CN104198601B - A kind of chromatographic column analytical equipment in parallel and method - Google Patents
A kind of chromatographic column analytical equipment in parallel and method Download PDFInfo
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- CN104198601B CN104198601B CN201410412638.6A CN201410412638A CN104198601B CN 104198601 B CN104198601 B CN 104198601B CN 201410412638 A CN201410412638 A CN 201410412638A CN 104198601 B CN104198601 B CN 104198601B
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Abstract
The invention discloses a kind of chromatographic column analytical equipment in parallel and method, comprise a sample feeding pipe, sample feeding pipe is connected with the second sampling valve interface I with the first sampling valve interface V respectively, the interface II of the first sampling valve is connected with the first chromatographic column entrance, interface VI is connected after quantity tube I and is connected with interface III, interface IV is connected with atmospheric valve, and interface I connects carrier gas; The outlet of the first chromatographic column is connected with the first detecting device; The second described sampling valve interface II is connected after quantity tube II and is connected with interface V, and interface III connects carrier gas, and interface IV connects the entrance of the second chromatographic column; Interface VI connects atmospheric valve III, and the outlet of the second chromatographic column connects the interface I of four-way switching valve, and interface II connects atmospheric valve IV, and interface III connects carrier gas, and interface IV connects the second detecting device.Single injected sampling of the present invention, two root chromatogram columns parallel connections are separated, and do not interfere with each other, and both can prevent from, because the multi-detector peak type caused of connecting is widened, can saving test period greatly again.
Description
Technical field
The present invention relates to a kind of gas chromatographic analysis device, 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 a quantity tube, chromatographic column, but the major defect of this flow process is: 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 observe little content component, and pole unsightly; 4th, the flow process that detecting device is connected even to be had adopts the detection mode of Coupled columns, and it is longer that the result directly caused is exactly detection time.Technically existing, due at SF
6the component concentration later going out peak is less and not easily and SF
6be separated, the mode of general employing secondary separation, an i.e. two root chromatogram columns (packed column, one capillary post) connecting is separated, but because two root chromatogram columns are all in same post case, and two kinds of pillar requirements to column temperature differ greatly, the control difficulty of post case temperature is very large, and is unfavorable for quick detection.To sum up, invent and a kind ofly novel can realize SF fast
6the chromatographic analysis device that decomposition product full constituent carries out detecting is necessary.
Summary of the invention
In order to overcome the above problems, the present invention proposes a kind of chromatographic column analytical equipment in parallel and method.
The technical solution adopted in the present invention is:
A kind of chromatographic column analytical equipment in parallel, comprise a sample feeding pipe, described sample feeding pipe is connected with the second sampling valve interface I with the first sampling valve interface V respectively, the interface II of the first described sampling valve is connected with the first chromatographic column entrance, interface VI is connected after quantity tube I and is connected with interface III, interface IV is connected with atmospheric valve, and interface I connects carrier gas; The outlet of the first described chromatographic column is connected with the first detecting device; The second described sampling valve interface II is connected after quantity tube II and is connected with interface V, and interface III connects carrier gas, and interface IV connects the entrance of the second chromatographic column; Interface VI connects atmospheric valve III, and the outlet of the second chromatographic column connects the interface I of four-way switching valve, and interface II connects atmospheric valve IV, and interface III connects carrier gas, and interface IV connects the second detecting device.
The first described detecting device connects an atmospheric valve II, and the second detecting device connects an atmospheric valve V.
The first described chromatographic column is packed column, and filler is PorapakQ;
Described second chromatographic column is Gaspro capillary column;
The volume of quantity tube I is 0.5mL, and the volume of quantity tube II is 0.15mL, is maximumly no more than 0.25mL.
The first described chromatographic column is arranged on first and solely controls in post case, and the second described chromatographic column is arranged on second and solely controls post case, and controllable temperature scope is 20 DEG C ~ 280 DEG C.
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.
The analytical approach of chromatographic column analytical equipment in parallel is as follows:
Before sample introduction, sample enters quantity tube I through the first sampling valve interface V and the first sampling valve interface VI, flow through the first sampling valve interface III, first sampling valve interface IV again from atmospheric valve I emptying, meanwhile, sample enters quantity tube II through the second sampling valve interface I and the second sampling valve interface II, then flows through the second sampling valve interface V and the second sampling valve interface VI from atmospheric valve III 25 emptying; During sample introduction, first sampling valve and the second sampling valve switch simultaneously, carrier gas enters the first chromatographic column respectively with quantity tube I and the sample in quantity tube II respectively and is separated respectively with the second chromatographic column, and first only control post case and second solely control post case adjusts column temperature separately to the optimum value being conducive to most being separated; Sample in quantity tube I enters the first detecting device by connecting line after the first chromatographic column is separated, detect complete tail gas via atmospheric valve II emptying, sample in quantity tube II enters the second detecting device through a four-way switching valve, finally by atmospheric valve V emptying after being separated via the second chromatographic column; Before four-way switching valve switches, sample is in emptying state, enters the second detecting device after switching, can realize SF
6component does not enter the second detecting device and detects.
The course of work of the present invention is as follows:
Two sampling valves are installed, realize single injected sampling, sample enters different chromatographic columns at one time respectively and is separated, then it detects to enter different detections, connect a four-way valve before wherein detecting the detecting device of sulfide, two chromatographic columns respectively can in the post case of independent temperature control at two.
The invention has the beneficial effects as follows,
Single injected sampling, two root chromatogram column parallel connections are separated, do not interfere with each other, both can prevent because the multi-detector peak type caused of connecting is widened, can save test period greatly again, the post case of independent temperature control can ensure that the component of column temperature to each self-separation residing for two root chromatogram columns is favourable, four-way valve can realize allowing sulfur hexafluoride not enter detecting device and detect, while ensureing that sulfur hexafluoride is separated with the perfection of weather, whole spectrogram is also made to seem attractive in appearance.
Accompanying drawing explanation
Fig. 1 concrete structure figure of the present invention;
In Fig. 1: 1. sample feeding pipe; 2. quantity tube I; 3. carrier gas; 4. the first sampling valve interface I; 5. the first sampling valve interface II; 6. the first sampling valve; 7. the first sampling valve interface III; 8. the first sampling valve interface IV; 9. the first sampling valve interface V; 10. the first sampling valve interface VI; 11. atmospheric valves I; 12. first chromatographic columns; 13. first solely control post case; 14. connecting lines; 15. first detecting devices; 16. atmospheric valves II; 17. quantity tubes II; 18. second sampling valve interfaces I; 19. second sampling valve interfaces II; 20. second sampling valve interfaces III; 21. second sampling valve interfaces IV; 22. second sampling valve interfaces V; 23. second sampling valve interfaces VI; 24. second sampling valves; 25. atmospheric valves III; 26. second chromatographic columns; 27. second solely control post case; 28. four-way switching valves; 29. four-way switching valve interfaces I; 30. four-way switching valve interfaces II; 31. four-way switching valve interfaces III; 32. four-way switching valve interfaces IV; 33. atmospheric valves IV; 34. four-way valve auxiliary carrier gas; 35. second detecting devices; 36. atmospheric valves V.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in detail:
Sample feeding pipe 1 respectively with the first sampling valve interface V 9 is connected with the second sampling valve interface I 18, and belongs in parallel; Quantity tube I 2 one end and the first sampling valve interface VI (being connected), the other end is connected with the first sampling valve interface III 7, and atmospheric valve I 11 is connected with the first sampling valve interface IV 8; Quantity tube II 17 one end is connected with the second sampling valve interface II 19, and the other end is connected with the second sampling valve interface V 22, and atmospheric valve III 25 is connected with the second sampling valve interface VI 23; First sampling valve interface II is connected with chromatogram first chromatographic column 12 sample introduction end, and the first detecting device 15 is connected with the sample outlet end of chromatogram first chromatographic column 12, and atmospheric valve II 16 is connected with detecting device; Second sampling valve interface IV 21 chromatogram second chromatographic column 26 sample introduction end is connected, chromatogram second chromatographic column sample outlet end is connected with four-way switching valve interface I 29, atmospheric valve IV 33 is connected with four-way switching valve interface II 30, four-way valve auxiliary carrier gas 34 is connected into four-way switching valve interface III 31, four-way switching valve interface IV 32 is connected with the second detecting device 35, and atmospheric valve V 36 is connected with the second detecting device 35.
Before sample introduction, sample enters quantity tube I 2 through the first sampling valve interface V 9 and the first sampling valve interface VI 10, flow through the first sampling valve interface III 7, first sampling valve interface IV 8 again from atmospheric valve I 11 emptying, meanwhile, sample enters quantity tube II 17 through the second sampling valve interface I 18 and the second sampling valve interface II 19, then flows through the second sampling valve interface V 22 and the second sampling valve interface VI 23 from atmospheric valve III 25 emptying; During sample introduction, first sampling valve 6 and the second sampling valve 24 switch simultaneously, carrier gas 3 enters the first chromatographic column 12 respectively with quantity tube I 2 and the sample in quantity tube II 17 respectively and is separated respectively with the second chromatographic column 26, and first solely controls post case 13 and second only optimum value controlled the respective adjustment column temperature of post case 27 and be extremely conducive to most being separated; Sample in quantity tube I 2 enters the first detecting device 15 by connecting line 14 after the first chromatographic column 12 is separated, detect complete tail gas via atmospheric valve II 16 emptying, sample in quantity tube II 17 enters the second detecting device 35 through a four-way switching valve 28, finally by atmospheric valve V 36 emptying after being separated via the second chromatographic column 26; Before four-way switching valve 28 switches, sample is in emptying state, enters the second detecting device 35, can realize SF after switching
6component does not enter the second detecting device and detects.
First chromatographic column is packed column, and filler can be PorapakQ, does not get rid of other to being separated favourable filler; Described second chromatographic column is Gaspro capillary column, does not get rid of other effective capillary columns.Corresponding, the volume of quantity tube I is 0.5mL, and the volume of quantity tube II is 0.15mL, is maximumly no more than 0.25mL.
First solely controls post case and second solely control post case, and controllable temperature scope is 20 DEG C ~ 280 DEG C, and set temperature experimentally condition is chosen.
Four-way switching valve 28 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 SF6 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.
First detecting device can be PPD helium ion detector, also can be TCD thermal conductivity detector (TCD).The second described detecting device can be PPD helium ion detector, and can be also FPD sulfide detecting device, carrier gas used be helium.
Claims (10)
1. a chromatographic column analytical equipment in parallel, it is characterized in that: comprise a sample feeding pipe, described sample feeding pipe is connected with the second sampling valve interface I with the first sampling valve interface V respectively, the interface II of the first described sampling valve is connected with the first chromatographic column entrance, interface VI is connected after quantity tube I and is connected with interface III, interface IV is connected with atmospheric valve, and interface I connects carrier gas; The outlet of the first described chromatographic column is connected with the first detecting device; The second described sampling valve interface II is connected after quantity tube II and is connected with interface V, and interface III connects carrier gas, and interface IV connects the entrance of the second chromatographic column; Interface VI connects atmospheric valve III, and the outlet of the second chromatographic column connects the interface I of four-way switching valve, and interface II connects atmospheric valve IV, and interface III connects carrier gas, and interface IV connects the second detecting device.
2. chromatographic column as claimed in claim 1 analytical equipment in parallel, it is characterized in that: the first described detecting device connects an atmospheric valve II, the second detecting device connects an atmospheric valve V.
3. chromatographic column as claimed in claim 1 analytical equipment in parallel, it is characterized in that: the first described chromatographic column is packed column, filler is PorapakQ.
4. chromatographic column as claimed in claim 1 analytical equipment in parallel, is characterized in that: described second chromatographic column is Gaspro capillary column.
5. chromatographic column as claimed in claim 1 analytical equipment in parallel, it is characterized in that: the volume of quantity tube I is 0.5mL, the volume of quantity tube II is 0.15 ~ 0.25mL.
6. chromatographic column as claimed in claim 1 analytical equipment in parallel, it is characterized in that: the first described chromatographic column is arranged on first and solely controls in post case, the second described chromatographic column is arranged on second and solely controls post case, and the first controllable temperature scope solely controlling post case and second only control post case is 20 DEG C ~ 280 DEG C.
7. chromatographic column as claimed in claim 1 analytical equipment in parallel, is characterized in that: the first described detecting device is PPD helium ion detector, or TCD thermal conductivity detector (TCD).
8. chromatographic column as claimed in claim 1 analytical equipment in parallel, is characterized in that: the second described detecting device is PPD helium ion detector, or FPD sulfide detecting device.
9. chromatographic column as claimed in claim 1 analytical equipment in parallel, is characterized in that: carrier gas used is helium.
10. the analytical approach of the analytical equipment in parallel of the chromatographic column as described in as arbitrary in claim 1-9, is characterized in that, as follows:
Before sample introduction, sample enters quantity tube I through the first sampling valve interface V and the first sampling valve interface VI, flow through the first sampling valve interface III, first sampling valve interface IV again from atmospheric valve I emptying, meanwhile, sample enters quantity tube II through the second sampling valve interface I and the second sampling valve interface II, then flows through the second sampling valve interface V and the second sampling valve interface VI from atmospheric valve III 25 emptying; During sample introduction, first sampling valve and the second sampling valve switch simultaneously, carrier gas enters the first chromatographic column respectively with quantity tube I and the sample in quantity tube II respectively and is separated respectively with the second chromatographic column, and first only control post case and second solely control post case adjusts column temperature separately to the optimum value being conducive to most being separated; Sample in quantity tube I enters the first detecting device by connecting line after the first chromatographic column is separated, detect complete tail gas via atmospheric valve II emptying, sample in quantity tube II enters the second detecting device through a four-way switching valve, finally by atmospheric valve V emptying after being separated via the second chromatographic column; Before four-way switching valve switches, sample is in emptying state, enters the second detecting device after switching, can realize SF
6component does not enter the second detecting device and detects.
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| CN201410412638.6A CN104198601B (en) | 2014-08-20 | 2014-08-20 | A kind of chromatographic column analytical equipment in parallel and method |
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| CN201410412638.6A CN104198601B (en) | 2014-08-20 | 2014-08-20 | A kind of chromatographic column analytical equipment in parallel and method |
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| CN104198601B true CN104198601B (en) | 2015-11-18 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105353048A (en) * | 2015-09-23 | 2016-02-24 | 南京白云化工环境监测有限公司 | Device and method for determination of non-methane total hydrocarbon by gas chromatographic analysis |
| US10466224B2 (en) * | 2015-10-22 | 2019-11-05 | Separation Systems, Inc. | Method and system for contemporaneous analysis of a crude oil front end and a crude oil boiling point distribution via a single gas chromatograph |
| CN108732277A (en) * | 2018-07-31 | 2018-11-02 | 瑞丽中检检验认证有限公司 | The detection device and its detection method of total sulfur and sulfide in a kind of natural gas |
| 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 |
| CN109507321B (en) * | 2018-11-28 | 2021-03-16 | 浙江博瑞电子科技有限公司 | Method for improving detection sensitivity of special impurities in high-purity hydrogen chloride |
| 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 |
| CN115201343A (en) * | 2021-04-09 | 2022-10-18 | 株式会社岛津制作所 | Continuous monitoring device |
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