CN103134876B - Chromatographic analysis device and working method thereof - Google Patents
Chromatographic analysis device and working method thereof Download PDFInfo
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- CN103134876B CN103134876B CN201210598592.2A CN201210598592A CN103134876B CN 103134876 B CN103134876 B CN 103134876B CN 201210598592 A CN201210598592 A CN 201210598592A CN 103134876 B CN103134876 B CN 103134876B
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Abstract
The invention provides a chromatographic analysis device and a working method thereof. The chromatographic analysis device comprises a ration module, a sample valve, a sample gas channel, a carrier gas channel and a chromatographic column and further comprises a switch module. The switch module is used for being matched with the sample valve and enabling a ration ring to be selectively communicated with the sample gas channel and the carrier gas channel through the sample valve. The chromatographic analysis device has the advantages of being capable of solving the problems of baseline fluctuation and narrow band, adjusting sample introduction size and the like.
Description
Technical field
The present invention relates to species analysis, particularly effectively can solve chromatographic analysis device and the method for work thereof of baseline fluctuation problem.
Background technology
Valve injection is that on-line chromatograph commonly uses input mode, and Fig. 1 schematically illustrates the constitutional diagram of sampling valve when sample introduction is analyzed, and as shown in Figure 1, quantitative loop is flow through in carrier gas, is brought in chromatographic column by sample.Fig. 2 schematically illustrates the constitutional diagram of valve when rinsing quantitative, and as shown in Figure 2, sample gas is quantitative by quantitative loop, carrier gas flushing line, chromatographic column.
Mainly there is the problem of baseline fluctuation in above-mentioned valve injection mode, as shown in Figure 3.Before sample introduction, in quantitative loop, sample atmospheric pressure can equilibrate to atmospheric pressure usually; and be pressed between 150kPa ~ 300kPa (gauge pressure) before the post used; when forwarding the sample introduction analysis phase to from the flushing quantitative loop stage; carrier gas enters in quantitative loop; pressure can decline suddenly; need one stage adjust equilibration time to make pressure again reach original pressure, spectrogram shows as the fluctuation of baseline.
At present, prior art does not solve the scheme of baseline fluctuation, just by extending chromatographic column, or changes analysis condition, thus makes baseline fluctuation can not occur in chromatographic peak place, thus avoids fluctuation for the impact analyzed.
Summary of the invention
In order to solve the deficiency in above-mentioned prior art, the invention provides a kind of chromatographic analysis device and the method for work thereof that effectively can solve baseline fluctuation problem.
The object of the invention is to be achieved through the following technical solutions:
A kind of chromatographic analysis device, described chromatographic analysis device comprises quantitative module, sampling valve, sample gas passage, carrier gas passage and chromatographic column, and described chromatographic analysis device comprises further:
Handover module, described handover module is used for and described sampling valve coordinates, and described quantitative loop is optionally communicated with described sample gas passage, carrier gas passage by described sampling valve.
According to above-mentioned chromatographic analysis device, preferably, described sampling valve is ten-way valve.
According to above-mentioned chromatographic analysis device, preferably, described handover module is T-valve.
According to above-mentioned chromatographic analysis device, alternatively, described handover module comprises:
First valve, described sample gas passage is communicated with described quantitative module by described first valve, sampling valve;
Second valve, described carrier gas passage is communicated with described quantitative module by described second valve, sampling valve.
Object of the present invention is also achieved by the following technical programs:
A kind of chromatogram analysis method, described chromatogram analysis method comprises with the next stage:
In the quantitative stage, by the switching of handover module and the work of sampling valve, sample gas is quantitative by entering quantitative module after handover module, sampling valve;
Pre-compression phase, by the switching of described handover module and the work of described sampling valve, carrier gas enters described quantitative module by described handover module, sampling valve; Meanwhile, carrier gas enters chromatographic column by described sampling valve;
In the sample introduction stage, by the switching of described handover module and the work of described sampling valve, carrier gas is by described sampling valve, quantitative loop, thus the sample gas that carry in described quantitative module enters chromatographic column;
Analysis phase, analyze the sample gas entering chromatographic column, thus know the content of each composition in sample gas.
According to above-mentioned chromatogram analysis method, alternatively, in the described quantitative stage, carrier gas is by chromatographic column described in described sampling valve post-flush.
According to above-mentioned chromatogram analysis method, preferably, described sampling valve is ten-way valve.
According to above-mentioned chromatogram analysis method, preferably, described handover module is T-valve.
According to above-mentioned chromatogram analysis method, alternatively, described handover module comprises:
First valve, described sample gas passage is communicated with described quantitative module by described first valve, sampling valve;
Second valve, described carrier gas passage is communicated with described quantitative module by described second valve, sampling valve.
Compared with prior art, the beneficial effect that the present invention has is:
1, experimental result shows, sample gas is through precompression, and sample introduction bands of a spectrum are narrower;
2, before sample introduction, sample is compressed to pressure before post, solves the problem of baseline fluctuation in valve injection with this;
3, by controlling the switching time of sampling valve, sampling volume can be regulated.
Accompanying drawing explanation
With reference to accompanying drawing, disclosure of the present invention will be easier to understand.Those skilled in the art it is easily understood that: these accompanying drawings only for illustrating technical scheme of the present invention, and and are not intended to be construed as limiting protection scope of the present invention.In figure:
Fig. 1 is according to the state diagram of chromatographic analysis device in prior art when sample introduction is analyzed;
Fig. 2 is according to the state diagram of chromatographic analysis device in prior art when quantitatively rinsing;
Fig. 3 is the spectrogram according to recording in stratographic analysis process in prior art;
Fig. 4 is according to the chromatographic analysis device of the embodiment of the present invention 1 sketch in the quantitative stage;
Fig. 5 is according to the chromatographic analysis device of the embodiment of the present invention 1 sketch at pre-compression phase;
Fig. 6 is according to the chromatographic analysis device of the embodiment of the present invention 1 sketch in the sample introduction stage.
Embodiment
Fig. 4-6 and following description describe Alternate embodiments of the present invention and how to implement to instruct those skilled in the art and to reproduce the present invention.In order to instruct technical solution of the present invention, simplifying or having eliminated some conventional aspects.Those skilled in the art should understand that the modification that is derived from these embodiments or replace will within the scope of the invention.Those skilled in the art should understand that following characteristics can combine to form multiple modification of the present invention in every way.Thus, the present invention is not limited to following Alternate embodiments, and only by claim and their equivalents.
Embodiment 1:
Fig. 4 schematically illustrates the structure diagram of the chromatographic analysis device of the embodiment of the present invention, and as shown in Figure 4, described chromatographic analysis device comprises:
Quantitative module (as quantitative loop), sampling valve (as ten-way valve), sample gas passage, carrier gas passage and chromatographic column, above-mentioned quantitative module, passage, valve, chromatographic column and between connected mode be the state of the art, do not repeat them here;
Handover module, described handover module is used for and described sampling valve coordinates, and described quantitative loop is optionally communicated with described sample gas passage, carrier gas passage by described sampling valve.
Preferably, described handover module is T-valve.
The chromatogram analysis method of the embodiment of the present invention, be also the course of work of above-mentioned chromatographic analysis device, described chromatogram analysis method comprises with the next stage:
The quantitative stage, Fig. 4 schematically illustrates the state diagram that above-mentioned chromatographic analysis device is in the quantitative stage, as shown in Figure 4, by the switching of handover module (as T-valve) and the work of sampling valve, make sample gas quantitative by entering quantitative module after handover module, sampling valve;
Pre-compression phase, Fig. 5 schematically illustrates the state diagram that above-mentioned chromatographic analysis device is in the quantitative stage, as shown in Figure 5, by the switching of described handover module (as T-valve) and the work of sampling valve, carrier gas enters described quantitative module by described handover module, sampling valve; Meanwhile, carrier gas enters chromatographic column by described sampling valve; Thus pressure is consistent before making quantitative module and chromatographic column;
The sample introduction stage, Fig. 6 schematically illustrates the state diagram that above-mentioned chromatographic analysis device is in the quantitative stage, as shown in Figure 6, by the switching of described handover module (as T-valve) and as described in the work of sampling valve, carrier gas is by described sampling valve, quantitative loop, thus the sample gas that carry in described quantitative module enters chromatographic column;
Analysis phase, analyze the sample gas entering chromatographic column, thus know the content of each composition in sample gas.
Be according to the benefit that the embodiment of the present invention 1 reaches: by arranging handover module, make before sample introduction, by the switching of handover module, carrier gas enters quantitative module and chromatographic column respectively, thus make the quantitative module when sample introduction identical with pressure before chromatographic column, efficiently avoid the appearance of baseline fluctuation problem.Meanwhile, by controlling the switching time of sampling valve, go to regulate sampling volume.
Embodiment 2:
The chromatographic analysis device of the embodiment of the present invention, as different from Example 1:
Handover module is made up of the first valve and the second valve, and described sample gas passage is communicated with described quantitative module by described first valve, sampling valve; Described carrier gas passage is communicated with described quantitative module by described second valve, sampling valve.In the quantitative stage, open the first valve and close the second valve; At pre-compression phase, close the first valve and open the second valve; In the sample introduction stage, open the first valve and close the second valve.
Claims (4)
1. a chromatogram analysis method, described chromatogram analysis method comprises with the next stage:
In the quantitative stage, by the switching of handover module and the work of sampling valve, sample gas enters sampling valve by handover module, enters quantitative module quantitatively, enter sampling valve more afterwards, rear discharge sampling valve after discharging sampling valve;
Pre-compression phase, by the switching of described handover module and the work of described sampling valve, carrier gas enters sampling valve by described handover module, enters described quantitative module, enter sampling valve more afterwards and discharge after discharging sampling valve; Meanwhile, carrier gas enters described sampling valve, enters chromatographic column, enter sampling valve more afterwards and discharge after discharging sampling valve; Pressure before quantitative module and before chromatographic column is consistent;
The sample introduction stage, by the switching of described handover module and the work of sampling valve, carrier gas enters described sampling valve, quantitative module is entered after discharging sampling valve, again enter described sampling valve afterwards and discharge, thus the sample gas that carry in described quantitative module enters chromatographic column, again enters sampling valve afterwards, enter sampling valve again after discharge, finally discharge.
2. chromatogram analysis method according to claim 1, is characterized in that: described sampling valve is ten-way valve.
3. chromatogram analysis method according to claim 1, is characterized in that: described handover module is T-valve.
4. chromatogram analysis method according to claim 1, is characterized in that: described handover module comprises:
First valve, described sample gas passage is communicated with described quantitative module by described first valve, sampling valve;
Second valve, described carrier gas passage is communicated with described quantitative module by described second valve, sampling valve.
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| CN201210598592.2A CN103134876B (en) | 2012-12-29 | 2012-12-29 | Chromatographic analysis device and working method thereof |
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| CN201210598592.2A CN103134876B (en) | 2012-12-29 | 2012-12-29 | Chromatographic analysis device and working method thereof |
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| CN103134876B true CN103134876B (en) | 2015-04-08 |
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106885864A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | The more bundles of capillaries post and flight time mass spectrum of sampling sample introduction integration are used in conjunction device |
| CN106053667A (en) * | 2016-07-14 | 2016-10-26 | 湘潭大学 | Multi-position hydrocarbon online detection equipment and method |
| CN106018863A (en) * | 2016-07-29 | 2016-10-12 | 北京宝德仪器有限公司 | Measuring device and process for measuring by virtue of standard addition method |
| CN107367421A (en) * | 2017-09-19 | 2017-11-21 | 四川省科源工程技术测试中心 | Shale gas automatic dilution device and system |
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