CN104280486B - A kind of chromatogram analysis method - Google Patents
A kind of chromatogram analysis method Download PDFInfo
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- CN104280486B CN104280486B CN201410573078.2A CN201410573078A CN104280486B CN 104280486 B CN104280486 B CN 104280486B CN 201410573078 A CN201410573078 A CN 201410573078A CN 104280486 B CN104280486 B CN 104280486B
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- 238000004458 analytical method Methods 0.000 title claims abstract description 26
- 239000007789 gas Substances 0.000 claims abstract description 97
- 238000013016 damping Methods 0.000 claims abstract description 53
- 239000012159 carrier gas Substances 0.000 claims abstract description 48
- 238000005070 sampling Methods 0.000 claims abstract description 31
- 238000001514 detection method Methods 0.000 claims abstract description 25
- 239000012530 fluid Substances 0.000 claims abstract description 5
- 239000002808 molecular sieve Substances 0.000 claims description 20
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 20
- 238000001914 filtration Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 13
- 230000008569 process Effects 0.000 claims description 12
- 230000008676 import Effects 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 abstract description 2
- 238000004587 chromatography analysis Methods 0.000 description 12
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000002347 injection Methods 0.000 description 6
- 239000007924 injection Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 230000000712 assembly Effects 0.000 description 1
- 238000000429 assembly Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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Abstract
The present invention relates to a kind of chromatogram analysis method, it adopts gas chromatograph and sampling device, and described sampling device provides fluid to be detected for gas chromatograph, and described gas chromatograph includes the first chromatographic column, the second chromatographic column, damping column and fid detector；Described sampling device includes ten-way valve and six-way valve, and described six-way valve may be selected to be state one and state two, and described ten-way valve may be selected to be the first state and the second state, described chromatogram analysis method include sample gas quantitatively, detection and blowback step.The chromatogram analysis method of the present invention has the advantage that the consumption saving carrier gas, also improves the degree of accuracy that sample gas separates；Improve the degree of accuracy of sample gas detection, improve the life-span of chromatographic column；Measure two kinds of different materials of same sample gas simultaneously, substantially increase work efficiency.
Description
Technical field
The present invention relates to a kind of chromatogram analysis method.
Background technology
At present, detection for NMHC, great majority method described in Chinese Ministry of Environmental Protection standard HJ/T38-1999 is analyzed, owing to the component residence time in the chromatography column of the big polarity of the high boiling point in sample gas is longer, the easily analysis of the next sample gas of interference, and easily pollute chromatographic column, shorten chromatographic column service life.
Summary of the invention
In view of this, it is necessary to provide a kind of single injected sampling can measure two kinds of compositions simultaneously and improve the chromatogram analysis method in chromatographic column service life in fact.
The purpose of the present invention is achieved through the following technical solutions:
A kind of chromatogram analysis method, adopts gas chromatograph and sampling device, and described sampling device provides fluid to be detected for gas chromatograph, and described gas chromatograph includes the first chromatographic column, the second chromatographic column, damping column and fid detector；Described sampling device includes ten-way valve and six-way valve, and described six-way valve may be selected to be state one and state two, and described ten-way valve may be selected to be the first state and the second state, and described chromatogram analysis method comprises the following steps:
Sample gas is quantitative: make described ten-way valve be in described first state, sample gas to be measured is injected described ten-way valve and carries out quantitatively；
Detection: make described ten-way valve be in the second state, described six-way valve is in state one, carrier gas divides two-way to enter described ten-way valve, two-way is divided to take out of sample gas to be measured, one road flows through the second chromatographic column and damping column is delivered to fid detector and detected, another road flows through six-way valve successively, (as shown in Figure 2) flow through the first chromatographic column, damping column in the first direction after, deliver to fid detector and detect；
Blowback: making described ten-way valve be in the second state, described six-way valve is in state two, described carrier gas is by, after described six-way valve, (as shown in Figure 3) flowing through described first chromatographic column in a second direction, described first chromatographic column is carried out blowback；Described second direction is opposite to the first direction, when carrier gas is flowed in a second direction, can remove the impurity in described first chromatographic column.
Preferably, described sampling device farther includes flow controller, and carrier gas is divided into the first branch road and the second branch road by described flow controller, and described first branch road and the second branch road are connected with ten-way valve respectively through pipeline.
Preferably, described ten-way valve is provided with ten openings, respectively the tenth opening, the first opening, the second opening, the 3rd opening, the 4th opening, the 5th opening, the 6th opening, the 7th opening, the 8th opening and the 9th opening, described tenth opening is sample gas import to be measured, and described 9th opening is sample gas to be measured outlet；Described second opening and described 6th opening are carrier gas inlet；Described first opening is connected by pipeline with described 4th opening, and described 5th opening is connected by pipeline with described 8th opening；Described first branch road is connected with described second opening line, and described second branch road is connected with described 6th opening.
Preferably, described sampling device includes the first quantitative loop for quantitatively keeping in sample gas to be detected and the second quantitative loop, and described first quantitative loop is located on the pipeline between the first opening and described 4th opening；Described second quantitative loop is located on the pipeline between described 5th opening and described 8th opening.
Preferably, described six-way valve is provided with six perforates, respectively the first perforates, the second perforate, the 3rd perforate, the 4th perforate, the 5th perforate and the 6th perforate；Described 7th opening is connected with described 6th perforate pipeline, and described first chromatographic column includes first end and relative the second end, and described second chromatographic column includes the first port and the second relative port, and described damping column includes first end and relative the second end；The first end of described first chromatographic column is connected with described first perforate pipeline；The second end of described first chromatographic column is connected with described 3rd perforate pipeline；First port of described second chromatographic column is connected with described 3rd opening conduit；Second port of described second chromatographic column respectively with described second perforate, described 4th perforate, described damping column the second end pipeline be connected；The first end of described damping column is connected with described fid detector pipeline.
Preferably, described sampling device farther includes molecular sieve filtration pipe, and described carrier gas filters laggard inbound traffics controller through molecular sieve filtration pipe.
Preferably, the state switching of described six-way valve is switched over by manually or automatically mode.
Preferably, described first chromatographic column is polarity capillary column, and described polarity capillary column is aluminium sesquioxide capillary column or molecular sieve capillary column；Described second chromatographic column and described damping column are hollow capillary column.
A kind of chromatogram analysis method, adopts gas chromatograph and sampling device, and described sampling device provides sample gas to be detected for described gas chromatograph, and described gas chromatograph includes the first chromatographic column, the second chromatographic column, damping column and fid detector；
Described sampling device includes flow controller, ten-way valve, six-way valve, the first quantitative loop and the second quantitative loop；
Carrier gas is divided into the first branch road and the second branch road by described flow controller, and the sample gas in the first quantitative loop and the second quantitative loop is taken out of by the carrier gas of described first branch road and the second branch road respectively；
Described ten-way valve is provided with ten openings, respectively the tenth opening, the first opening, the second opening, the 3rd opening, the 4th opening, the 5th opening, the 6th opening, the 7th opening, the 8th opening and the 9th opening, described tenth opening is sample gas import to be measured, described 9th opening is sample gas to be measured outlet, and described second opening and described 6th opening are carrier gas inlet；Described first opening is connected by pipeline with described 4th opening, and described first quantitative loop is series on the pipeline between the first opening and described 4th opening；Described 5th opening is connected by pipeline with described 8th opening, and described second quantitative loop is series on the pipeline between described 5th opening and described 8th opening；Described first branch road and the second opening connect, and described second branch road and the 6th opening connect；Described ten-way valve may be selected to be the first state and the second state；
Described six-way valve is provided with six perforates, respectively the first perforates, the second perforate, the 3rd perforate, the 4th perforate, the 5th perforate and the 6th perforate, and described 7th opening is connected with described 6th perforate pipeline；Described six-way valve may be selected to be state one and state two；
Described first chromatographic column includes first end and relative the second end, and described second chromatographic column includes the first port and the second relative port, and described damping column includes first end and relative the second end；The first end of described first chromatographic column is connected with described first perforate pipeline；The second end of described first chromatographic column is connected with described 3rd perforate pipeline；First port of described second chromatographic column is connected with described 3rd opening conduit；Second port of described second chromatographic column respectively with described second perforate, described 4th perforate, described damping column the second end pipeline be connected；The first end of described damping column is connected with described fid detector pipeline；Described chromatogram analysis method comprises the steps:
Sample gas is quantitative: allow described ten-way valve be in described first state, sample gas injects from described tenth opening, flow through described first opening, described first quantitative loop, described 4th opening, described 5th opening, described second quantitative loop, described 8th opening successively, last by described 9th opening outflow, when full described first quantitative loop and described second quantitative loop, stop sample introduction, complete dosing process.
Detection: make described ten-way valve be in the second state, described six-way valve is in the first state, the carrier gas of described first branch road flows through the first opening after entering described ten-way valve the second opening successively, first quantitative loop, 4th opening, 3rd opening, after second chromatographic column and damping column, deliver to fid detector to detect, the carrier gas of described second branch road flows through the 5th opening after entering the 6th opening successively, second quantitative loop, 8th opening, 7th opening, 6th perforate of described six-way valve, first perforate, first end along the first chromatographic column enters described first chromatographic column, 3rd perforate, deliver to fid detector after 4th perforate and damping column to detect；
Blowback: making described ten-way valve be in the second state, described six-way valve is in the second state, described carrier gas is by after described six-way valve, and the second end along described first chromatographic column flows through described first chromatographic column, and described first chromatographic column is carried out blowback.
Preferably, described sampling device farther includes molecular sieve filtration pipe, and described carrier gas filters laggard inbound traffics controller through molecular sieve filtration pipe.
Compared with prior art, chromatogram analysis method of the present invention has the advantages that
(1) chromatogram analysis method of the present invention, analyzes load volume required during sample gas less, and chromatogram peak out is sharper, does not have conditions of streaking, not only saves the consumption of carrier gas, also improves the degree of accuracy that sample gas separates.
(2) chromatogram analysis method of the present invention adopts six-way valve, this six-way valve can flow through the direction of chromatographic column by changing carrier gas, thus realizing the blowing function to chromatographic column, significantly reduce the pollution of chromatographic column, decrease the interference that next sample gas is measured by a sample gas residual, when particularly separating the component of the big polarity of high boiling point, effect is especially apparent, this improves the degree of accuracy of sample gas detection, extend the life-span of chromatographic column.
(3) additionally, chromatogram analysis method of the present invention also applies ten-way valve, thus realize measuring two kinds of different materials of same sample gas simultaneously, work efficiency is substantially increased.
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 each component names corresponding to accompanying drawing labelling is listed:
400 chromatographic analysis system 512 second perforates
100 sampling device 513 the 3rd perforates
10 flow controller 514 the 4th perforates
11 first branch road 515 the 5th perforates
13 second branch road 516 the 6th perforates
30 ten-way valve 60 second quantitative loop
311 first opening 70 molecular sieve filtration pipes
312 second opening 90 ecp assemblies
313 the 3rd opening 901 entrances
314 the 4th opening 200 gas chromatograpies
315 the 5th opening 210 first chromatographic columns
316 the 6th opening 211 first ends
317 the 7th opening 213 the second ends
318 the 8th opening 230 second chromatographic columns
319 the 9th opening 231 first ports
310 the tenth opening 233 second ports
40 first quantitative loop 250 damping columns
50 six-way valve 251 first ends
511 first perforate 253 the second ends
270 fid detector 290 injection ports
Detailed description of the invention
The chromatographic analysis system of the present invention is example for detected gas, in the preferred embodiment, is illustrated for the NMHC that it is applied to measure in air and waste gas.
Chromatographic analysis system 400 such as Fig. 1 present pre-ferred embodiments includes sampling device 100 and gas chromatograph 200, and 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 (FlameIonizationDetector, fid detector) 270.Described sampling device 100 includes flow controller 10, ten-way valve 30 and six-way valve 50.During detection, the carrier gas flowing through described flow controller 10 forms tow channel gas stream respectively after ten-way valve 30, and a road air-flow is delivered to FID detector 270 after sample gas to be measured is blown into the second chromatographic column 230 and damping column 250 and detected；Another road air-flow is delivered to FID detector 270 after damping column 250 after sample gas to be measured is blown into six-way valve 50 and the first chromatographic column 210 and is detected, it is achieved thereby that detect while two kinds of components in same sample gas.
Described ten-way valve 30 is for carrying out sample introduction to described first chromatographic column 210 and described second chromatographic column 230 simultaneously, thus realize the two kinds of different components detecting in sample gas in single injected sampling simultaneously, for instance the content of detection Determination of Total Hydrocarbon In Atomsphere and methane.Described six-way valve 50 is used for controlling gas flow direction, realize that sample gas is delivered to described first chromatographic column 210 from forward and be easily separated detection, carrier gas is reversely sent into described first chromatographic column 210, described first chromatographic column 210 is carried out blowback, to remove the sample gas of residual in chromatographic column.
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 separation；Flow counterflow through and described first chromatographic column 210 is carried out blowback.The present invention realizes the sample gas of the removing residual of the blowback to polarity chromatographic column by increasing six-way valve 50, improves the degree of 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, and in the preferred embodiment, described first branch road 11 is 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, respectively the tenth opening the 310, first opening the 311, second opening the 312, the 3rd 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 opening 318 and the 9th opening 319.Described tenth opening 310 is sample gas import, and described 9th opening 319 exports for sample gas.Described second opening 312 and described 6th opening 316 are carrier gas inlet.Described first opening 311 is connected by pipeline (figure does not mark) with described 4th opening 314, and the pipeline between described first opening 311 and described 4th opening 314 is provided with the first quantitative loop 40；Described 5th opening 315 is connected by pipeline with described 8th opening 318, and the pipeline between described 5th opening 315 and described 8th opening 318 is provided with the second quantitative loop 60.Described first quantitative loop 40 and described second quantitative loop 60 are for quantitatively 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), can switch between described first state and described second state.Described switching both can manually control, it is also possible to is realized by electric controlled pneumatic control.When described ten-way valve 30 is in described first state, sample gas injects from described tenth opening 310, flow through described 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 successively, finally flowed out by described 9th opening 319, this be sample gas quantitative time air flow direction process, airflow direction is such 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 flows into from 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, the sample gas in described first quantitative loop 40 is taken out of, after flowing through described 4th opening 314, described 3rd opening 313 successively, entering described second chromatographic column 230 and be easily separated, through described damping column 250, finally enter fid detector and carry out detection by quantitative.Another road gas enters described 6th opening 316 from described second branch road 13, through described 5th opening 315, the sample gas in described second quantitative loop 60 is taken out of, after flowing through described 8th opening 318, described 7th opening 317, described six-way valve 50 successively, entering described first chromatographic column 210 and be easily separated, through described damping column 250, finally enter fid detector and carry out detection by quantitative.
Described six-way valve 50 is provided with six perforates, respectively the first perforate 511, the second perforate 512, the 3rd perforate 513, the 4th perforate 514, the 5th perforate 515 and the 6th perforate 516.Described six-way valve 50 has two states, and respectively state one (as shown in Figure 2) and state two (as shown in Figure 3), can switch between described state one and described state two mutually.Described switching action both can manually control, it is also possible to is realized by electric controlled pneumatic control.
As shown in Figure 2, described six-way valve 50 is in state one, when air-flow flows into described six-way valve 50 from described 7th opening 317, flow through described 6th perforate 516 successively, described first perforate 511, forward enter after described first chromatographic column 210 is easily separated, through described damping column 250, finally enter fid detector and carry out detection by quantitative (i.e. detection process air flow direction).As shown in Figure 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, flow through described 6th perforate 516, described 3rd perforate 513, reversely described first chromatographic column 210 of inflow successively, flow through described first perforate 511, described second perforate 512, described damping column 250 more successively, finally enter fid detector and residuals is discharged (i.e. blowback process air flow direction).
Described first chromatographic column 210 includes first end 211 and relative the second end 213.Described second chromatographic column 230 includes the first port 231 and the second relative port 233.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, and described polarity capillary column is aluminium sesquioxide capillary column or molecular sieve capillary column.Described second chromatographic column 230 and described damping column 250 are hollow capillary column.For using packed column, when described first chromatographic column 210 and described second chromatographic column 230 are capillary column, carrier gas consumption required during detection is less, and chromatogram peak out is sharper, it is to avoid conditions of streaking, improves the degree of accuracy that sample gas separates.When described six-way valve 50 carries out state switching, the fluid flow in pipeline can be undergone mutation, and fluid flow caused when described damping column 250 is for cushioning the switching of described six-way valve 50 state suddenlys change, it is prevented that described fid detector 270 stops 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, and described second branch road 13 is connected with described 6th opening 316 pipeline.Described 7th opening 317 is connected with described 6th perforate 516 pipeline.The first end 211 of described first chromatographic column 210 is connected with described first perforate 511 pipeline.The second end 213 of described first chromatographic column 210 is connected with described 3rd perforate 513 pipeline.First port 231 of described second chromatographic column 230 is connected with described 3rd opening 313 pipeline.Second port 233 of described second chromatographic column 230 respectively with described second perforate 512, described 4th perforate 514, described damping column 250 the second end 253 pipeline be connected.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, and carrier gas is delivered to flow controller 10 pipeline after the purification of molecular sieve filtration pipe 70 and connects.
In the preferred embodiment, described sampling device 100 is further provided with ecp assembly 90.Described ecp assembly 90 is provided with carrier gas inlet 901, and switchs (not shown go out) pipeline with the switching of described six-way valve 50 and be connected.When needing the state switching described six-way valve 50, starting carrier gas, described six-way valve 50 just promotes described six-way valve 50 to switch between described state one and state two under the air pressure of carrier gas.
Sample gas dosing process: as shown in Figure 1, described ten-way valve 30 is in described first state, sample gas injects from described tenth opening 310, flow through described 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 successively, finally flowed out by described 9th opening 319, this be sample gas quantitative time air flow direction process, airflow direction is such as shown in Fig. 1 direction of arrow.When full described first quantitative loop 40 and described second quantitative loop 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, described six-way valve 50 is adjusted to described state one.Carrier gas, for instance 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, after flowing through described 4th opening 314, described 3rd opening 313 successively, entering described second chromatographic column 230 and be easily separated, through described damping column 250, finally enter fid detector and carry out detection by quantitative.Another road gas enters described 6th opening 316 from described second branch road 13, through described 5th opening 315, the sample gas in described second quantitative loop 60 is taken out of, flow through described 8th opening 318, described 7th opening 317, described 6th perforate 516, described first perforate 511 successively, enter after (forward entrance) described first chromatographic column 210 is easily separated from the first end 211 of described first chromatographic column 210, through described damping column 250, finally enter fid detector and carry out detection by quantitative.
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, for instance 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, after flowing through described 4th opening 314, described 3rd opening 313 successively, entering described second chromatographic column 230 and be easily separated, through described damping column 250, finally enter fid detector and carry out detection by quantitative.Another road gas enters described 6th opening 316 from described second branch road 13, through described 5th opening 315, sample gas in described second quantitative loop 60 is taken out of, flow through described 8th opening 318 successively, described 7th opening 317, described 6th perforate 516, described 3rd perforate 513, after entering (being redirected back into) described first chromatographic column 210 from the second end 213 of described first chromatographic column 210, flow through described first perforate 511 successively, described second perforate 512, described damping column 250, finally enter fid detector to be discharged by the impurity remained in described first chromatographic column 210..
As shown in Figure 4, in another embodiment of the invention, described chromatographic analysis system 400 includes six-way valve 50 and gas chromatograph 200.
Described six-way valve 50 includes six perforates, respectively the first perforate 511, the second perforate 512, the 3rd perforate 513, the 4th perforate 514, the 5th perforate 515 and the 6th perforate 516.Described six-way valve 50 has two states, and respectively state one (as shown in Figure 4) and state two (as shown in Figure 5), can switch between described state one and described state two mutually.Described switching action both can manually control, it is also possible to is 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, and described polarity capillary column is aluminium sesquioxide 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 is connected with described first perforate 511 pipeline；The second end 213 of described first chromatographic column 210 is connected with described 3rd perforate 513 pipeline.The first end 251 of described damping column 250 is connected with described fid detector pipeline；The second end 253 of described damping column 250 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, and carrier 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.Described ecp assembly 90 is provided with carrier gas inlet 901, and switchs (not shown go out) pipeline with the switching of described six-way valve 50 and be connected.When needing the state switching described six-way valve 50, starting carrier gas, described six-way valve 50 just promotes described six-way valve 50 to switch between described state one and state two under the air pressure of carrier gas.
Detection process: as shown in Figure 4, described six-way valve 50 is in described state one.Sample gas enters from described injection port 290, successively through described 6th perforate 516, described first perforate 511, enter after (forward entrance) described first chromatographic column 210 is easily separated from the first end 211 of described first chromatographic column 210, through described damping column 250, finally enter fid detector and carry out detection by quantitative.
Blowback process: as it is shown in figure 5, described six-way valve 50 is in described state two.Carrier gas, such as nitrogen, after described molecular sieve filtration pipe 70 purifies, flow through described injection port 290 successively, described 6th perforate 516, described 3rd perforate 513, the second end 213 from described first chromatographic column 210 enter (being redirected back into) described first chromatographic column 210 after, flow through described first perforate 511, described second perforate 512, described damping column 250 successively, finally enter the impurity that fid detector will remain in described first chromatographic column 210 and discharge.
The invention is not limited in above-mentioned embodiment, if to the various changes of the present invention or deformation without departing from the spirit and scope of the present invention, if these are changed and deform within the claim or the equivalent technologies scope that belong to the present invention, then the present invention is also intended to comprise these changes and deformation.
Claims (8)
1. a chromatogram analysis method, it is characterised in that: adopting gas chromatograph and sampling device, described sampling device provides fluid to be detected for gas chromatograph, and described gas chromatograph includes the first chromatographic column, the second chromatographic column, damping column and fid detector；Described sampling device includes ten-way valve and six-way valve, and described six-way valve may be selected to be state one and state two, and described ten-way valve may be selected to be the first state and the second state, and described chromatogram analysis method comprises the following steps:
Sample gas is quantitative: make described ten-way valve be in described first state, sample gas to be measured is injected described ten-way valve and carries out quantitatively；
Detection: make described ten-way valve be in the second state, described six-way valve is in state one, carrier gas divides two-way to enter described ten-way valve, two-way is divided to take out of sample gas to be measured, after one road flows through the second chromatographic column, damping column, deliver to fid detector to detect, another road flows through six-way valve successively, flow through the first chromatographic column and damping column in the first direction after, deliver to fid detector and detect；
Blowback: making described ten-way valve be in the second state, described six-way valve is in state two, described carrier gas is by, after described six-way valve, flowing through described first chromatographic column in a second direction, described first chromatographic column is carried out blowback；Described second direction is opposite to the first direction, when carrier gas is flowed in a second direction, can remove the impurity in described first chromatographic column；Described carrier gas, after described first chromatographic column, enters fid detector through described damping column；
Described sampling device farther includes flow controller, and carrier gas is divided into the first branch road and the second branch road by described flow controller, and described first branch road and the second branch road are connected with ten-way valve respectively through pipeline；
Described ten-way valve is provided with ten openings, respectively the tenth opening, the first opening, the second opening, the 3rd opening, the 4th opening, the 5th opening, the 6th opening, the 7th opening, the 8th opening and the 9th opening, described tenth opening is sample gas import to be measured, and described 9th opening is sample gas to be measured outlet；Described second opening and described 6th opening are carrier gas inlet；Described first opening is connected by pipeline with described 4th opening, and described 5th opening is connected by pipeline with described 8th opening；Described first branch road is connected with described second opening line, and described second branch road is connected with described 6th opening.
2. chromatogram analysis method according to claim 1, it is characterized in that, described sampling device includes the first quantitative loop for quantitatively keeping in sample gas to be detected and the second quantitative loop, and described first quantitative loop is located on the pipeline between the first opening and described 4th opening；Described second quantitative loop is located on the pipeline between described 5th opening and described 8th opening.
3. chromatogram analysis method according to claim 2, it is characterised in that described six-way valve is provided with six perforates, respectively the first perforates, the second perforate, the 3rd perforate, the 4th perforate, the 5th perforate and the 6th perforate；Described 7th opening is connected with described 6th perforate pipeline, and described first chromatographic column includes first end and relative the second end, and described second chromatographic column includes the first port and the second relative port, and described damping column includes first end and relative the second end；The first end of described first chromatographic column is connected with described first perforate pipeline；The second end of described first chromatographic column is connected with described 3rd perforate pipeline；First port of described second chromatographic column is connected with described 3rd opening conduit；Second port of described second chromatographic column respectively with described second perforate, described 4th perforate, described damping column the second end pipeline be connected；The first end of described damping column is connected with described fid detector pipeline.
4. chromatogram analysis method according to claim 1, it is characterised in that described sampling device farther includes molecular sieve filtration pipe, described carrier gas filters laggard inbound traffics controller through molecular sieve filtration pipe.
5. chromatogram analysis method according to claim 4, it is characterised in that the state switching of described six-way valve is switched over by manually or automatically mode.
6. the chromatogram analysis method according to any one of claim 1-5, it is characterised in that described first chromatographic column is polarity capillary column, described polarity capillary column is aluminium sesquioxide capillary column or molecular sieve capillary column；Described second chromatographic column and described damping column are hollow capillary column.
7. a chromatogram analysis method, it is characterised in that: adopting gas chromatograph and sampling device, described sampling device provides sample gas to be detected for described gas chromatograph, and described gas chromatograph includes the first chromatographic column, the second chromatographic column, damping column and fid detector；
Described sampling device includes flow controller, ten-way valve, six-way valve, the first quantitative loop and the second quantitative loop；Carrier gas is divided into the first branch road and the second branch road by described flow controller, and the sample gas in the first quantitative loop and the second quantitative loop is taken out of by the carrier gas of described first branch road and the second branch road respectively；
Described ten-way valve is provided with ten openings, respectively the tenth opening, the first opening, the second opening, the 3rd opening, the 4th opening, the 5th opening, the 6th opening, the 7th opening, the 8th opening and the 9th opening, described tenth opening is sample gas import to be measured, described 9th opening is sample gas to be measured outlet, and described second opening and described 6th opening are carrier gas inlet；Described first opening is connected by pipeline with described 4th opening, and described first quantitative loop is series on the pipeline between the first opening and described 4th opening；Described 5th opening is connected by pipeline with described 8th opening, and described second quantitative loop is series on the pipeline between described 5th opening and described 8th opening；Described first branch road and the second opening connect, and described second branch road and the 6th opening connect；Described ten-way valve may be selected to be the first state and the second state；
Described six-way valve is provided with six perforates, respectively the first perforates, the second perforate, the 3rd perforate, the 4th perforate, the 5th perforate and the 6th perforate, and described 7th opening is connected with described 6th perforate pipeline；Described six-way valve may be selected to be state one and state two；
Described first chromatographic column includes first end and relative the second end, and described second chromatographic column includes the first port and the second relative port, and described damping column includes first end and relative the second end；The first end of described first chromatographic column is connected with described first perforate pipeline；The second end of described first chromatographic column is connected with described 3rd perforate pipeline；First port of described second chromatographic column is connected with described 3rd opening conduit；Second port of described second chromatographic column respectively with described second perforate, described 4th perforate, described damping column the second end pipeline be connected；The first end of described damping column is connected with described fid detector pipeline；Described chromatogram analysis method comprises the steps:
Sample gas is quantitative: allow described ten-way valve be in described first state, sample gas injects from described tenth opening, flow through described first opening, described first quantitative loop, described 4th opening, described 5th opening, described second quantitative loop, described 8th opening successively, last by described 9th opening outflow, when full described first quantitative loop and described second quantitative loop, stop sample introduction, complete dosing process；
Detection: make described ten-way valve be in the second state, described six-way valve is in the first state, the carrier gas of described first branch road flows through the first opening after entering described ten-way valve the second opening successively, first quantitative loop, 4th opening, 3rd opening, after second chromatographic column and damping column, deliver to fid detector to detect, the carrier gas of described second branch road flows through the 5th opening after entering the 6th opening successively, second quantitative loop, 8th opening, 7th opening, 6th perforate of described six-way valve, first perforate, first end along the first chromatographic column enters described first chromatographic column, 3rd perforate, deliver to fid detector after 4th perforate and damping column to detect；
Blowback: making described ten-way valve be in the second state, described six-way valve is in the second state, described carrier gas is by after described six-way valve, and the second end along described first chromatographic column flows through described first chromatographic column, and described first chromatographic column is carried out blowback；Described carrier gas, after described first chromatographic column, enters fid detector through described damping column.
8. chromatogram analysis method according to claim 7, it is characterised in that described sampling device farther includes molecular sieve filtration pipe, described carrier gas filters laggard inbound traffics controller through molecular sieve filtration pipe.
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| CN105987967B (en) * | 2015-04-03 | 2018-08-14 | 常州磐诺仪器有限公司 | Non-methane total hydrocarbons and benezene material detect dedicated unit |
| 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 |
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| CN109283281B (en) * | 2018-10-15 | 2023-11-03 | 兰州东立龙信息技术有限公司 | Chromatographic column |
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| CN111257473A (en) * | 2020-03-25 | 2020-06-09 | 常州磐诺仪器有限公司 | Non-methane total hydrocarbon on-line detection device |
| CN112147248A (en) * | 2020-09-23 | 2020-12-29 | 浙江求实环境监测有限公司 | Method for rapidly determining content of benzene series components in waste gas of fixed pollution source |
| CN112461968A (en) * | 2020-11-19 | 2021-03-09 | 必睿思(杭州)科技有限公司 | Gas chromatography analysis method for four gases of human body exhaled breath |
| CN112986447A (en) * | 2021-04-23 | 2021-06-18 | 中国原子能科学研究院 | Gas chromatography device |
| CN113533601B (en) * | 2021-09-07 | 2022-10-04 | 河北智德检验检测股份有限公司 | Headspace sample injector |
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