CN104198638B - A kind of chromatographic analysis system and method detecting sulfur hexafluoride decomposition product - Google Patents
A kind of chromatographic analysis system and method detecting sulfur hexafluoride decomposition product Download PDFInfo
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- CN104198638B CN104198638B CN201410413157.7A CN201410413157A CN104198638B CN 104198638 B CN104198638 B CN 104198638B CN 201410413157 A CN201410413157 A CN 201410413157A CN 104198638 B CN104198638 B CN 104198638B
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Abstract
The invention discloses a kind of chromatographic analysis system and the method that detect sulfur hexafluoride decomposition product, 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, interface V is connected with the first root chromatogram column, and interface VI is connected with sampling valve carrier gas; The interface I of 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 shunt is connected with the second chromatographic column; The interface I of 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.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 while can detecting full constituent, avoids because the detecting device peak type caused of connecting is widened and SF
6the situation of hangover.
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 adopt dual-detector detecting pattern, the universal thermal conductivity detector (TCD) of general installation TCD, with sulfide detecting device (such as FPD sulfide detecting device), the former is for the carbon tetrafluoride (CF in 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, general employing detecting device Tandem analysis flow process, namely be that carrier gas enters two detecting devices successively with sample and detects after chromatographic column, 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, such as, fluoridize sulfonyl; Second, under same test condition, appearance time more rearward, then go out peak-to-peak type wider, more not easily detect, owing to being that detecting device adopts series system, sample enters sulfide detecting device again and component peaks type sulfide detecting device going out peak can be caused to widen after high temperature TCD detecting device (temperature of general TCD detecting device reaches more than 250 DEG C), quantitative error is comparatively large, is unfavorable for carrying out trace analysis; Three, SF
6the SF beyond doubt that in decomposition product, content is the highest
6if, SF
6component detects in sulfide detecting device, and its peak height even exceedes detecting device ultimate value (such as FPD detecting device) by very high, thus causes whole spectrogram not easily to carry out integration to little content component, and pole unsightly.
Summary of the invention
In order to solve the problem, the present invention proposes a kind of chromatographic analysis system detecting 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.
Quantity tube is connected with between sampling valve interface I and interface IV.
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 PorapakQ 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
Damping size is reconciled according to requiring.
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 via sampling valve interface IV and sampling valve interface III emptying, after switching, carrier gas enters quantity tube via sampling valve interface VI with sampling valve interface I and enters the first chromatographic column with sample wherein by sampling valve interface V and carries out first time and be separated;
Sample after first time is separated 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 detected is discharged by atmospheric valve II, treat first detecting device detect component detect after switch detector transfer valve, the component going out peak evening enters shunt when not entering the first detecting device by detecting device transfer valve interface I and detecting device transfer valve interface IV, sample flow enters the second chromatographic column after being reduced according to the ratio of setting by shunt, carries out second time and is separated;
Sample after secondary separation enters four-way switching valve by four-way switching valve interface II and carries out emptying by four-way switching valve interface I discharge again, treats SF
6component emptying is complete, switches four-way switching valve, and make sample enter the second detecting device by four-way switching valve interface II and four-way switching valve interface III and detect, the gas detected is from atmospheric valve V discharge.
The invention has the beneficial effects as follows,
After detecting device transfer valve is arranged on the first chromatographic column, sample carrier gas carried is switched to detecting device and shunt on request, all switch into the first detecting device by from the first chromatographic column sample out or all switch to shunt, make second time be separated sample 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 time initial, second chromatographic column is come is in emptying state, namely the second detecting device is not entered, after switching, sample enters the second detecting device, so just can control SF66 go out peak, do not allow SF6 component enter the second detecting device and detect, thus reduce, on the impact of component thereafter, also to make spectrogram more attractive in appearance.
The present invention passes through sampling valve, detecting device transfer valve, and four-way switching valve realizes the switching to sample trend, and shunt and air damping realize controlling the sample size of the second root chromatogram column, finally realizes the first detecting device and detects 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, secondary separation is carried out to not segregative component, main SF
6background gas then carries out emptying process by four-way switching valve.
Accompanying drawing explanation
Fig. 1 stratographic analysis flowage structure figure of the present invention;
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 valves I; 12. first chromatographic columns; 13. connecting lines; 14. detecting device transfer valves; 15. detecting device transfer valve interfaces I; 16. detecting device transfer valve interfaces II; 17. detecting device transfer valve interfaces III; 18. detecting device transfer valve interfaces IV; 19. first detecting devices; 20. atmospheric valves II; 21. shunts; 22. air-flow dampings; 23. atmospheric valves III; 24. second chromatographic columns; 25. four-way switching valves; 26. four-way switching valve interfaces I; 27. four-way switching valve interfaces II; 28. four-way switching valve interfaces III; 29. four-way switching valve interfaces IV; 30. atmospheric valves IV; 31. four-way valve carrier gas; 32. second detecting devices; 33. atmospheric valves 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 end, detecting device transfer valve interface I 15 is connected with the first chromatographic column 12 sample outlet end by connecting line 13, 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, 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, first detecting device 19, air-flow damping 22, four-way switching valve interface I 26, 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 via sampling valve interface IV 8 and sampling valve interface III 7 emptying, after switching, carrier gas 3 enters quantity tube 2 via sampling valve interface VI 10 with sampling valve interface I 5 and enters the first chromatographic column 12 with sample wherein by sampling valve interface V 9 and carries out first time and be separated, and this mainly separates CF
4, CO, CO
2, initial gross separation SF
6, F
2sO
2, F2SO, H
2s etc., sample after first time is separated 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 detected is discharged by atmospheric valve II 20, treat first detecting device 19 detect component detect after switch detector transfer valve 14, the component going out peak evening just enters shunt 21 when having little time to enter first detecting device 19 by detecting device transfer valve interface I 15 and detecting device transfer valve interface IV 18, sample flow enters the second chromatographic column 24 after being reduced according to certain ratio by shunt 21, carry out second time to be separated, second time is separated and contributes to SF
6go out the component at peak from SF later
6impact, the sample after secondary separation by four-way switching valve interface II 27 enter four-way switching valve 25 again by four-way switching valve interface I 26 discharge carry out emptying, treat SF
6component emptying is complete, switches four-way switching valve 25, and be 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, the gas detected is discharged from atmospheric valve V 33.
First detecting device is PPD helium ion detector or TCD thermal conductivity detector (TCD).
Second detecting device is PPD helium ion detector or FPD sulfide detecting device,
Carrier gas is helium.
First chromatographic column is PorapakQ 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 reconcile damping size as requested.
First detecting device can be PPD helium ion detector, also can be TCD thermal conductivity detector (TCD).Second detecting device can be PPD
Helium ion detector, can be also FPD sulfide detecting device, carrier gas used be 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 while can detecting full constituent, has both avoided because the detecting device peak type caused of connect is widened, and has passed through the second chromatographic column secondary separation and SF again
6the mode of background gas emptying solves SF
6the situation of hangover.
Claims (5)
1. detect a chromatographic analysis system for sulfur hexafluoride decomposition product, it is characterized in that: comprise sample feeding pipe, sampling valve, the first chromatographic column, detecting device transfer valve, the second chromatographic 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 chromatographic 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 chromatographic 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; The first described chromatographic column is PorapakQ 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.
2. the chromatographic analysis system detecting 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 detecting 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 detecting 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 detecting sulfur hexafluoride decomposition product as claimed in claim 1, is characterized in that: described carrier gas is helium.
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| CN201410413157.7A CN104198638B (en) | 2014-08-20 | 2014-08-20 | A kind of chromatographic analysis system and method detecting sulfur hexafluoride decomposition product |
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| CN104198638B true CN104198638B (en) | 2015-11-18 |
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