CN104198601A - Chromatographic column parallel-connection analysis device and method thereof - Google Patents

Chromatographic column parallel-connection analysis device and method thereof Download PDF

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Publication number
CN104198601A
CN104198601A CN201410412638.6A CN201410412638A CN104198601A CN 104198601 A CN104198601 A CN 104198601A CN 201410412638 A CN201410412638 A CN 201410412638A CN 104198601 A CN104198601 A CN 104198601A
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China
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chromatographic column
interface
valve
detecting device
sampling valve
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CN201410412638.6A
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CN104198601B (en
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米劲臣
齐国栋
于乃海
李嫱
胥婷
张杏梅
胡小男
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State Grid Corp of China SGCC
Electric Power Research Institute of State Grid Shandong Electric Power Co Ltd
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Abstract

The invention discloses a chromatographic column parallel-connection analysis device and a method thereof. The chromatographic column parallel-connection analysis device comprises a sample feeding pipe, wherein the sample feeding pipe is connected with a first sample feeding valve joint V and a second sample feeding valve joint I; a joint II of the first sample feeding valve is connected with an inlet of a first chromatographic column; a joint VI is connected with a quantifying pipe I in series and subsequently connected with a joint III; a joint IV is connected with a vent valve; the joint I is connected with carrier gas; an outlet of the first chromatographic column is connected with a first detector; a joint II of the second sample feeding valve is connected with a quantifying pipe II in series and subsequently connected with a joint V; a joint III is connected with carrier gas; a joint IV is connected with an inlet of a second chromatographic column; a joint VI is connected with a vent valve III; an outlet of the second chromatographic column is connected with a joint I of a four-way switching valve; a joint II is connected with a vent valve IV; a joint III is connected with carrier gas; a joint IV is connected with a second detector. By virtue of the chromatographic column parallel-connection analysis, the two chromatographic columns are connected with each other in parallel, are separated and are not interfered with each other by one-time sample feeding, so that the broadening of peak pattern caused by the series connection of a plurality of detectors can be avoided; the testing time also can be greatly saved.

Description

A kind of chromatographic column analytical equipment in parallel and method
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 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 a quantity tube, chromatographic column with sample, 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, 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 observing little content component, and the utmost point is not attractive in appearance; The 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 causing is exactly detection time.Existing technical, due at SF 6go out less and the difficult and SF of the component concentration at peak later 6separate, the general mode that adopts secondary separation, an i.e. two root chromatogram columns (packed column, one capillary post) connecting separates, but because two root chromatogram columns are all in same post case, and two kinds of pillars differ greatly to the requirement of column temperature, the control difficulty of post case temperature is very large, and is unfavorable for fast detecting.To sum up, invent a kind of novel can realizing fast SF 6the chromatographic analysis device that decomposition product full constituent detects 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, after interface VI series connection quantity tube I, be 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; After the second described sampling valve interface II series connection quantity tube II, be connected with interface V, 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 the 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, and maximum is 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, the first sampling valve interface IV from the emptying of atmospheric valve I again, meanwhile, sample enters quantity tube II through the second sampling valve interface I and the second sampling valve interface II, then flow through the second sampling valve interface V and the second sampling valve interface VI are from 25 emptying of atmospheric valve III; When sample introduction, the first sampling valve and the second sampling valve switch simultaneously, carrier gas enters respectively the first chromatographic column with quantity tube I and the sample in quantity tube II respectively and separates respectively with the second chromatographic column, and first only control post case and second solely control post case is adjusted column temperature separately to the optimum value that is conducive to separate most; Sample in quantity tube I enters the first detecting device by connecting line after the first chromatographic column separates, detect complete tail gas via the emptying of atmospheric valve II, sample in quantity tube II enters the second detecting device through a four-way switching valve after separating via the second chromatographic column, finally by the emptying of atmospheric valve V; Before four-way switching valve switches, sample, 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 respectively at one time different chromatographic columns and separates, then it detects to enter different detections, before wherein detecting the detecting device of sulfide, connect a four-way valve, two chromatographic columns respectively two can the post case of independent temperature control in.
The invention has the beneficial effects as follows,
Single injected sampling, two root chromatogram columns are in parallel to be separated, do not interfere with each other, both can prevent from widening because of the multi-detector peak type causing of connecting, can save greatly again test period, post case that can independent temperature control can ensure that the residing column temperature of two root chromatogram columns is favourable to the component of each self-separation, and four-way valve can be realized and allow sulfur hexafluoride not enter detecting device to detect, when the perfection of guarantee sulfur hexafluoride and weather separates, also make whole spectrogram seem attractive in appearance.
Brief description of the drawings
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 valve I; 12. first chromatographic columns; 13. first solely control post case; 14. connecting lines; 15. first detecting devices; 16. atmospheric valve II; 17. quantity tube II; 18. second sampling valve interface I; 19. second sampling valve interface II; 20. second sampling valve interface III; 21. second sampling valve interface IV; 22. second sampling valve interface V; 23. second sampling valve interface VI; 24. second sampling valves; 25. atmospheric valve III; 26. second chromatographic columns; 27. second solely control post case; 28. four-way switching valves; 29. four-way switching valve interface I; 30. four-way switching valve interface II; 31. four-way switching valve interface III; 32. four-way switching valve interface IV; 33. atmospheric valve IV; 34. four-way valve auxiliary carrier gas; 35. second detecting devices; 36. atmospheric valve 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 are 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; The first sampling valve interface II is connected with chromatogram the first chromatographic column 12 sample introduction ends, and the first detecting device 15 is connected with the sample outlet end of chromatogram the first chromatographic column 12, and atmospheric valve II 16 is connected with detecting device; Second sampling valve interface IV 21 chromatogram the second chromatographic column 26 sample introduction ends are connected, chromatogram the 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, the first sampling valve interface IV 8 from 11 emptying of atmospheric valve I again, meanwhile, sample enters quantity tube II 17 through the second sampling valve interface I 18 and the second sampling valve interface II 19, then flow through the second sampling valve interface V 22 and the second sampling valve interface VI 23 are from 25 emptying of atmospheric valve III; When sample introduction, the first sampling valve 6 and the second sampling valve 24 switch simultaneously, carrier gas 3 enters respectively the first chromatographic column 12 with quantity tube I 2 and the sample in quantity tube II 17 respectively and separates respectively with the second chromatographic column 26, and first only control post case 13 and second solely control post case 27 is adjusted column temperature separately to the optimum value that is conducive to separate most; Sample in quantity tube I 2 enters the first detecting device 15 by connecting line 14 after the first chromatographic column 12 separates, detect complete tail gas via 16 emptying of atmospheric valve II, sample in quantity tube II 17 enters the second detecting device 35 through a four-way switching valve 28 after separating via the second chromatographic column 26, finally by 36 emptying of atmospheric valve V; Before four-way switching valve 28 switches, sample, in emptying state, enters the second detecting device 35 after switching, can realize SF 6component does not enter the second detecting device and detects.
The first chromatographic column is packed column, and filler can be PorapakQ, does not get rid of other to separating favourable filler; Described the 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, and maximum is no more than 0.25mL.
First solely controls solely control post case of post case and second, and controllable temperature scope is 20 DEG C~280 DEG C, and set temperature is chosen according to experiment condition.
Four-way switching valve 28 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 SF6, 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 first detecting device can be PPD helium ion detector, can be also TCD thermal conductivity detector (TCD).The second described detecting device can be PPD helium ion detector, can be also FPD sulfide detecting device, and carrier gas used is 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, after interface VI series connection quantity tube I, be 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; After the second described sampling valve interface II series connection quantity tube II, be connected with interface V, 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, is characterized in that: the first described detecting device connects an atmospheric valve II, and the second detecting device connects an atmospheric valve V.
3. chromatographic column as claimed in claim 1 analytical equipment in parallel, is characterized in that: the first described chromatographic column is packed column, and filler is PorapakQ.
4. chromatographic column as claimed in claim 1 analytical equipment in parallel, is characterized in that: described the second chromatographic column is Gaspro capillary column.
5. chromatographic column as claimed in claim 1 analytical equipment in parallel, is characterized in that: the volume of quantity tube I is 0.5mL, and the volume of quantity tube II is 0.15mL, and maximum is no more than 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 of 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 chromatographic column analytical equipment in parallel 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, the first sampling valve interface IV from the emptying of atmospheric valve I again, meanwhile, sample enters quantity tube II through the second sampling valve interface I and the second sampling valve interface II, then flow through the second sampling valve interface V and the second sampling valve interface VI are from 25 emptying of atmospheric valve III; When sample introduction, the first sampling valve and the second sampling valve switch simultaneously, carrier gas enters respectively the first chromatographic column with quantity tube I and the sample in quantity tube II respectively and separates respectively with the second chromatographic column, and first only control post case and second solely control post case is adjusted column temperature separately to the optimum value that is conducive to separate most; Sample in quantity tube I enters the first detecting device by connecting line after the first chromatographic column separates, detect complete tail gas via the emptying of atmospheric valve II, sample in quantity tube II enters the second detecting device through a four-way switching valve after separating via the second chromatographic column, finally by the emptying of atmospheric valve V; Before four-way switching valve switches, sample, in emptying state, enters the second detecting device after switching, can realize SF 6component does not enter the second detecting device and detects.
CN201410412638.6A 2014-08-20 2014-08-20 A kind of chromatographic column analytical equipment in parallel and method Active CN104198601B (en)

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
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
CN108603863A (en) * 2015-10-22 2018-09-28 分离系统公司 Analyze the method and system of crude oil front end and crude oil boiling point distribution simultaneously by single gas-chromatography
CN109507321A (en) * 2018-11-28 2019-03-22 浙江博瑞电子科技有限公司 A kind of method of special impurities detection sensitivity in raising high-purity hydrogen chloride

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN108603863A (en) * 2015-10-22 2018-09-28 分离系统公司 Analyze the method and system of crude oil front end and crude oil boiling point distribution simultaneously by single gas-chromatography
CN109507321A (en) * 2018-11-28 2019-03-22 浙江博瑞电子科技有限公司 A kind of method of special impurities detection sensitivity in raising high-purity hydrogen chloride
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

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