CN104280486A - Chromatographic analysis method - Google Patents
Chromatographic analysis method Download PDFInfo
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- CN104280486A CN104280486A CN201410573078.2A CN201410573078A CN104280486A CN 104280486 A CN104280486 A CN 104280486A CN 201410573078 A CN201410573078 A CN 201410573078A CN 104280486 A CN104280486 A CN 104280486A
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- 238000000034 method Methods 0.000 title claims abstract description 18
- 238000004587 chromatography analysis Methods 0.000 title abstract description 17
- 239000007789 gas Substances 0.000 claims abstract description 95
- 238000013016 damping Methods 0.000 claims abstract description 51
- 239000012159 carrier gas Substances 0.000 claims abstract description 46
- 238000005070 sampling Methods 0.000 claims abstract description 31
- 239000012530 fluid Substances 0.000 claims abstract description 5
- 238000004458 analytical method Methods 0.000 claims description 25
- 238000012360 testing method Methods 0.000 claims description 22
- 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 19
- 238000001914 filtration Methods 0.000 claims description 16
- 230000008676 import Effects 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [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
- 238000000926 separation method Methods 0.000 abstract description 8
- 238000001514 detection method Methods 0.000 abstract description 7
- 238000011010 flushing procedure Methods 0.000 abstract 1
- 230000002035 prolonged effect Effects 0.000 abstract 1
- 238000011002 quantification Methods 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- 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
- 238000007664 blowing Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 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
- 230000009286 beneficial effect 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
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000035772 mutation Effects 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention relates to a chromatographic analysis method. According to the chromatographic analysis method, a gas chromatograph and a sampling device are used, wherein the sampling device is used for providing fluid to be detected to the gas chromatograph; the gas chromatograph comprises a first chromatographic column, a second chromatographic column, a damping column and an FID detector; the sampling device comprises a ten-way valve and a six-way valve; the six-way valve can be selected to be in a state I and a state II; the ten-way valve can be selected to be in a first state and a second state; and the chromatographic analysis method comprises the steps of sample gas quantification, detection and back flushing. The chromatographic analysis method has the advantages that the dosage of carrier gas is saved, the accuracy of the sample gas separation is improved, the accuracy of the sample gas detection is improved, the life of the chromatographic columns is prolonged, and two different substances of the same sample gas can be measured at the same time, so that the working efficiency is greatly improved.
Description
Technical field
The present invention relates to a kind of chromatogram analysis method.
Background technology
At present, for the detection of NMHC, great majority are analyzed according to the method described in Chinese Ministry of Environmental Protection standard HJ/T 38-1999, the time stopped in the chromatography column due to the component of the large polarity of the higher boiling in sample gas is longer, the analysis of the next sample gas of easy interference, and easily pollute chromatographic column, shorten chromatographic column serviceable life.
Summary of the invention
In view of this, be necessary provide a kind of single injected sampling can measure two kinds of compositions simultaneously and improve the chromatogram analysis method in chromatographic column serviceable life in fact.
Object 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 comprises the first chromatographic column, the second chromatographic column, damping column and fid detector; Described sampling device comprises 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, will treat that test sample gas injects described ten-way valve and carries out quantitatively;
Detect: 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, to treat that test sample gas divides two-way to take out of, one road flows through the second chromatographic column and damping column and delivers to fid detector and detect, another road flows through six-way valve successively, flow through the first chromatographic column, damping column along first direction (as shown in Figure 2) after, deliver to fid detector and detect;
Blowback: make described ten-way valve be in the second state, described six-way valve is in state two, described carrier gas, by after described six-way valve, flows through described first chromatographic column along second direction (as shown in Figure 3), carries out blowback to described first chromatographic column; Described second direction is opposite to the first direction, when carrier gas is flowed along second direction, can remove the impurity in described first chromatographic column.
Preferably, described sampling device comprises flow controller further, 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 by pipeline.
Preferably, described ten-way valve is provided with ten openings, be 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 for treating the import of test sample gas, and described 9th opening is for treating that test sample gas exports; 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 comprises the first quantitative loop and the second quantitative loop for quantitatively keeping in test sample gas to be checked, 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, is respectively the first perforate, 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, described first chromatographic column comprises first end and relative the second end, described second chromatographic column comprises the first port and the second relative port, and described damping column comprises 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 is connected with the second end pipeline of described second perforate, described 4th perforate, described damping column respectively; The first end of described damping column is connected with described fid detector pipeline.
Preferably, described sampling device comprises molecular sieve filtration pipe further, 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 by manual or automated manner.
Preferably, described first chromatographic column is polarity capillary column, and described polarity capillary column is alundum (Al2O3) 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 test sample gas to be checked for described gas chromatograph, and described gas chromatograph comprises the first chromatographic column, the second chromatographic column, damping column and fid detector;
Described sampling device comprises 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 band of gas in the first quantitative loop and the second quantitative loop goes out by the carrier gas of described first branch road and the second branch road respectively;
Described ten-way valve is provided with ten openings, be 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 for treating the import of test sample gas, described 9th opening is for treating that test sample gas exports, 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 is connected with the second opening, and described second branch road is connected with the 6th opening; 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, is respectively the first perforate, 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 comprises first end and relative the second end, and described second chromatographic column comprises the first port and the second relative port, and described damping column comprises 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 is connected with the second end pipeline of described second perforate, described 4th perforate, described damping column respectively; 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, finally flowed out by described 9th opening, when being full of described first quantitative loop and described second quantitative loop, stop sample introduction, complete dosing process.
Detect: make described ten-way valve be in the second state, described six-way valve is in the first state, the first opening is flowed through successively after the carrier gas of described first branch road enters described ten-way valve second opening, first quantitative loop, 4th opening, 3rd opening, after second chromatographic column and damping column, deliver to fid detector to detect, the 5th opening is flowed through successively after the carrier gas of described second branch road enters the 6th opening, 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: make 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, carries out blowback to described first chromatographic column.
Preferably, described sampling device comprises molecular sieve filtration pipe further, 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 following beneficial effect:
(1) chromatogram analysis method of the present invention, load volume required during analysis sample gas is less, and chromatogram peak is out sharper, does not have conditions of streaking, not only saves the consumption of carrier gas, also improves the degree of accuracy that sample gas is separated.
(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 the blowing function realized chromatographic column, significantly reduce the pollution of chromatographic column, decrease equally gas and remain the interference that next sample gas is measured, when being particularly separated the component of the large polarity of higher boiling, effect is especially obvious, this improves the degree of accuracy that sample gas detects, extend the life-span of chromatographic column.
(3) in addition, chromatogram analysis method of the present invention also applies ten-way valve, thus realizes the two kinds of different materials simultaneously measuring same equally gas, substantially increases work efficiency.
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 detected 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 detected 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 numeral is listed:
400-chromatographic analysis system 512-the second perforate
100-sampling device 513-the three perforate
10-flow controller 514-the four perforate
11-the first branch road 515-the five perforate
13-the second branch road 516-the six perforate
30-ten-way valve 60-the second quantitative loop
311-the first opening 70-molecular sieve filtration pipe
312-the second opening 90-ecp assembly
313-the three opening 901-entrance
314-the four opening 200-gas chromatograph
315-the five opening 210-the first chromatographic column
316-the six opening 211-first end
317-the seven opening 213-the second end
318-the eight opening 230-the second chromatographic column
319-the nine opening 231-the first port
310-the ten opening 233-the second port
40-the first quantitative loop 250-damping column
50-six-way valve, 251-first end
511-the first perforate 253-the second end
270-fid detector, 290-injection port
Embodiment
Chromatographic analysis system of the present invention is example for detection gas, in the preferred embodiment, is applied to the NMHC measured in air and waste gas is illustrated for it.
Chromatographic analysis system 400 as Fig. 1 present pre-ferred embodiments comprises 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 comprises the first chromatographic column 210, second chromatographic column 230, damping column 250 and flame ionization ditector (Flame Ionization Detector, fid detector) 270.Described sampling device 100 comprises 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 will enter to deliver to FID detector 270 after the second chromatographic column 230 and damping column 250 and detect until test sample air-blowing; Another road air-flow will enter after damping column 250, to deliver to FID detector 270 after six-way valve 50 and the first chromatographic column 210 and detect until test sample air-blowing, thus achieve and detect with while two kinds of components in the same 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 two kinds of different components that realization detects in sample gas in single injected sampling simultaneously, such as detect the content of Determination of Total Hydrocarbon In Atomsphere and methane.Described six-way valve 50 is for controlling gas flow direction, realize that sample gas is delivered to described first chromatographic column 210 from forward and carry out separation detection, carrier gas is oppositely sent into described first chromatographic column 210, blowback is carried out to described first chromatographic column 210, to remove sample gas 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 the separation of sample gas; Flow counterflow through and blowback is carried out to described first chromatographic column 210.The present invention realizes removing residual sample gas to the blowback of polarity chromatographic column by increasing six-way valve 50, improves the degree of accuracy that sample gas detects, extends the life-span of polarity chromatographic column.
Described flow controller 10 comprises 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, is respectively the tenth opening 310, first opening 311, second opening 312, the 3rd opening 313, the 4th opening 314, the 5th opening 315, the 6th opening 316, the 7th opening 317, the 8th opening 318 and the 9th opening 319.Described tenth opening 310 is the import of sample gas, and described 9th opening 319 is the outlet of sample gas.Described second opening 312 and described 6th opening 316 are carrier gas inlet.Described first opening 311 is connected by pipeline (scheming 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 treat test sample gas for quantitatively temporary.
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, and also can be 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 as shown in Fig. 1 direction of arrow.
As shown in Figure 2, when described ten-way valve 30 is in described second state, carrier gas flows into from 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 band of gas in described first quantitative loop 40 is gone out, flow through described 4th opening 314, described 3rd opening 313 successively, enter described second chromatographic column 230 carry out separation 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, the sample band of gas in described second quantitative loop 60 is gone out, flow through described 8th opening 318, described 7th opening 317, described six-way valve 50 successively, enter described first chromatographic column 210 carry out separation after, through described damping column 250, finally enter fid detector and quantitatively detect.
Described six-way valve 50 is provided with six perforates, is respectively the first perforate 511, second perforate the 512, three perforate the 513, four perforate the 514, five perforate 515 and the 6th perforate 516.Described six-way valve 50 has two states, is respectively state one (as shown in Figure 2) and state two (as shown in Figure 3), can mutually switches between described state one and described state two.Described switching action both can manually control, and also can be 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 separated, through described damping column 250, finally enter fid detector and quantitatively detect (i.e. testing 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 successively, oppositely flow into described first chromatographic column 210, 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 comprises first end 211 and relative the second end 213.Described second chromatographic column 230 comprises the first port 231 and the second relative port 233.Described damping column 250 comprises 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 alundum (Al2O3) capillary column or molecular sieve capillary column.Described second chromatographic column 230 and described damping column 250 are hollow capillary column.For use 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 is out sharper, avoids conditions of streaking, improves the degree of accuracy that sample gas is separated.When described six-way valve 50 carries out state switching, ducted fluid flow can be undergone mutation, and described damping column 250, for cushioning fluid flow sudden change caused when described six-way valve 50 state switches, prevents described fid detector 270 from stopping working.Described fid detector 270 is for carrying out quantitative test to the outflow component after separation.
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 is connected with the second end 253 pipeline of described second perforate 512, described 4th perforate 514, described damping column 250 respectively.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 provided with molecular sieve filtration pipe 70 further, and carrier gas is delivered to flow controller 10 pipeline and connects after the purification of molecular sieve filtration pipe 70.
In the preferred embodiment, described sampling device 100 is provided with ecp assembly 90 further.Described ecp assembly 90 is provided with carrier gas inlet 901, and is connected with change-over switch (the scheming not shown) pipeline of described six-way valve 50.When needing the state switching described six-way valve 50, start carrier gas, described six-way valve 50 just promotes described six-way valve 50 and switches 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 as shown in Fig. 1 direction of arrow.When being full of described first quantitative loop 40 and described second quantitative loop 60, stopping sample introduction, completing dosing process.
Testing process: as shown in Figure 2, after quantitatively completing, is adjusted to described second state by described ten-way valve 30, described six-way valve 50 is adjusted to described state one.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, the sample band of gas in described first quantitative loop 40 is gone out, flow through described 4th opening 314, described 3rd opening 313 successively, enter described second chromatographic column 230 carry out separation 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, the sample band of gas in described second quantitative loop 60 is gone out, flow through described 8th opening 318, described 7th opening 317, described 6th perforate 516, described first perforate 511 successively, enter after (forward enters) described first chromatographic column 210 is separated from the first end 211 of described first chromatographic column 210, through described damping column 250, finally enter fid detector and quantitatively detect.
Blowback process: as shown in Figure 3, described ten-way valve 30 is still in described second state, and 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, the sample band of gas in described first quantitative loop 40 is gone out, flow through described 4th opening 314, described 3rd opening 313 successively, enter described second chromatographic column 230 carry out separation 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, the sample band of gas in described second quantitative loop 60 is gone out, flow through described 8th opening 318 successively, described 7th opening 317, described 6th perforate 516, described 3rd perforate 513, after entering (oppositely entering) 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 the impurity remained in described first chromatographic column 210 is discharged.。
As shown in Figure 4, in another embodiment of the invention, described chromatographic analysis system 400 comprises six-way valve 50 and gas chromatograph 200.
Described six-way valve 50 comprises six perforates, is respectively the first perforate 511, second perforate the 512, three perforate the 513, four perforate the 514, five perforate 515 and the 6th perforate 516.Described six-way valve 50 has two states, is respectively state one (as shown in Figure 4) and state two (as shown in Figure 5), can mutually switches between described state one and described state two.Described switching action both can manually control, and also can be realized by electric controlled pneumatic control.
Described gas chromatograph 200 comprises the first chromatographic column 210, damping column 250, fid detector 270 and injection port 290.Described first chromatographic column 210 comprises first end 211 and relative the second end 213.Described damping column 250 comprises 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 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 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 provided with molecular sieve filtration pipe 70 further, 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 provided with ecp assembly 90 further.Described ecp assembly 90 is provided with carrier gas inlet 901, and is connected with change-over switch (the scheming not shown) pipeline of described six-way valve 50.When needing the state switching described six-way valve 50, start carrier gas, described six-way valve 50 just promotes described six-way valve 50 and switches between described state one and state two under the air pressure of carrier gas.
Testing 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 enters) described first chromatographic column 210 is separated from the first end 211 of described first chromatographic column 210, through described damping column 250, finally enter fid detector and quantitatively detect.
Blowback process: as 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, after flowing through described injection port 290, described 6th perforate 516, described 3rd perforate 513 successively, entering (oppositely entering) described first chromatographic column 210 from the second end 213 of described first chromatographic column 210, 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 present invention is not limited to above-mentioned embodiment, if do not depart from the spirit and scope of the present invention to various change of the present invention or distortion, if these are changed and distortion belongs within claim of the present invention or equivalent technologies scope, then the present invention is also intended to comprise these changes and distortion.
Claims (10)
1. a chromatogram analysis method, is characterized in that: adopt gas chromatograph and sampling device, and described sampling device provides fluid to be detected for gas chromatograph, and described gas chromatograph comprises the first chromatographic column, the second chromatographic column, damping column and fid detector; Described sampling device comprises 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, will treat that test sample gas injects described ten-way valve and carries out quantitatively;
Detect: 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, to treat that test sample gas divides two-way to take out of, after one road flows through the second chromatographic column, damping column, after delivering to fid detector to detect, another road flows through six-way valve successively, flowing through the first chromatographic column and damping column along first direction, deliver to fid detector and detect;
Blowback: make described ten-way valve be in the second state, described six-way valve is in state two, described carrier gas, by after described six-way valve, flows through described first chromatographic column along second direction, carries out blowback to described first chromatographic column; Described second direction is opposite to the first direction, when carrier gas is flowed along second direction, can remove the impurity in described first chromatographic column.
2. chromatogram analysis method according to claim 1, it is characterized in that: described sampling device comprises flow controller further, 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 by pipeline.
3. chromatogram analysis method according to claim 2, it is characterized in that, described ten-way valve is provided with ten openings, be 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 for treating the import of test sample gas, and described 9th opening is for treating that test sample gas exports; 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.
4. chromatogram analysis method according to claim 3, it is characterized in that, described sampling device comprises the first quantitative loop and the second quantitative loop for quantitatively keeping in test sample gas to be checked, 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.
5. chromatogram analysis method according to claim 4, is characterized in that, described six-way valve is provided with six perforates, is respectively the first perforate, 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, described first chromatographic column comprises first end and relative the second end, described second chromatographic column comprises the first port and the second relative port, and described damping column comprises 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 is connected with the second end pipeline of described second perforate, described 4th perforate, described damping column respectively; The first end of described damping column is connected with described fid detector pipeline.
6. chromatogram analysis method according to claim 2, is characterized in that, described sampling device comprises molecular sieve filtration pipe further, and described carrier gas filters laggard inbound traffics controller through molecular sieve filtration pipe.
7. chromatogram analysis method according to claim 6, is characterized in that, the state of described six-way valve switches and switched by manual or automated manner.
8. the chromatogram analysis method according to any one of claim 1-7, is characterized in that, described first chromatographic column is polarity capillary column, and described polarity capillary column is alundum (Al2O3) capillary column or molecular sieve capillary column; Described second chromatographic column and described damping column are hollow capillary column.
9. a chromatogram analysis method, it is characterized in that: adopt gas chromatograph and sampling device, described sampling device provides test sample gas to be checked for described gas chromatograph, and described gas chromatograph comprises the first chromatographic column, the second chromatographic column, damping column and fid detector;
Described sampling device comprises 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 band of gas in the first quantitative loop and the second quantitative loop goes out by the carrier gas of described first branch road and the second branch road respectively;
Described ten-way valve is provided with ten openings, be 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 for treating the import of test sample gas, described 9th opening is for treating that test sample gas exports, 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 is connected with the second opening, and described second branch road is connected with the 6th opening; 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, is respectively the first perforate, 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 comprises first end and relative the second end, and described second chromatographic column comprises the first port and the second relative port, and described damping column comprises 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 is connected with the second end pipeline of described second perforate, described 4th perforate, described damping column respectively; 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, finally flowed out by described 9th opening, when being full of described first quantitative loop and described second quantitative loop, stop sample introduction, complete dosing process.
Detect: make described ten-way valve be in the second state, described six-way valve is in the first state, the first opening is flowed through successively after the carrier gas of described first branch road enters described ten-way valve second opening, first quantitative loop, 4th opening, 3rd opening, after second chromatographic column and damping column, deliver to fid detector to detect, the 5th opening is flowed through successively after the carrier gas of described second branch road enters the 6th opening, 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: make 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, carries out blowback to described first chromatographic column.
10. chromatogram analysis method according to claim 9, is characterized in that, described sampling device comprises molecular sieve filtration pipe further, and described carrier gas filters laggard inbound traffics controller through molecular sieve filtration pipe.
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