867A (en) * | 2017-11-10 | 2019-05-21 | 中国科学院大连化学物理研究所 | A kind of gas-chromatography-ion mobility spectrometry combination device for sulfur hexafluoride decomposer detection |
| CN110726794A (en) * | 2019-10-23 | 2020-01-24 | 朗析仪器（上海）有限公司 | Analysis system for full analysis of decomposition products in sulfur hexafluoride mixed gas |
| CN111679025A (en) * | 2020-04-24 | 2020-09-18 | 中国电力科学研究院有限公司 | Gas chromatography detection system and method for determining gas components of perfluoroisobutyronitrile |
| CN112362766A (en) * | 2020-10-13 | 2021-02-12 | 广西电网有限责任公司电力科学研究院 | System for detecting gas components in sulfur hexafluoride electrical equipment |
| CN114609283A (en) * | 2022-03-16 | 2022-06-10 | 国网安徽省电力有限公司电力科学研究院 | System and method for measuring decomposition products in perfluoroisobutyronitrile |
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| CN106124670B (en) * | 2016-09-06 | 2019-05-10 | 嘉必优生物技术（武汉）股份有限公司 | A method of detection lycopene |
| CN106124670A (en) * | 2016-09-06 | 2016-11-16 | 嘉必优生物技术（武汉）股份有限公司 | A kind of method detecting lycopene |
| CN109781867A (en) * | 2017-11-10 | 2019-05-21 | 中国科学院大连化学物理研究所 | A kind of gas-chromatography-ion mobility spectrometry combination device for sulfur hexafluoride decomposer detection |
| CN109085280B (en) * | 2018-10-16 | 2024-04-12 | 广东电网有限责任公司 | System for quantitatively detecting sulfur hexafluoride gas component |
| CN109085280A (en) * | 2018-10-16 | 2018-12-25 | 广东电网有限责任公司 | A kind of system of quantitative detection sulfur hexafluoride gas ingredient |
| CN109459511A (en) * | 2018-11-14 | 2019-03-12 | 中国南方电网有限责任公司超高压输电公司检修试验中心 | Helium ion detector and subject breaker decomposition product mixed gas separation method |
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| CN110726794A (en) * | 2019-10-23 | 2020-01-24 | 朗析仪器（上海）有限公司 | Analysis system for full analysis of decomposition products in sulfur hexafluoride mixed gas |
| CN111679025A (en) * | 2020-04-24 | 2020-09-18 | 中国电力科学研究院有限公司 | Gas chromatography detection system and method for determining gas components of perfluoroisobutyronitrile |
| CN112362766A (en) * | 2020-10-13 | 2021-02-12 | 广西电网有限责任公司电力科学研究院 | System for detecting gas components in sulfur hexafluoride electrical equipment |
| CN114609283A (en) * | 2022-03-16 | 2022-06-10 | 国网安徽省电力有限公司电力科学研究院 | System and method for measuring decomposition products in perfluoroisobutyronitrile |
| CN114609283B (en) * | 2022-03-16 | 2023-10-27 | 国网安徽省电力有限公司电力科学研究院 | System and method for measuring decomposition products in perfluoroisobutyronitrile |
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