CN104297391B - A kind of chromatographic analysis system - Google Patents

A kind of chromatographic analysis system Download PDF

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Publication number
CN104297391B
CN104297391B CN201410570941.9A CN201410570941A CN104297391B CN 104297391 B CN104297391 B CN 104297391B CN 201410570941 A CN201410570941 A CN 201410570941A CN 104297391 B CN104297391 B CN 104297391B
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China
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perforate
column
way valve
state
chromatographic
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CN201410570941.9A
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Chinese (zh)
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CN104297391A (en
Inventor
周健能
陈鉴祥
简颖涛
杨文远
冯毅明
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佛山市南海区环境保护监测站
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Abstract

The present invention relates to a kind of chromatographic analysis system, be provided with gas chromatograph, it is characterised in that: described chromatographic analysis system farther includes six-way valve;Described gas chromatograph includes the first chromatographic column, damping column, fid detector and injection port;Described six-way valve may be selected to be state one and state two;During detection, described six-way valve is in state one, and sample gas enters from described injection port, delivers to fid detector and detect after flowing through six-way valve, the first chromatographic column and damping column;During blowback, described six-way valve is in state two, and described carrier gas is by, after described six-way valve, flowing through described first chromatographic column in the opposite direction along with the stream of state one, described first chromatographic column is carried out blowback.The chromatographic analysis system of the present invention, analyzes load volume required during sample gas less, saves the consumption of carrier gas, improves the accuracy that sample gas separates.Significantly reduce the pollution of chromatographic column, improve accuracy and the life-span of chromatographic column of sample gas detection.

Description

A kind of chromatographic analysis system
Technical field
The present invention relates to a kind of chromatographic analysis system.
Background technology
Currently for the detection of NMHC, great majority are according to the method described in Chinese Ministry of Environmental Protection standard HJ/T 38-1999 It is analyzed, owing to the component residence time in the chromatography column of the big polarity of the higher boiling in sample gas is longer, easily disturbs next The analysis of individual sample gas, and easily pollute chromatographic column, shortens chromatographic column service life.
Summary of the invention
In view of this, it is necessary to provide a kind of chromatographic analysis system that can improve chromatographic column service life in fact.
The purpose of the present invention is achieved through the following technical solutions:
A kind of chromatographic analysis system, is provided with gas chromatograph, it is characterised in that: described chromatographic analysis system farther includes Six-way valve;Described gas chromatograph includes the first chromatographic column, damping column, fid detector and injection port;Described six-way valve may select For state one and state two;
During detection, described six-way valve is in state one, and sample gas enters from described injection port, flows through six-way valve, along first party After (as shown in Figure 4) flows through described first chromatographic column, damping column, deliver to fid detector detect;
During blowback, described six-way valve is in state two, and described carrier gas is by, after described six-way valve, flowing through institute in a second direction State the first chromatographic column, described first chromatographic column is carried out blowback;Described second direction is opposite to the first direction, when carrier gas edge During second direction (as shown in Figure 5) flowing, the impurity in described first chromatographic column can be removed.Preferably, described six-way valve includes Six perforates, the respectively first perforate, the second perforate, the 3rd perforate, the 4th perforate, the 5th perforate and the 6th perforate;Described One chromatographic column includes first end and relative the second end;Described damping column includes first end and relative the second end; Described injection port is connected with described 6th perforate pipeline;The first end of described first chromatographic column is with described first perforate pipeline even Connect;The second end of described first chromatographic column is connected with described 3rd perforate pipeline;The first end of described damping column is with described Fid detector pipeline connects;The second end of described damping column is respectively with described second perforate, described 4th perforate pipeline even Connect;
During detection, described six-way valve is in described state one;Sample gas enters from described injection port, opens through the described 6th successively Hole, described first perforate, enter from the first end of described first chromatographic column described first chromatographic column separate after, through described Damping column, finally deliver to fid detector and detect;
During blowback, described six-way valve is in state two, and described carrier gas enters from described injection port, flows through the described 6th successively Perforate, described 3rd perforate, after the second end of described first chromatographic column enters described first chromatographic column, successively flow through described First perforate, described second perforate, described damping column, finally entering fid detector will remain in described first chromatographic column Impurity is discharged.
Preferably, can mutually switch between described state one and described state two;Described state one and described state two Between state switching switched over by manually or automatically mode.
Preferably, described first chromatographic column is polarity capillary column, and described damping column is hollow capillary column.
Preferably, described polarity capillary column is alundum (Al2O3) capillary column or molecular sieve capillary column.
Preferably, described sampling device farther includes molecular sieve filtration pipe, and described carrier gas is filtered through molecular sieve filtration pipe After from described injection port enter described six-way valve.
Preferably, described chromatographic analysis system is further provided with ecp assembly;Described ecp assembly is provided with Carrier gas inlet, and be connected with the switching switch pipeline of described six-way valve;Described ecp assembly is used for controlling described six-way valve State switching.
Preferably, described carrier gas flows through the air pressure of described chromatographic analysis system is 80kpa.
The application of a kind of above-mentioned chromatographic analysis system, it is for the detection of NMHC.
Compared with prior art, chromatographic analysis system of the present invention has the advantages that
(1) present invention capillary column replaces traditional packed column, analyzes load volume required during sample gas less, out Chromatogram peak is sharper, it is to avoid conditions of streaking, not only saves the consumption of carrier gas, also improves the accuracy that sample gas separates.
(2) chromatographic analysis system of the present invention is provided with six-way valve, and this six-way valve can flow through chromatographic column by changing carrier gas Direction, thus realize blowing function to chromatographic column, significantly reduce the pollution of chromatographic column, decrease a sample gas remain right The interference that next sample gas is measured, when particularly separating the component of the big polarity of higher boiling, effect is especially apparent, and this improves The accuracy of sample gas detection, extends the life-span of chromatographic column.
Accompanying drawing explanation
Fig. 1 is the structural representation of the quantitative state of chromatographic analysis system sample gas of present pre-ferred embodiments.
Fig. 2 is the structural representation of the chromatographic analysis system detection state of present pre-ferred embodiments.
Fig. 3 is the structural representation of the chromatographic analysis system blowback state of present pre-ferred embodiments.
Fig. 4 is the structural representation of the chromatographic analysis system sample gas detection state of another embodiment of the present invention.
Fig. 5 is the structural representation of the chromatographic analysis system blowback state of another embodiment of the present invention.
Here the component names corresponding to each reference is listed:
400 chromatographic analysis system 310 the tenth openings
100 sampling device 40 first quantitative loop
10 flow controller 50 six-way valves
11 first branch road 511 first perforates
13 second branch road 512 second perforates
30 ten-way valve 513 the 3rd perforates
311 first opening 514 the 4th perforates
312 second opening 515 the 5th perforates
313 the 3rd opening 516 the 6th perforates
314 the 4th opening 60 second quantitative loop
315 the 5th opening 70 molecular sieve filtration pipes
316 the 6th opening 90 ecp assemblies
317 the 7th opening 901 entrances
318 the 8th opening 200 gas chromatographs
319 the 9th opening 210 first chromatographic columns
211 first end 250 damping columns
213 the second end 251 first ends
230 second chromatographic column 253 the second ends
231 first port 270 fid detectors
233 second port 290 injection ports
Detailed description of the invention
As a example by the chromatographic analysis system of the present invention is for detection gas, in the preferred embodiment, should with it It is illustrated as a example by measuring the NMHC in air and waste gas.
As the chromatographic analysis system 400 of Fig. 1 present pre-ferred embodiments includes sampling device 100 and gas chromatograph 200, Described sampling device 100 provides gas to be detected or carrier gas for gas chromatograph 200.Described gas chromatograph 200 includes first Chromatographic column the 210, second chromatographic column 230, damping column 250 and flame ionization ditector (Flame Ionization Detector, fid detector) 270.Described sampling device 100 includes flow controller 10, ten-way valve 30 and six-way valve 50.Inspection During survey, flow through described flow controller 10 carrier gas formed tow channel gas stream respectively after ten-way valve 30, a road air-flow will treat test sample Air-blowing is delivered to FID detector 270 after entering the second chromatographic column 230 and damping column 250 and is detected;Another road air-flow is by sample gas to be measured After damping column 250, deliver to FID detector 270 after being blown into six-way valve 50 and the first chromatographic column 210 detect, it is achieved thereby that Detect while two kinds of components in same sample gas.
Described ten-way valve 30 is used for described first chromatographic column 210 and described second chromatographic column 230 being carried out sample introduction simultaneously, from And realize in single injected sampling, detect two kinds of different components in sample gas, containing of such as detection Determination of Total Hydrocarbon In Atomsphere and methane simultaneously Amount.Described six-way valve 50 is used for controlling gas flow direction, it is achieved from forward, sample gas is delivered to described first chromatographic column 210 and carries out Separate detection, carrier gas is reversely sent into described first chromatographic column 210, described first chromatographic column 210 is carried out blowback, to remove look The sample gas of residual in spectrum post.
Described six-way valve 50 is for controlling the direction of the first chromatographic column 210 described in airflow passes, and forward flows through and carries out sample gas Separate;Flow counterflow through and described first chromatographic column 210 is carried out blowback.The present invention realizes polarity look by increasing six-way valve 50 The sample gas of residual is removed in the blowback of spectrum post, improves the accuracy of sample gas detection, extends the life-span of polarity chromatographic column.
Described flow controller 10 includes the first branch road 11 and the second branch road 13, in the preferred embodiment, institute State the first branch road 11 identical with the air pressure of the second branch road 13.Preferably, the pressure of the first branch road 11 and the second branch road 13 is 80kpa。
Described ten-way valve 30 is provided with ten openings, the respectively the tenth opening the 310, first opening the 311, second opening 312, Three opening the 313, the 4th opening the 314, the 5th opening the 315, the 6th opening the 316, the 7th opening the 317, the 8th openings 318 and the 9th are opened Mouth 319.Described tenth opening 310 is sample gas import, and described 9th opening 319 exports for sample gas.Described second opening 312 and institute Stating the 6th opening 316 is carrier gas inlet.Described first opening 311 is connected by pipeline (figure is not marked) with described 4th opening 314, It is provided with the first quantitative loop 40 on pipeline between described first opening 311 and described 4th opening 314;Described 5th opening 315 are connected by pipeline with described 8th opening 318, the pipeline between described 5th opening 315 and described 8th opening 318 It is provided with the second quantitative loop 60.Described first quantitative loop 40 and described second quantitative loop 60 are for the most temporary sample gas to be measured.
Described ten-way valve 30 has the first state (as shown in Figure 1) and the second state (as shown in Figure 2), described first state And can switch between described second state.Described switching both can manually control, it is also possible to passes through electric controlled pneumatic control Realize.When described ten-way valve 30 is in described first state, sample gas is injected from described tenth opening 310, is flowed through institute successively State the first opening 311, described first quantitative loop 40, described 4th opening 314, described 5th opening 315, described second quantitative loop 60, described 8th opening 318, is finally flowed out by described 9th opening 319, this be sample gas quantitative time air flow direction process, gas Flow path direction is as shown in Fig. 1 direction of arrow.
As in figure 2 it is shown, when described ten-way valve 30 is in described second state, carrier gas is flowed from described flow controller 10 Enter, form two-way gas.One road gas enters described second opening 312 from described first branch road 11, through described first opening 311, the sample gas in described first quantitative loop 40 is taken out of, flow through described 4th opening 314, described 3rd opening 313 successively, enter Enter described second chromatographic column 230 separate after, through described damping column 250, finally enter fid detector and quantitatively detect. Another road gas enters described 6th opening 316 from described second branch road 13, through described 5th opening 315, determines described second Sample gas in amount ring 60 is taken out of, flows through described 8th opening 318, described 7th opening 317, described six-way valve 50 successively, enters After described first chromatographic column 210 separates, through described damping column 250, finally enter fid detector and quantitatively detect.
Described six-way valve 50 is provided with six perforates, the respectively first perforate 511, the second perforate 512, the 3rd perforate 513, and Four perforates 514, the 5th perforate 515 and the 6th perforate 516.Described six-way valve 50 has two states, and respectively state one is (such as figure Shown in 2) and state two (as shown in Figure 3), can mutually switch between described state one and described state two.Described switching action Both can manually control, it is also possible to realized by electric controlled pneumatic control.
As in figure 2 it is shown, described six-way valve 50 is in state one, lead to when air-flow flows into described six from described 7th opening 317 During valve 50, flow through successively described 6th perforate 516, described first perforate 511, forward enter described first chromatographic column 210 carry out After separation, through described damping column 250, finally enter fid detector and quantitatively detect (i.e. detection process air flow direction).Such as figure Shown in 3, described six-way valve 50 is in state two, when air-flow flows into described six-way valve 50 from described 7th opening 317, flows successively Through described 6th perforate 516, described 3rd perforate 513, reversely flow into described first chromatographic column 210, then flow through described the successively One perforate 511, described second perforate 512, described damping column 250, finally enter fid detector and discharge (the most anti-by residuals Blow over journey air flow direction).
Described first chromatographic column 210 includes first end 211 and relative the second end 213.Described second chromatographic column 230 Including the first port 231 and the second relative port 233.Described damping column 250 includes first end 251 and the second relative end Portion 253.In the preferred embodiment, described first chromatographic column 210 is polarity capillary column, and described polarity capillary column is three Al 2 O capillary column or molecular sieve capillary column.Described second chromatographic column 230 and described damping column 250 are hollow capillary Post.For using packed column, when described first chromatographic column 210 and described second chromatographic column 230 are capillary column, inspection Carrier gas consumption required during survey is less, and chromatogram peak out is sharper, it is to avoid conditions of streaking, improves the accurate of sample gas separation Degree.When described six-way valve 50 carries out state switching, the fluid flow in pipeline can be undergone mutation, and described damping column 250 is used for Buffer fluid flow sudden change caused during the switching of described six-way valve 50 state, prevent described fid detector 270 from stopping working.Described Fid detector 270 is for carrying out quantitative analysis to the outflow component after separating.
Described first branch road 11 is connected with described second opening 312 pipeline, described second branch road 13 and described 6th opening 316 pipelines connect.Described 7th opening 317 is connected with described 6th perforate 516 pipeline.The first of described first chromatographic column 210 End 211 is connected with described first perforate 511 pipeline.The second end 213 and described 3rd perforate of described first chromatographic column 210 513 pipelines connect.First port 231 of described second chromatographic column 230 is connected with described 3rd opening 313 pipeline.Described second Second port 233 of chromatographic column 230 respectively with described second perforate 512, described 4th perforate 514, the of described damping column 250 Two end 253 pipelines connect.The first end 251 of described damping column 250 is connected with described fid detector 270 pipeline.
In the preferred embodiment, described sampling device 100 is further provided with molecular sieve filtration pipe 70, carrier gas warp Cross and be delivered to flow controller 10 pipeline after molecule is sieved through the purification of chimney filter 70 and connect.
In the preferred embodiment, described sampling device 100 is further provided with ecp assembly 90.Described electricity Control Pneumatic assembly 90 is provided with carrier gas inlet 901, and is connected with switching switch (not shown) pipeline of described six-way valve 50.When When needing the state switching described six-way valve 50, starting carrier gas, described six-way valve 50 just promotes described six under the air pressure of carrier gas Logical valve 50 switches between described state one and state two.
Sample gas dosing process: as it is shown in figure 1, described ten-way valve 30 is in described first state, sample gas is opened from the described tenth Mouthfuls 310 inject, and flow through described first opening 311, described first quantitative loop 40, described 4th opening 314 successively, the described 5th open Mouth 315, described second quantitative loop 60, described 8th opening 318, finally flowed out by described 9th opening 319, and this is that sample gas is quantitative Time air flow direction process, airflow direction is as shown in Fig. 1 direction of arrow.When full described first quantitative loop 40 and described second is determined During amount ring 60, stop sample introduction, complete dosing process.
Detection process: as in figure 2 it is shown, after quantitatively completing, described ten-way valve 30 is adjusted to described second state, by described Six-way valve 50 adjusts to described state one.Carrier gas, such as nitrogen, after described molecular sieve filtration pipe 70 purifies, through described flow Controller 10, forms two-way gas.One road gas enters described second opening 312 from described first branch road 11, through described first Opening 311, the sample gas in described first quantitative loop 40 is taken out of, flow through described 4th opening 314, described 3rd opening successively 313, enter described second chromatographic column 230 separate after, through described damping column 250, finally enter fid detector and carry out quantitatively Detection.Another road gas enters described 6th opening 316 from described second branch road 13, through described 5th opening 315, by described Sample gas in two quantitative loop 60 is taken out of, flows through described 8th opening 318, described 7th opening 317, described 6th perforate successively 516, described first perforate 511, enters (forward entrance) described first look from the first end 211 of described first chromatographic column 210 After spectrum post 210 separates, through described damping column 250, finally enter fid detector and quantitatively detect.
Blowback process: as it is shown on figure 3, described ten-way valve 30 is still in described second state, described six-way valve 50 is adjusted To state 2.Carrier gas, such as nitrogen, after described molecular sieve filtration pipe 70 purifies, through described flow controller 10, form two-way Gas.One road gas enters described second opening 312 from described first branch road 11, through described first opening 311, by described first Sample gas in quantitative loop 40 is taken out of, flows through described 4th opening 314, described 3rd opening 313 successively, enters described second chromatogram After post 230 separates, through described damping column 250, finally enter fid detector and quantitatively detect.Another road gas is from institute State the second branch road 13 and enter described 6th opening 316, through described 5th opening 315, by the sample gas in described second quantitative loop 60 Take out of, flow through successively described 8th opening 318, described 7th opening 317, described 6th perforate 516, described 3rd perforate 513, After the second end 213 of described first chromatographic column 210 enters (being redirected back into) described first chromatographic column 210, flow through institute successively State the first perforate 511, described second perforate 512, described damping column 250, finally enter fid detector and will remain in described first Impurity in chromatographic column 210 is discharged..
As shown in Figure 4, in another embodiment of the invention, described chromatographic analysis system 400 includes six-way valve 50 and gas Chromatography 200.
Described six-way valve 50 includes six perforates, the respectively first perforate 511, the second perforate 512, the 3rd perforate 513, Four perforates 514, the 5th perforate 515 and the 6th perforate 516.Described six-way valve 50 has two states, and respectively state one is (such as figure Shown in 4) and state two (as shown in Figure 5), can mutually switch between described state one and described state two.Described switching action Both can manually control, it is also possible to realized by electric controlled pneumatic control.
Described gas chromatograph 200 includes the first chromatographic column 210, damping column 250, fid detector 270 and injection port 290. Described first chromatographic column 210 includes first end 211 and relative the second end 213.Described damping column 250 includes first end 251 and relative the second end 253.In the preferred embodiment, described first chromatographic column 210 is polarity capillary column, Described polarity capillary column is alundum (Al2O3) capillary column or molecular sieve capillary column.Described damping column 250 is hollow capillary column.
Described injection port 290 is connected with described 6th perforate 516 pipeline.The first end 211 of described first chromatographic column 210 It is connected with described first perforate 511 pipeline;The second end 213 and described 3rd perforate 513 pipeline of described first chromatographic column 210 Connect.The first end 251 of described damping column 250 is connected with described fid detector pipeline;Second end of described damping column 250 Portion 253 is connected with described second perforate 512, described 4th perforate 514 pipeline respectively.
In the preferred embodiment, described chromatographic analysis system 400 is further provided with molecular sieve filtration pipe 70, carries Gas enters described six-way valve from described injection port after the purification of molecular sieve filtration pipe 70.
In the preferred embodiment, described chromatographic analysis system 400 is further provided with ecp assembly 90.Institute State ecp assembly 90 and be provided with carrier gas inlet 901, and switch (not shown) pipeline even with the switching of described six-way valve 50 Connect.When needing the state switching described six-way valve 50, starting carrier gas, described six-way valve 50 just promotes institute under the air pressure of carrier gas State six-way valve 50 to switch between described state one and state two.
Detection process: as shown in Figure 4, described six-way valve 50 is in described state one.Sample gas is entered from described injection port 290 Enter, successively through described 6th perforate 516, described first perforate 511, enter from the first end 211 of described first chromatographic column 210 After (forward entrance) described first chromatographic column 210 separates, through described damping column 250, finally enter fid detector and carry out determining Amount detection.
Blowback process: as it is shown in figure 5, described six-way valve 50 is in described state two.Carrier gas, such as nitrogen, through described point Son be sieved through chimney filter 70 purify after, flow through successively described injection port 290, described 6th perforate 516, described 3rd perforate 513, from institute State the second end 213 of the first chromatographic column 210 enter (being redirected back into) described first chromatographic column 210 after, flow through described successively One perforate 511, described second perforate 512, described damping column 250, finally enter fid detector and will remain in described first chromatogram Impurity in post 210 is discharged.
The invention is not limited in above-mentioned embodiment, if various changes or deformation to the present invention are without departing from the present invention Spirit and scope, if these are changed and within the scope of deformation belongs to claim or the equivalent technologies of the present invention, then this Bright being also intended to comprises these changes and deformation.

Claims (3)

1. a chromatographic analysis system, is provided with gas chromatograph, it is characterised in that: described chromatographic analysis system farther includes six Logical valve;Described gas chromatograph includes the first chromatographic column, damping column, fid detector and injection port;Described six-way valve may be selected to be State one and state two;Described injection port is connected with a perforate pipeline in described six-way valve;Wherein, described six-way valve includes Six perforates, the respectively first perforate, the second perforate, the 3rd perforate, the 4th perforate, the 5th perforate and the 6th perforate;Described One chromatographic column includes first end and relative the second end;Described damping column includes first end and relative the second end; Described injection port is connected with described 6th perforate pipeline;The first end of described first chromatographic column is with described first perforate pipeline even Connect;The second end of described first chromatographic column is connected with described 3rd perforate pipeline;The first end of described damping column is with described Fid detector pipeline connects;The second end of described damping column is respectively with described second perforate, described 4th perforate pipeline even Connect;Described first chromatographic column is alundum (Al2O3) capillary column or molecular sieve capillary column, and described damping column is hollow capillary column;
During detection, described six-way valve is in state one, and carrier gas drives sample gas to enter from described injection port, flows through the described of six-way valve 6th perforate, described first perforate, flow through the first end of described first chromatographic column, damping column in the first direction after deliver to FID Detector detects;
During blowback, described six-way valve is in state two, and described carrier gas enters from described injection port, described in described six-way valve After 6th perforate, described 3rd perforate, flow through the second end of described first chromatographic column in a second direction, to described first chromatogram Post carries out blowback;Described second direction is opposite to the first direction, after carrier gas flows through described first chromatographic column in a second direction, Flow through described first perforate, described second perforate, described damping column the most successively, finally enter described fid detector and remove described Impurity in first chromatographic column;
Described sampling device farther includes molecular sieve filtration pipe, described carrier gas through molecular sieve filtration pipe filter after from described sample introduction Mouth enters described six-way valve;
It is 80kpa that described carrier gas flows through the air pressure of described chromatographic analysis system.
Chromatographic analysis system the most according to claim 1, it is characterised in that can between described state one and described state two With mutually switching;State switching between described state one and described state two is switched over by manually or automatically mode.
Chromatographic analysis system the most according to claim 1, it is characterised in that described chromatographic analysis system is further provided with electricity Control Pneumatic assembly, described ecp assembly is for controlling the state switching of described six-way valve.
CN201410570941.9A 2014-10-23 2014-10-23 A kind of chromatographic analysis system CN104297391B (en)

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CN105717065B (en) * 2016-04-07 2018-05-22 南京波腾科技工程有限公司 The continuous monitoring device and its method of work of non-methane total hydrocarbons
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