CN112595791A - Gas chromatography device based on automatic sample introduction of electromagnetic valve and detection method - Google Patents
Gas chromatography device based on automatic sample introduction of electromagnetic valve and detection method Download PDFInfo
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- 238000004817 gas chromatography Methods 0.000 title claims abstract description 104
- 238000001514 detection method Methods 0.000 title claims abstract description 63
- 238000010926 purge Methods 0.000 claims abstract description 58
- 238000005070 sampling Methods 0.000 claims abstract description 32
- 238000002347 injection Methods 0.000 claims abstract description 31
- 239000007924 injection Substances 0.000 claims abstract description 31
- 239000012159 carrier gas Substances 0.000 claims description 131
- 239000007789 gas Substances 0.000 claims description 80
- 238000000034 method Methods 0.000 claims description 37
- 230000008569 process Effects 0.000 claims description 36
- 238000000926 separation method Methods 0.000 claims description 14
- 238000004458 analytical method Methods 0.000 claims description 11
- 238000005057 refrigeration Methods 0.000 claims description 9
- 238000003795 desorption Methods 0.000 claims description 8
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 238000011161 development Methods 0.000 abstract description 2
- 238000004587 chromatography analysis Methods 0.000 description 48
- 230000009977 dual effect Effects 0.000 description 14
- 238000012360 testing method Methods 0.000 description 10
- 238000005516 engineering process Methods 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 6
- 238000010586 diagram Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000011002 quantification Methods 0.000 description 3
- 230000005526 G1 to G0 transition Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000037361 pathway Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/24—Automatic injection systems
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/66—Thermal conductivity detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/68—Flame ionisation detectors
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N2030/022—Column chromatography characterised by the kind of separation mechanism
- G01N2030/025—Gas chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
- G01N2030/201—Injection using a sampling valve multiport valves, i.e. having more than two ports
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Abstract
The invention provides a gas chromatography device based on automatic sample injection of an electromagnetic valve and a detection method, wherein the functions of purging, sampling, sample injection, detection and the like of the gas chromatography device can be realized by performing ordered flow path switching based on the electromagnetic valve, and the micro electromagnetic valve with low power consumption is adopted, so that the power consumption of the gas chromatography device can be reduced, and the miniaturization of the gas chromatography device is facilitated based on the characteristics of small volume and light weight of the micro electromagnetic valve, so that the development of low power consumption and miniaturization of the gas chromatography device is facilitated, the operation convenience of the gas chromatography device is improved, and the application range of the gas chromatography device is expanded.
Description
Technical Field
The invention belongs to the field of analytical chemistry, and relates to a gas chromatography device based on automatic sample injection of an electromagnetic valve and a detection method.
Background
The chromatography is a separation and detection technology for complex mixed components, and has wide application in the fields of petrochemical industry, exploration, environmental monitoring and the like. Gas chromatography refers to chromatography using a gas as the mobile phase. Due to the fast transport speed of the sample in the gas phase, the components of the sample can reach equilibrium between the mobile phase and the stationary phase instantaneously. In addition, the materials which can be selected as the stationary phase are more, so that the gas chromatography is a separation analysis method with high analysis speed and high separation efficiency. In recent years, a high-sensitivity selective detector is adopted, so that the method has the advantages of high analysis sensitivity, wide application range and the like.
The gas chromatograph is a chromatographic analysis device using gas as a mobile phase. The principle is mainly to realize the separation of the mixture by utilizing the differences of the boiling point, the polarity and the adsorption property of the substances. The sample to be analyzed is gasified in the gasifying chamber and carried into the chromatographic column with inert gas, liquid or solid fixed phase, and the components are separated in the column through repeated distribution and adsorption of the components in the sample under the flushing of the carrier gas.
Traditional gas chromatographs are powerful, can realize separation and detection to complicated material component, but traditional gas chromatographs power consumption is high, bulky, weight is heavy, generally can only use in the laboratory. With the development of society and economy and the rise of internet of things technology, more and more application occasions need to carry out real-time, on-site, quick and on-line detection on complex components, and the application occasions generally require that a gas chromatography device has an automatic sample introduction function and require that the whole device realizes low power consumption and microminiaturization. At present, the automatic sample introduction of the gas chromatography device generally adopts an electrically driven mechanical six-way valve, which has large volume, heavy weight and high power consumption and is not beneficial to realizing low power consumption and microminiaturization of the gas chromatography device.
Therefore, it is necessary to provide a gas chromatography device and a detection method based on electromagnetic valve automatic sample injection.
Disclosure of Invention
In view of the above drawbacks of the prior art, an object of the present invention is to provide a gas chromatograph apparatus and a detection method based on electromagnetic valve automatic sample injection, which are used to solve the problems of the prior art that when an electrically driven mechanical six-way valve is used for automatic sample injection in the gas chromatograph apparatus, the gas chromatograph apparatus has a large volume, a heavy weight, and high power consumption, which is not beneficial to realizing low power consumption and miniaturization of the gas chromatograph apparatus.
To achieve the above and other related objects, the present invention provides a gas chromatography apparatus based on automatic sample injection by a solenoid valve, the gas chromatography apparatus comprising:
a first three-way solenoid valve including a first port K1, a second port K2, and a third port K3;
a second three-way solenoid valve including a first port K4, a second port K5, and a third port K6;
a third three-way solenoid valve including a first port K7, a second port K8, and a third port K9;
a sampler comprising a sampler inlet and a sampler outlet;
a chromatography column comprising a chromatography column inlet and a chromatography column outlet;
a detector comprising a detector inlet and a detector outlet;
the first port K1 and the first port K7 are carrier gas inlets, the second port K2 is a sample gas inlet, and the second port K5 and the detector outlet are evacuation ports;
the third port K3 is connected with the sampler inlet, the first port K4 is connected with the sampler outlet, the third port K6 is connected with the second port K8, the third port K9 is connected with the chromatographic column inlet, and the chromatographic column outlet is connected with the detector inlet.
Optionally, the sampler comprises a dosing loop or an enricher.
Optionally, when the sampler employs the enricher, the gas chromatography apparatus further comprises:
a first two-way solenoid valve including a first two-way solenoid valve inlet and a first two-way solenoid valve outlet;
a second two-way solenoid valve comprising a second two-way solenoid valve inlet and a second two-way solenoid valve outlet;
wherein, the first two-way solenoid valve entry with third port K3 is connected, the first two-way solenoid valve export is connected with the enricher entry, the second two-way solenoid valve entry is connected with the enricher export, the second two-way solenoid valve export with first port K4 is connected.
Optionally, the detector comprises one of a hydrogen Flame Ionization Detector (FID), a Photo Ionization Detector (PID), and a Helium Ionization Detector (HID).
Optionally, the gas chromatography apparatus comprises a dual column gas chromatography apparatus comprising:
a first chromatography column comprising a first chromatography column inlet and a first chromatography column outlet;
a second chromatography column comprising a second chromatography column inlet and a second chromatography column outlet;
a dual-path detector comprising a detector first inlet, a detector second inlet, a detector first outlet, and a detector second outlet;
the inlet of the second chromatographic column is a carrier gas inlet, and the first outlet of the detector and the second outlet of the detector are evacuation ports;
the first chromatographic column inlet is connected with the third port K9, the first chromatographic column outlet is connected with the first detector inlet, and the second chromatographic column outlet is connected with the second detector inlet.
Optionally, the detector comprises a Thermal Conductivity Detector (TCD).
Optionally, the gas chromatography apparatus further includes a micro pump, an inlet of the micro pump is connected to the second port K5, and an outlet of the micro pump is a drain.
Optionally, the power consumption value of the solenoid valve is less than 1 watt; the size range of the electromagnetic valve is 1-10 cm; the weight range of the electromagnetic valve is 5 g-100 g.
The invention also provides a detection method of the gas chromatography device, which comprises the following steps:
providing any one of the above gas chromatography apparatuses, starting the gas chromatography apparatus, and performing the following operations:
purging: communicating the first port K1, the third port K3, the sampler, the first port K4 and the second port K5 to form a first purge path; communicating the first port K7, third port K9, chromatography column and detector to form a second purge path; a first carrier gas completes the purging of the sampler through the first purging path; a second carrier gas completes the purging of the chromatographic column and the detector through the second purging path;
sampling: the second port K2, the third port K3, the sampler, the first port K4 and the second port K5 are communicated to form a sampling path; the sampling path is used for filling the sampler with sample gas to finish sampling;
sample introduction: communicating the first port K1, the third port K3, the sampler, the first port K4, the third port K6, the second port K8, the third port K9, the chromatographic column and the detector to form a sample injection path; the first carrier gas sends the sample gas in the sampler into the chromatographic column through the sample injection path to complete sample injection;
and (3) detection: the first carrier gas finishes the purging of the sampler through the first purging path, and the second carrier gas pushes the sample gas in the sample introduction process to continuously flow through the chromatographic column through the second purging path, so that the component separation is realized, the sample gas sequentially flows through the detector, and the detection of the sample gas is finished.
Optionally, when the sampler employs an enricher, the sampling comprises the steps of:
refrigerating: closing the first two-way solenoid valve and the second two-way solenoid valve to refrigerate the enricher;
enrichment: communicating the second port K2, the third port K3, the first two-way solenoid valve, the enricher, the second two-way solenoid valve, the first port K4, the second port K5 to form an enrichment path; sample gas completes adsorption in the enricher via the enrichment pathway;
and (3) analysis: and closing the first two-way electromagnetic valve and the second two-way electromagnetic valve, and heating the enricher to finish desorption.
Optionally, the temperature of the concentrator is 20 ℃ or less during refrigeration and 250 ℃ or more during desorption; the temperature of the enrichment device during enrichment is the same as the temperature during refrigeration, and the temperature of the enrichment device during sample injection is the same as the temperature during analysis.
Optionally, when the gas chromatography apparatus is a dual column gas chromatography apparatus, the detecting comprises the following paths:
detecting a path: the third port K9 and the first chromatographic column are communicated with the first inlet of the detector to form a detection path; the sample gas is subjected to separation detection through the detection path;
reference path: the second chromatographic column is communicated with the second inlet of the detector to form a detection path; a carrier gas provides a reference gas to the detector via the detection path.
As mentioned above, the gas chromatography device and the detection method based on the automatic sample injection of the electromagnetic valve have the following beneficial effects:
the electromagnetic valve can realize the functions of automatic purging, sampling, sample introduction, detection and the like of the gas chromatography device, and the miniature electromagnetic valve with low power consumption is adopted, so that the power consumption of the gas chromatography device can be reduced, and the gas chromatography device and the detection method based on the automatic sample introduction of the electromagnetic valve are favorable for realizing the low power consumption and the microminiaturization of the gas chromatography device based on the characteristics of small volume and light weight of the miniature electromagnetic valve, so that the operation convenience of the gas chromatography device is improved, and the application range of the gas chromatography device is expanded.
Drawings
Fig. 1 is a schematic structural diagram of a single-column gas chromatography apparatus based on electromagnetic valve automatic enrichment sampling according to an embodiment of the present invention.
Fig. 2 is a schematic structural diagram of a single-column gas chromatography apparatus based on electromagnetic valve automatic sample injection in the second embodiment of the present invention.
Fig. 3 is a schematic structural diagram of a dual-column gas chromatography device based on electromagnetic valve automatic enrichment sampling in the third embodiment of the present invention.
Fig. 4 is a schematic structural diagram of a dual-column gas chromatography device based on electromagnetic valve automatic sample injection in the fourth embodiment of the present invention.
Description of the element reference numerals
110. 130 enricher
120. 140 quantitative ring
210. 220 chromatographic column
231. 241 first chromatographic column
232. 242 second chromatography column
310. 320 detector
330. 340 two-way detector
410. 420, 430, 440 micropump
511. 521, 531, 541 first three-way electromagnetic valve
512. 522, 532 and 542 second three-way electromagnetic valve
513. 523, 533, 543 third three-way solenoid valve
611. 631 first two-way solenoid valve
612. 632 second two-way solenoid valve
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
As in the detailed description of the embodiments of the present invention, the cross-sectional views illustrating the device structures are not partially enlarged in general scale for convenience of illustration, and the schematic views are only examples, which should not limit the scope of the present invention. In addition, the three-dimensional dimensions of length, width and depth should be included in the actual fabrication.
For convenience in description, spatial relational terms such as "below," "beneath," "below," "under," "over," "upper," and the like may be used herein to describe one element or feature's relationship to another element or feature as illustrated in the figures. It will be understood that these terms of spatial relationship are intended to encompass other orientations of the device in use or operation in addition to the orientation depicted in the figures. Further, when a layer is referred to as being "between" two layers, it can be the only layer between the two layers, or one or more intervening layers may also be present. As used herein, "between … …" is meant to include both endpoints.
In the context of this application, a structure described as having a first feature "on" a second feature may include embodiments in which the first and second features are formed in direct contact, and may also include embodiments in which additional features are formed in between the first and second features, such that the first and second features may not be in direct contact.
It should be noted that the drawings provided in the present embodiment are only for illustrating the basic idea of the present invention, and the drawings only show the components related to the present invention rather than being drawn according to the number, shape and size of the components in actual implementation, and the type, quantity and proportion of each component in actual implementation may be changed freely, and the layout of the components may be more complicated.
The gas chromatography apparatus in this embodiment is an improvement based on an existing automatic gas chromatography apparatus, and therefore, reference may be made to the existing gas chromatography apparatus as to a control system, a circuit connection system, a display system, and the like of the gas chromatography apparatus.
The embodiment provides a gas chromatography device based on solenoid valve autoinjection, gas chromatography device includes:
a first three-way solenoid valve including a first port K1, a second port K2, and a third port K3;
a second three-way solenoid valve including a first port K4, a second port K5, and a third port K6;
a third three-way solenoid valve including a first port K7, a second port K8, and a third port K9;
a sampler comprising a sampler inlet and a sampler outlet;
a chromatography column comprising a chromatography column inlet and a chromatography column outlet;
a detector comprising a detector inlet and a detector outlet;
the first port K1 and the first port K7 are carrier gas inlets, the second port K2 is a sample gas inlet, and the second port K5 and the detector outlet are evacuation ports;
the third port K3 is connected with the sampler inlet, the first port K4 is connected with the sampler outlet, the third port K6 is connected with the second port K8, the third port K9 is connected with the chromatographic column inlet, and the chromatographic column outlet is connected with the detector inlet.
In the embodiment, the automatic sample introduction of the gas chromatography device can be realized based on the electromagnetic valve, the electromagnetic valve with low power consumption is adopted, the power consumption of the gas chromatography device can be reduced, and the gas chromatography device is beneficial to microminiaturization based on the characteristics of small size and light weight of the electromagnetic valve, so that the gas chromatography device based on the automatic sample introduction of the electromagnetic valve and the detection method are beneficial to realizing low power consumption and microminiaturization of the gas chromatography device, the operation convenience of the gas chromatography device is improved, and the application range is expanded.
By way of example, the sampler may include, but is not limited to, a dosing ring or an enricher.
As an example, when the sampler employs the enricher, the gas chromatography apparatus further comprises:
a first two-way solenoid valve including a first two-way solenoid valve inlet and a first two-way solenoid valve outlet;
a second two-way solenoid valve comprising a second two-way solenoid valve inlet and a second two-way solenoid valve outlet;
wherein, the first two-way solenoid valve entry with third port K3 is connected, the first two-way solenoid valve export is connected with the enricher entry, the second two-way solenoid valve entry is connected with the enricher export, the second two-way solenoid valve export with first port K4 is connected.
By way of example, the detector may include one of a hydrogen Flame Ionization Detector (FID), a Photo Ionization Detector (PID), and a Helium Ionization Detector (HID), but is not limited thereto.
As an example, the gas chromatography apparatus may comprise a dual column gas chromatography apparatus, wherein the dual column gas chromatography apparatus comprises:
a first chromatography column comprising a first chromatography column inlet and a first chromatography column outlet;
a second chromatography column comprising a second chromatography column inlet and a second chromatography column outlet;
a dual-path detector comprising a detector first inlet, a detector second inlet, a detector first outlet, and a detector second outlet;
the inlet of the second chromatographic column is a carrier gas inlet, and the first outlet of the detector and the second outlet of the detector are evacuation ports;
the first chromatographic column inlet is connected with the third port K9, the first chromatographic column outlet is connected with the first detector inlet, and the second chromatographic column outlet is connected with the second detector inlet.
By way of example, the detector in the dual column gas chromatography device may include, but is not limited to, a Thermal Conductivity Detector (TCD).
As an example, the gas chromatography apparatus may further include a micro pump, and a micro pump inlet of the micro pump is connected to the second port K5, and a micro pump outlet of the micro pump is a drain. So as to provide pressure for the gas through the micro pump, wherein the micro pump may be a pump with a small volume and weight, and the specific type is not limited herein.
As an example, the power consumption value of the solenoid valve is less than 1 watt; the size range of the electromagnetic valve is 1-10 cm; the weight range of the electromagnetic valve is 5-100 g.
Specifically, the solenoid valve may be a miniature solenoid valve, so as to further provide the solenoid valve with low power consumption, small volume and light weight, wherein the power consumption value of the solenoid valve may be less than 1 watt, such as, but not limited to, 0.2 watt, 0.5 watt, 0.8 watt, and the like; the size range of the electromagnetic valve can be 1 cm-10 cm, such as 1 cm, 5 cm, 8 cm, 10 cm and the like, but is not limited thereto; the weight of the solenoid valve may range from 5 grams to 100 grams, such as 5 grams, 10 grams, 20 grams, 50 grams, 100 grams, and the like, but is not limited thereto.
As an example, the quantification ring, the concentrator, the chromatography column and the detector may be a quantification ring, a concentrator, a chromatography column and a detector prepared based on a conventional process, or a quantification ring, a concentrator, a chromatography column and a detector chip prepared based on a Micro Electro Mechanical System (MEMS) technology.
The embodiment also provides a detection method of the gas chromatography device, which comprises the following steps:
providing any one of the above gas chromatography apparatuses, starting the gas chromatography apparatus, and performing the following operations:
purging: communicating the first port K1, the third port K3, the sampler, the first port K4 and the second port K5 to form a first purge path; communicating the first port K7, third port K9, chromatography column and detector to form a second purge path; a first carrier gas completes the purging of the sampler through the first purging path; a second carrier gas completes the purging of the chromatographic column and the detector through the second purging path;
sampling: the second port K2, the third port K3, the sampler, the first port K4 and the second port K5 are communicated to form a sampling path; the sampling path is used for filling the sampler with sample gas to finish sampling;
sample introduction: communicating the first port K1, the third port K3, the sampler, the first port K4, the third port K6, the second port K8, the third port K9, the chromatographic column and the detector to form a sample injection path; the first carrier gas sends the sample gas in the sampler into the chromatographic column through the sample injection path to complete sample injection;
and (3) detection: the first carrier gas finishes the purging of the sampler through the first purging path, and the second carrier gas pushes the sample gas in the sample introduction process to continuously flow through the chromatographic column through the second purging path, so that the component separation is realized, the sample gas sequentially flows through the detector, and the detection of the sample gas is finished.
As an example, when the sampler employs an enricher, the sampling comprises the steps of:
refrigerating: closing the first two-way solenoid valve and the second two-way solenoid valve to refrigerate the enricher;
enrichment: communicating the second port K2, the third port K3, the first two-way solenoid valve, the enricher, the second two-way solenoid valve, the first port K4, the second port K5 to form an enrichment path; sample gas completes adsorption in the enricher via the enrichment pathway;
and (3) analysis: and closing the first two-way electromagnetic valve and the second two-way electromagnetic valve, and heating the enricher to finish desorption.
By way of example, but not limitation, the temperature of the concentrator during refrigeration is preferably less than or equal to 20 ℃, such as-5 ℃, 10 ℃, 15 ℃, etc. The temperature of the enriching device during desorption is preferably more than or equal to 250 ℃, such as 250 ℃, 300 ℃, 400 ℃, 500 ℃ and the like, but not limited to the temperature; the temperature of the enrichment device during enrichment is the same as the temperature during refrigeration, and the temperature of the enrichment device during sample injection is the same as the temperature during analysis.
As an example, when the gas chromatography apparatus is a dual column gas chromatography apparatus, the detecting comprises the following paths:
detecting a path: the third port K9, the first chromatographic column and the first inlet of the detector are communicated to form a detection path; the sample gas is subjected to separation detection through the detection path;
reference path: the second chromatographic column is communicated with a second inlet of the detector to form a detection path; a carrier gas provides a reference gas to the detector via the detection path.
The present invention will be further described with reference to the following specific embodiments and accompanying drawings.
Example one
As shown in fig. 1, the present embodiment provides a single-column gas chromatography apparatus based on electromagnetic valve for automatic enrichment and sample injection, the gas chromatography apparatus includes: the enricher 110, the chromatography column 210, the detector 310, the micro-pump 410, the first three-way solenoid valve 511, the second three-way solenoid valve 512, the third three-way solenoid valve 513, the first two-way solenoid valve 611, and the second two-way solenoid valve 612. Wherein the concentrator 110, the chromatographic column 210 and the detector 310 can be a quantitative ring, a concentrator, a chromatographic column and a detector prepared based on a conventional process, or a concentrator, a chromatographic column and a detector chip prepared based on a micro-electro-mechanical system (MEMS) technology.
Referring to fig. 1, the detector 310 may be a hydrogen Flame Ionization Detector (FID), a Photo Ionization Detector (PID), or a Helium Ionization Detector (HID), but the type of the detector 310 is not limited thereto. In this embodiment, the detector 310 has only one flow path, and thus only one of the columns 210 needs to be connected thereto. The first two-way solenoid valve 611, the enricher 110 and the second two-way solenoid valve 612 are connected as the sampler, and the micro pump 410 is adopted in this embodiment to provide power for gas flow. In this embodiment, the electromagnetic valves are all micro electromagnetic valves, but not limited thereto, and the types and models of the micro electromagnetic valves can be selected according to the needs, which is not limited herein.
Specifically, the first three-way solenoid valve 511 includes a first port K1, a second port K2, and a third port K3; the first two-way solenoid valve 611 includes a first two-way solenoid valve inlet and a first two-way solenoid valve outlet; the enricher 110 comprises an enricher inlet and an enricher outlet; the second two-way solenoid valve 612 comprises a second two-way solenoid valve inlet and a second two-way solenoid valve outlet; the second three-way solenoid valve 512 includes a first port K4, a second port K5, and a third port K6; the third three-way solenoid valve 513 includes a first port K7, a second port K8, and a third port K9; the chromatography column 210 comprises a chromatography column inlet and a chromatography column outlet; the detector 310 comprises a detector inlet and a detector outlet; the micro pump 410 includes a micro pump inlet and a micro pump outlet.
The first port K1 is a carrier gas inlet C1, the first port K7 is a carrier gas inlet C2, the second port K2 is a sample gas inlet S, the outlet of the micro pump is an evacuation port O1, and the outlet of the detector is an evacuation port O2.
Third port K3 with first two-way solenoid valve entry is connected, first two-way solenoid valve export with the enricher entry is connected, second two-way solenoid valve entry is connected with the enricher export, second two-way solenoid valve export with first port K4 is connected, second port K5 with the micropump entry is connected, third port K6 with second port K8 is connected, third port K9 with the chromatographic column entry is connected, the chromatographic column export with the detector entry is connected.
When the electromagnetic valve-based single-column gas chromatography device for automatic enrichment and sample introduction is adopted for detection, the gas chromatography device is firstly opened, and then the main working process is as follows:
purging: the first port K1 and the third port K3 of the first three-way solenoid valve 511 are communicated with each other, the first port K4 and the second port K5 of the second three-way solenoid valve 512 are communicated with each other, the first two-way solenoid valve 611 and the second two-way solenoid valve 612 are communicated with each other, the micro pump 410 is started, and the first port K7 and the third port K9 of the third three-way solenoid valve 513 are communicated with each other. One path of carrier gas flows through the first two-way solenoid valve 611, the enricher 110, the second two-way solenoid valve 612, the first port K4 of the second three-way solenoid valve 512, and the second port K5 from the first port K1 and the third port K3 of the first three-way solenoid valve 511 through the carrier gas inlet C1, and finally flows out through the micro pump 410 and the evacuation port O1, and purging of the enricher 110 is completed, in this process, the enricher 110 is maintained at a high temperature of not less than 250 ℃, and the specific temperature can be set as required. Meanwhile, another carrier gas flows through the chromatography column 210 and the detector 310 from the first port K7 and the third port K9 of the third three-way solenoid valve 513 through the carrier gas inlet C2, and finally flows out of the evacuation port O2.
Refrigerating: the first three-way solenoid valve 511, the second three-way solenoid valve 512, and the third three-way solenoid valve 513 are in the same state as the purging process, the first two-way solenoid valve 611 and the second two-way solenoid valve 612 are turned off, and the micro pump 410 is turned off. At this point, the concentrator 110 is chilled to a temperature of 20 ℃ or below 20 ℃ and stabilized at a suitable temperature, with the specific temperature set as needed to prepare for the next enrichment sample. At this time, another carrier gas still flows through the chromatography column 210 and the detector 310 from the first port K7 and the third port K9 of the third three-way solenoid valve 513 through the carrier gas inlet C2, and finally flows out of the evacuation port O2.
Enrichment: the second port K2 and the third port K3 of the first three-way solenoid valve 511 are communicated, the first port K4 and the second port K5 of the second three-way solenoid valve 512 are communicated, the first two-way solenoid valve 611 and the second two-way solenoid valve 612 are communicated, the micro pump 410 is started, and the first port K7 and the third port K9 of the third three-way solenoid valve 513 are communicated. The sample gas flows through the first two-way solenoid valve 611, the enricher 110, the second two-way solenoid valve 612, the first port K4 of the second three-way solenoid valve 512, and the second port K5 from the second port K2 and the third port K3 of the first three-way solenoid valve 511 through the sample gas inlet S, and finally flows out through the micro pump 410 and the evacuation port O1, the sample gas is adsorbed in the enricher 110, enrichment is completed, and the enricher 110 maintains a low temperature set in a refrigeration process in this process. At this time, another carrier gas still flows through the chromatography column 210 and the detector 310 from the first port K7 and the third port K9 of the third three-way solenoid valve 513 through the carrier gas inlet C2, and finally flows out of the evacuation port O2.
And (3) analysis: the states of the first three-way solenoid valve 511, the second three-way solenoid valve 512 and the third three-way solenoid valve 513 are the same as the state in the purging process, the first two-way solenoid valve 611 and the second two-way solenoid valve 612 are turned off, and the micro pump 410 is turned off. At this time, the concentrator 110 is heated to a temperature of not less than 250 ℃, and is stabilized at a suitable temperature, which is set as required, so that the sample gas enriched at a low temperature will be desorbed at a high temperature. At this time, another carrier gas still flows through the chromatography column 210 and the detector 310 from the first port K7 and the third port K9 of the third three-way solenoid valve 513 through the carrier gas inlet C2, and finally flows out of the evacuation port O2.
Sample introduction: the first port K1 and the third port K3 of the first three-way solenoid valve 511 are communicated, the first port K4 and the third port K6 of the second three-way solenoid valve 512 are communicated, the first two-way solenoid valve 611 and the second two-way solenoid valve 612 are communicated, the micro pump 410 is closed, and the second port K8 and the third port K9 of the third three-way solenoid valve 513 are communicated. A path of carrier gas flows from the first port K1 and the third port K3 of the first three-way solenoid valve 511 through the first two-way solenoid valve 611, the enricher 110, the second two-way solenoid valve 612, the first port K4 of the second three-way solenoid valve 512, the third port K6, the second port K8 of the third three-way solenoid valve 513, the third port K9, the chromatographic column 210 via the carrier gas inlet C1, finally flows through the detector 310 and flows out of the evacuation port O2; while the carrier gas from the carrier gas inlet C2 is cut off. In this process, the temperature of the enricher 110 is the same as the temperature in the desorption process. The sample gas thus desorbed is carried into the chromatography column 210 by the carrier gas.
And (3) detection: the first port K1 and the third port K3 of the first three-way solenoid valve 511 are communicated, the first port K4 and the second port K5 of the second three-way solenoid valve 512 are communicated, the first two-way solenoid valve 611 and the second two-way solenoid valve 612 are communicated, the micro pump 410 is started, and the first port K7 and the third port K9 of the third three-way solenoid valve 513 are communicated. One path of carrier gas flows through the first two-way solenoid valve 611, the enricher 110, the second two-way solenoid valve 612, the first port K4 of the second three-way solenoid valve 512, and the second port K5 from the first port K1 and the third port K3 of the first three-way solenoid valve 511 through the carrier gas inlet C1, and finally flows out through the micro pump 410 and the evacuation port O1 thereof, and purging of the enricher 110 is completed, wherein the temperature of the enricher 110 in the process is the same as the temperature in the analytic process. Meanwhile, the carrier gas from the carrier gas inlet C2 flows into the chromatographic column 210 from the first port K7 and the third port K9 of the third three-way electromagnetic valve 513, and pushes the sample gas in the sample injection process to continuously flow through the chromatographic column 210, so that component separation is realized, the sample gas sequentially flows through the detector 310, and finally flows out from the evacuation port O2, and the detection of the sample gas is completed.
Since the purge has been completed during the test step, if the test is continued, a second test may be started directly from the cooling step.
Example two
Referring to fig. 2, the present embodiment provides a single column gas chromatography device based on electromagnetic valve automatic sample injection, which is different from the first embodiment mainly in that: in this embodiment, the metering ring 120 replaces the enricher 110 of embodiment one, and the first two-way solenoid 611 and the second two-way solenoid 612 are eliminated. The gas chromatography apparatus of the present embodiment includes: the quantitative ring 120, the chromatographic column 220, the detector 320, the micro pump 420, the first three-way solenoid valve 521, the second three-way solenoid valve 522 and the third three-way solenoid valve 523. For specific connection, reference may be made to the first embodiment, which is not described herein. The quantitative ring 120, the chromatographic column 220 and the detector 320 may be quantitative rings, chromatographic columns and detectors prepared based on conventional processes, or quantitative rings, chromatographic columns and detector chips prepared based on micro-electro-mechanical systems (MEMS) technology.
When the single-column gas chromatography device based on the automatic sample injection of the electromagnetic valve is adopted for detection, the gas chromatography device is firstly opened, and then the main working process is as follows:
purging: the first port K1 and the third port K3 of the first three-way solenoid valve 521 are communicated with each other, the first port K4 and the second port K5 of the second three-way solenoid valve 522 are communicated with each other, the micro pump 420 is turned on, and the first port K7 and the third port K9 of the third three-way solenoid valve 523 are communicated with each other. One path of carrier gas flows through the dosing ring 120, the first port K4 of the second three-way electromagnetic valve 522, the second port K5 from the first port K1 and the third port K3 of the first three-way electromagnetic valve 521 through the carrier gas inlet C1, and finally flows out through the micro pump 420 and the evacuation port O1, so that the purging of the dosing ring 120 is completed. Meanwhile, another carrier gas flows through the chromatography column 220 and the detector 320 from the first port K7 and the third port K9 of the third three-way solenoid valve 523 via the carrier gas inlet C2, and finally flows out of the evacuation port O2.
Sampling: the second port K2 and the third port K3 of the first three-way solenoid valve 521 are communicated, the first port K4 and the second port K5 of the second three-way solenoid valve 522 are communicated, the micro pump 420 is started, and the first port K7 and the third port K9 of the third three-way solenoid valve 523 are communicated. The sample gas flows through the quantitative ring 120, the first port K4 of the second three-way solenoid valve 522, the second port K5 from the second port K2 and the third port K3 of the first three-way solenoid valve 521 through the sample gas inlet S, and finally flows out through the micro pump 420 and the evacuation port O1, and the quantitative ring 220 is filled with the sample gas, thereby completing sampling. At this time, another carrier gas still flows through the chromatographic column 220 and the detector 320 from the first port K7 and the third port K9 of the third three-way solenoid valve 523 through the carrier gas inlet C2, and finally flows out of the evacuation port O2.
Sample introduction: the first port K1 and the third port K3 of the first three-way solenoid valve 521 are communicated, the first port K4 and the third port K6 of the second three-way solenoid valve 522 are communicated, the micro pump 420 is closed, and the second port K8 and the third port K9 of the third three-way solenoid valve 523 are communicated. One path of carrier gas flows through the quantitative ring 220, the first port K4 of the second three-way solenoid valve 522, the third port K6, the second port K8 of the third three-way solenoid valve 523, the third port K9, the chromatographic column 220 from the first port K1 and the third port K3 of the first three-way solenoid valve 521 through the carrier gas inlet C1, finally flows through the detector 320 and flows out from the evacuation port O2, and the sample gas in the quantitative ring 220 is sent into the chromatographic column 220 by the carrier gas. While the carrier gas from the carrier gas inlet C2 is cut off.
And (3) detection: the first port K1 and the third port K3 of the first three-way solenoid valve 521 are communicated, the first port K4 and the second port K5 of the second three-way solenoid valve 522 are communicated, the micro pump 420 is started, and the first port K7 and the third port K9 of the third three-way solenoid valve 523 are communicated. One path of carrier gas flows through the dosing ring 120, the first port K4 of the second three-way solenoid valve 522, the second port K5 from the first port K1 and the third port K3 of the first three-way solenoid valve 511 through the carrier gas inlet C1, and finally flows out through the micro pump 420 and the evacuation port O1 thereof, so that the purging of the dosing ring 120 is completed. Meanwhile, the carrier gas from the carrier gas inlet C2 flows into the chromatographic column 220 from the first port K7 and the third port K9 of the third three-way electromagnetic valve 523, and pushes the sample gas in the sample injection process to continuously flow through the chromatographic column 220, so that component separation is realized, the sample gas sequentially flows through the detector 320, and finally flows out of the evacuation port O2, and the detection of the sample gas is completed.
Since the purging is completed at the detection step, the second test may start directly from the sampling step if the tests are continued.
EXAMPLE III
Referring to fig. 3, the present embodiment provides a dual-column gas chromatography apparatus based on electromagnetic valve automatic enrichment sampling, wherein the related detector adopts a dual-path detector 330, the dual-column gas chromatography apparatus includes: an enricher 130, a first chromatographic column 231, a second chromatographic column 232, a two-way detector 330, a micro-pump 430, a first three-way solenoid valve 531, a second three-way solenoid valve 532, a third three-way solenoid valve 533, a first two-way solenoid valve 631, and a second two-way solenoid valve 632. The concentrator 130, the first chromatographic column 231, the second chromatographic column 232 and the two-way detector 330 may be prepared based on a conventional process, or may be prepared based on micro-electro-mechanical systems (MEMS) technology.
Referring to fig. 3, the dual path detector 330 is a Thermal Conductivity Detector (TCD), but not limited to this, the dual path detector 330 has two flow paths, and two chromatography columns, i.e. the first chromatography column 231 and the second chromatography column 232, are connected to the two flow paths: wherein the first chromatography column 231 comprises a first chromatography column inlet and a first chromatography column outlet; the second chromatography column 232 comprises a second chromatography column inlet and a second chromatography column outlet; the two-way detector 330 comprises a first detector inlet, a second detector inlet, a first detector outlet, and a second detector outlet; the inlet of the second chromatographic column is a carrier gas inlet C3, the first outlet of the detector is an evacuation port O2, and the second outlet of the detector is an evacuation port O3; the first chromatographic column inlet is connected with a third port K9 of the third three-way solenoid valve 523, the first chromatographic column outlet is connected with the first detector inlet, and the second chromatographic column outlet is connected with the second detector inlet. For other specific connections, reference may be made to the first embodiment, which is not described herein.
Wherein, the sample gas is separated when flowing through the first chromatographic column 231 under the driving of the carrier gas, flows through the two-way detector 330 for detection, and flows out from the first outlet of the detector of the two-way detector 330, i.e. the evacuation port O2, and this flow path is called a detection path; the second chromatographic column inlet of the second chromatographic column 232 is directly connected with a carrier gas as the carrier gas inlet C3, the second chromatographic column outlet of the second chromatographic column 232 is connected with the second detector inlet of the two-way detector 330, the carrier gas flows through the second chromatographic column 232 from the carrier gas inlet C3, enters another flow path of the two-way detector 330, and flows out from the evacuation port O3 of the two-way detector 330, and this flow path provides a reference gas for the detector, which is called a reference path.
When the electromagnetic valve-based automatic enrichment sample injection double-column gas chromatography device is adopted for detection, the gas chromatography device is firstly opened, and then the main working process is as follows:
purging: the first port K1 and the third port K3 of the first three-way solenoid valve 531 are communicated with each other, the first port K4 and the second port K5 of the second three-way solenoid valve 532 are communicated with each other, the first two-way solenoid valve 631 and the second two-way solenoid valve 632 are connected with each other, the micro pump 430 is started, and the first port K7 and the third port K9 of the third three-way solenoid valve 533 are communicated with each other. One path of carrier gas flows through the first port K1 and the third port K3 of the first three-way solenoid valve 531 from the carrier gas inlet C1, flows through the first two-way solenoid valve 631, the enricher 130, the second two-way solenoid valve 632, the first port K4 and the second port K5 of the second three-way solenoid valve 532, and finally flows out through the micro pump 430 and the evacuation port O1, and purging of the enricher 130 is completed, wherein in the process, the enricher 130 is maintained at a high temperature of not less than 250 ℃, and the specific temperature can be set as required. At the same time, the gas flowing through the two-way detector 330 is a two-way carrier gas: a channel of carrier gas flows through a channel of the first chromatographic column 231 and the two-way detector 330 from the first port K7 and the third port K9 of the third three-way solenoid valve 533 via a carrier gas inlet C2, and finally flows out of the evacuation port O2; the other path of the carrier gas flows through the second chromatographic column 232 from the carrier gas inlet C3, enters the other path of the two-path detector 330, and flows out from the evacuation port O3, at this time, the carrier gas passes through both paths of the two-path detector 330, and no signal is output.
Refrigerating: the states of the first three-way solenoid valve 531, the second three-way solenoid valve 532, and the third three-way solenoid valve 533 are the same as the state of the purge process, the first two-way solenoid valve 631 and the second two-way solenoid valve 632 are turned off, and the micro pump 430 is turned off. At this point, the enricher 130 is chilled to reduce its temperature to 20 ℃ or below 20 ℃ and stabilized at a suitable temperature, with the specific temperature set as needed to prepare for the next enrichment sample. At this time, the two-way detector 330 still has two carrier gases from the carrier gas inlet C2 and the carrier gas inlet C3, and the two-way detector has no signal output at this time, as in the purging process.
Enrichment: the second port K2 and the third port K3 of the first three-way solenoid valve 531 are communicated, the first port K4 and the second port K5 of the second three-way solenoid valve 532 are communicated, the first two-way solenoid valve 631 and the second two-way solenoid valve 632 are communicated, the micro pump 430 is started, and the first port K7 and the third port K9 of the third three-way solenoid valve 533 are communicated. The sample gas flows through the first two-way solenoid valve 631, the enricher 130, the second two-way solenoid valve 632, the first port K4 of the second three-way solenoid valve 532, and the second port K5 from the second port K2 and the third port K3 of the first three-way solenoid valve 531 through the sample gas inlet S, and finally flows out through the micro pump 430 and the evacuation port O1, the sample gas is adsorbed in the enricher 130 to complete enrichment, and the enricher 130 maintains the low temperature set in the refrigeration process in this process. At this time, the two-way detector 330 still has two carrier gases from the carrier gas inlet C2 and the carrier gas inlet C3 flowing through the two-way detector 330, and the two-way detector 330 has no signal output as in the purging process.
And (3) analysis: the states of the first three-way solenoid valve 531, the second three-way solenoid valve 532 and the third three-way solenoid valve 533 are the same as the state of the purging process, the first two-way solenoid valve 631 and the second two-way solenoid valve 632 are turned off, and the micro pump 430 is turned off. At this time, the enricher 130 is heated to a temperature of not less than 250 ℃ and stabilized at a suitable temperature, which is set as required, so that the sample gas enriched at a low temperature will be desorbed at a high temperature. The two-way detector 330 is still flowing two-way carrier gas from the carrier gas inlet C2 and carrier gas inlet C3, as is the case during purging, at which point the two-way detector has no signal output.
Sample introduction: the first port K1 and the third port K3 of the first three-way solenoid valve 531 are communicated, the first port K4 and the third port K6 of the second three-way solenoid valve 532 are communicated, the first two-way solenoid valve 631 and the second two-way solenoid valve 632 are communicated, the micro pump 430 is closed, and the second port K8 and the third port K9 of the third three-way solenoid valve 533 are communicated. One path of carrier gas flows from the first port K1 and the third port K3 of the first three-way solenoid valve 531, through the first two-way solenoid valve 631, the enricher 130, the second two-way solenoid valve 632, the first port K4 of the second three-way solenoid valve 532, the third port K6, the second port K8 of the third three-way solenoid valve 533, the third port K9 and the first chromatographic column 231 via the carrier gas inlet C1, finally flows through the two-way detector 330 and flows out of the exhaust port O2; while the carrier gas from the carrier gas inlet C2 is turned off; the carrier gas from carrier gas inlet C3 still passes through the second chromatography column 232 and the dual path detector 330 and out the vent O3. At this point the enricher temperature is the same as the temperature during desorption. The sample gas thus resolved is carried into the first chromatographic column 231 by a carrier gas.
And (3) detection: the first port K1 and the third port K3 of the first three-way solenoid valve 531 are communicated, the first port K4 and the second port K5 of the second three-way solenoid valve 532 are communicated, the first two-way solenoid valve 631 and the second two-way solenoid valve 632 are communicated, the micro pump 430 is started, and the first port K7 and the third port K9 of the third three-way solenoid valve 533 are communicated. One path of carrier gas flows through the first two-way solenoid valve 631, the enricher 110, the second two-way solenoid valve 632, the first port K4 and the second port K5 of the second three-way solenoid valve 532 from the first port K1 and the third port K3 of the first three-way solenoid valve 531 through the carrier gas inlet C1, and finally flows out through the micro pump 430 and the evacuation port O1, and purging of the enricher 130 is completed, wherein the temperature of the enricher 130 in the process is the same as the temperature in the analytic process. The gas flowing through the two-way detector 330 is the two-way carrier gas from the carrier gas inlet C2 and the carrier gas inlet C3, the state is the same as that in the purging process, the sample gas from the sample injection process continuously flows through the first chromatographic column 231 under the pushing of the carrier gas from the carrier gas inlet C2 to realize component separation, and then sequentially flows through the two-way detector 330, and finally flows out from the evacuation port O2; the carrier gas from the carrier gas inlet C3 still passes through the second chromatography column 232 and the dual path detector 330 and flows out of the vent O3. Since the two-way detector 330 has a flow path through which pure carrier gas flows and a flow path through which the carrier gas carries the separated sample gas components, the two-way detector 330 outputs a detection signal to complete the detection of the sample gas.
Since the purge has been completed during the test step, if the test is continued, a second test may be started directly from the cooling step.
Example four
Referring to fig. 4, the present embodiment provides a dual-column gas chromatography device based on electromagnetic valve auto-sampling, which is different from the third embodiment in that: in this embodiment, the metering ring 140 replaces the enricher 130 of the third embodiment and the first two-way solenoid 631 and the second two-way solenoid 632 are eliminated. The gas chromatography apparatus includes: a quantitative loop 140, a first chromatographic column 241, a second chromatographic column 242, a two-way detector 340, a micro pump 440, a first three-way solenoid valve 541, a second three-way solenoid valve 542, and a third three-way solenoid valve 543. For specific connection, reference may be made to the third embodiment, which is not described herein. The quantitative ring 140, the first chromatographic column 241, the second chromatographic column 242 and the two-way detector 340 may be a quantitative ring, a chromatographic column and a detector prepared based on a conventional process, or a quantitative ring, a chromatographic column and a detector chip prepared based on a Micro Electro Mechanical System (MEMS) technology.
When the double-column gas chromatography device based on the automatic sample introduction of the electromagnetic valve is adopted for detection, the gas chromatography device is firstly opened, and then the main working process is as follows:
purging: the first port K1 and the third port K3 of the first three-way solenoid valve 541 are communicated with each other, the first port K4 and the second port K5 of the second three-way solenoid valve 542 are communicated with each other, the micro pump 440 is turned on, and the first port K7 and the third port K9 of the third three-way solenoid valve 543 are communicated with each other. One path of carrier gas flows through the dosing ring 140, the first port K4 of the second three-way solenoid valve 542, the second port K5 from the first port K1 and the third port K3 of the first three-way solenoid valve 541 through the carrier gas inlet C1, and finally flows out through the micro pump 440 and the evacuation port O1, so that the purging of the dosing ring 140 is completed. At the same time, the gas flowing through the two-way detector 340 is a two-way carrier gas: one path of carrier gas flows through a flow path of the first chromatographic column 241 and the two-way detector 340 from the first port K7 and the third port K9 of the third three-way electromagnetic valve 543 through the carrier gas inlet C2, and finally flows out of an exhaust port O2; the other path of carrier gas flows through the second chromatographic column 242 from the carrier gas inlet C3, enters the other flow path of the two-path detector 340, and flows out from the evacuation port O3 of the two-path detector 340, at this time, the carrier gas passes through both flow paths of the two-path detector 340, and no signal is output.
Sampling: the second port K2 and the third port K3 of the first three-way solenoid valve 541 are communicated, the first port K4 and the second port K5 of the second three-way solenoid valve 542 are communicated, the micro pump 440 is turned on, and the first port K7 and the third port K9 of the third three-way solenoid valve 543 are communicated. The sample gas flows through the dosing ring 140, the first port K4 of the second three-way solenoid valve 542, the second port K5 from the second port K2 and the third port K3 of the first three-way solenoid valve 541 through the sample gas inlet S, and finally flows out through the micro pump 440 and the evacuation port O1, and the sample gas fills the dosing ring 240, thereby completing sampling. At this time, the two-way carrier gas from the carrier gas inlet C2 and the carrier gas inlet C3 still flows through the two-way detector 340, and the detector outputs no signal as in the purging process.
Sample introduction: the first port K1 and the third port K3 of the first three-way solenoid valve 541 are communicated, the first port K4 and the third port K6 of the second three-way solenoid valve 542 are communicated, the micro pump 440 is turned off, and the second port K8 and the third port K9 of the third three-way solenoid valve 543 are communicated. A path of carrier gas flows through the quantitative ring 240, the first port K4 of the second three-way solenoid valve 542, the third port K6, the second port K8 of the third three-way solenoid valve 543, the third port K9, and the first chromatographic column 241 from the first port K1 and the third port K3 of the first three-way solenoid valve 541 through the carrier gas inlet C1, finally flows through the two-way detector 340 and flows out of the exhaust port O2; while the carrier gas from the carrier gas inlet C2 is turned off; the carrier gas from the carrier gas inlet C3 still passes through the second chromatographic column 242 and the dual path detector 340 and flows out of the evacuation port O3 of the dual path detector 340. The sample gas in the quantitative ring 140 is fed into the first chromatographic column 241 by a carrier gas.
And (3) detection: the first port K1 and the third port K3 of the first three-way solenoid valve 541 are communicated, the first port K4 and the second port K5 of the second three-way solenoid valve 542 are communicated, the micro pump 440 is turned on, and the first port K7 and the third port K9 of the third three-way solenoid valve 543 are communicated. One path of carrier gas flows through the dosing ring 140 from the first port K1 and the third port K3 of the first three-way solenoid valve 541 through the carrier gas inlet C1, the first port K4 and the second port K5 of the second three-way solenoid valve 542, and finally flows out through the micro pump 440 and the evacuation port O1, so that the dosing ring 140 is purged. The gas flowing through the two-way detector 340 is the two-way carrier gas from the carrier gas inlet C2 and carrier gas inlet C3, and is the same as during purging: the sample gas from the sample injection process continuously flows through the first chromatographic column 241 under the pushing of the carrier gas from the carrier gas inlet C2 to realize component separation, and sequentially flows through the two-way detector 340, and finally flows out of the evacuation port O2; the carrier gas from the carrier gas inlet C3 still passes through the second chromatographic column 242 and the dual path detector 340 and flows out of the evacuation O3 of the dual path detector 340. Since the pure carrier gas flows through one flow path of the two-way detector 340, the carrier gas in one flow path carries the separated sample gas component, and the two-way detector 340 outputs a detection signal to complete the detection of the sample gas.
Since the purging is completed at the detection step, the second test may start directly from the sampling step if the tests are continued.
It should be noted that the micropump in the above four embodiments can also be eliminated if the sample gas itself has a certain pressure, and the sample gas enters the enricher or the quantitative ring by the pressure of the sample gas itself to complete enrichment or sampling.
In summary, the gas chromatography device and the detection method based on the automatic sample injection of the electromagnetic valve have the following beneficial effects:
the electromagnetic valve can realize the functions of automatic purging, sampling, sample introduction, detection and the like of the gas chromatography device, and the miniature electromagnetic valve with low power consumption is adopted, so that the power consumption of the gas chromatography device can be reduced, and the gas chromatography device and the detection method based on the automatic sample introduction of the electromagnetic valve are favorable for realizing the low power consumption and the microminiaturization of the gas chromatography device based on the characteristics of small volume and light weight of the miniature electromagnetic valve, so that the operation convenience of the gas chromatography device is improved, and the application range of the gas chromatography device is expanded.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (12)
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