CN113219108A - Gas chromatograph - Google Patents

Gas chromatograph Download PDF

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Publication number
CN113219108A
CN113219108A CN202110700342.4A CN202110700342A CN113219108A CN 113219108 A CN113219108 A CN 113219108A CN 202110700342 A CN202110700342 A CN 202110700342A CN 113219108 A CN113219108 A CN 113219108A
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China
Prior art keywords
interface
gas
carrier gas
chromatographic column
quantitative
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CN202110700342.4A
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Chinese (zh)
Inventor
蒲友强
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Chengdu Chang Ai Electronic Science & Technology Co ltd
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Chengdu Chang Ai Electronic Science & Technology Co ltd
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/16Injection
    • G01N30/20Injection using a sampling valve
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N2030/022Column chromatography characterised by the kind of separation mechanism
    • G01N2030/025Gas chromatography
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/16Injection
    • G01N30/20Injection using a sampling valve
    • G01N2030/201Injection using a sampling valve multiport valves, i.e. having more than two ports

Abstract

The present invention relates to a gas chromatograph. The gas chromatograph comprises a six-way pneumatic valve, a ten-way pneumatic valve, a pneumatic reversing valve, a stop valve, a first chromatographic column, a second chromatographic column, a first quantitative tube, a second quantitative tube, a sampling device, a first carrier gas introduction device and a first detection device. By connecting the components in a certain way, the gas chromatograph can be effectively adapted to the high-temperature working environment. And through the configuration of the six-way pneumatic valve, the ten-way pneumatic valve and the pneumatic reversing valve, the whole gas circuit can keep a better balance state relative to the ambient atmospheric pressure, and the accuracy of a later-period detection result is improved beneficially. In addition, the gas chromatograph is used for one-time sample injection, and system errors caused by multiple sample injections are effectively reduced.

Description

Gas chromatograph
Technical Field
The present invention relates to a gas chromatograph.
Background
The gas chromatograph is a chromatographic analysis device using gas as a mobile phase. The main work flow of the gas chromatograph comprises volume sampling, sample introduction separation and purging. Wherein, sampling refers to the process that a sample enters the chromatograph from a sample gas inlet and flows out of the chromatograph from a sample gas outlet, so that the sample washes the quantitative tube and ensures the sample volume in the quantitative tube to be constant. Under the influence of factors such as pressure, temperature, the sample volume of gathering in the quantification pipe can't keep invariable, so the pipeline of chromatograph and sample processing part need all to be placed in the thermostat, require pipeline, sample processing equipment can tolerate high temperature.
In the prior art, an electromagnetic valve is usually used as a switching valve of a balance gas circuit, and the common electromagnetic valve cannot resist high temperature. When the electromagnetic valve works in a high-temperature environment for a long time, the performance of the electromagnetic valve is affected, so that the use requirement is difficult to meet. For the high temperature resistant solenoid valve, the price is very expensive, and many enterprises or laboratories cannot accept the high equipment cost.
Aiming at some defects of the existing electromagnetic valve, a more reasonable technical scheme is required to be provided, so that the electromagnetic valve can effectively balance the gas circuit and adapt to a high-temperature working environment.
Disclosure of Invention
The invention provides a gas chromatograph, which can effectively balance gas paths and adapt to a high-temperature working environment.
In order to realize the effect, the invention adopts the technical scheme that:
a gas chromatograph comprises a six-way pneumatic valve, a ten-way pneumatic valve, a pneumatic reversing valve, a stop valve, a sampling device, a first chromatographic column, a second chromatographic column, a first quantitative tube, a second quantitative tube, a first carrier gas introduction device and a first detection device;
wherein the six-way pneumatic valve has an S1 port, an S2 port, an S3 port, an S4 port, an S5 port, and an S6 port arranged in series in a first direction, the ten-way pneumatic valve has a P1 port, a P2 port, a P3 port, a P4 port, a P5 port, a P6 port, a P7 port, a P8 port, a P9 port, and a P10 port arranged in series in the first direction, and the pneumatic directional valve has a Q1 port, a Q2 port, a Q3 port, a Q4 port, a Q5 port, and a Q6 port arranged in series in the first direction, the first direction being either clockwise or counterclockwise;
the S1 interface is connected to a sample gas outlet of the sampling device, the S2 interface is connected to a sample gas inlet of the sampling device, the S3 interface is connected to the P1 interface, the S4 interface is connected to a drain port, the S5 interface is connected to the stop valve, and the S6 interface is connected to the Q3 interface;
the first carrier gas introducing device is used for introducing carrier gas A and is provided with a first carrier gas pipe, a second carrier gas pipe and a third carrier gas pipe, the first carrier gas pipe is connected with the P7 interface, the second carrier gas pipe is connected with the P4 interface, and the third carrier gas pipe is connected with the Q6 interface;
the P8 interface is externally connected with an exhaust gas discharge port;
one end of the first chromatographic column is connected to the P5 interface, and the other end of the first chromatographic column is connected to the P9 interface; the first detection device is connected to the P6 interface; one end of the second chromatographic column is connected to the first detection device, and the other end of the second chromatographic column is connected to the Q5 interface;
one end of the first quantitative pipe is connected to the P3 interface, and the other end of the first quantitative pipe is connected to the P10 interface; one end of the second quantitative pipe is connected to the Q1 interface, and the other end of the second quantitative pipe is connected to the Q4 interface;
the gas chromatograph is provided with a sampling stage, a balancing stage and a sample introduction stage;
in the sampling phase, the sample gas inlet, the S2 interface, the S3 interface, the P1 interface, the P10 interface, the first quantitative tube, the P3 interface, the P2 interface, the Q2 interface, the Q1 interface, the second quantitative tube, the Q4 interface, the Q3 interface, the S6 interface, the S1 interface, and the sample gas outlet are sequentially communicated with each other to form a sample gas channel for sample gas to flow, so that the sample gas fills the first quantitative tube and the second quantitative tube;
the six-way pneumatic valve is switched to enable the gas chromatograph to enter a balance phase from a sampling phase;
in the balancing stage, the drain port, the S4 interface, the S3 interface, the P1 interface, the P10 interface, the first quantitative pipe, the P3 interface, the P2 interface, the Q2 interface, the Q1 interface, the second quantitative pipe, the Q4 interface, the Q3 interface, the S6 interface, the S5 interface, and the stop valve are sequentially communicated, so that the sample gas pressure in the first quantitative pipe and the second quantitative pipe is kept balanced with the ambient atmospheric pressure, and the S2 interface is connected to the S1 interface;
the ten-way pneumatic valve and the pneumatic reversing valve are used for switching the valve, so that the gas chromatograph enters a sample injection stage from the balance stage;
in the sample introduction stage, the second carrier gas pipe, the P4 interface, the P3 interface, the first quantitative pipe, the P10 interface, the P9 interface, the first chromatographic column, the P5 interface, the P6 interface, and the first detection device are sequentially communicated, and the carrier gas a pushes the sample gas in the first quantitative pipe to enter the first chromatographic column, and enters the first detection device after being separated by the first chromatographic column;
the third carrier gas pipe, the Q6 interface, the Q1 interface, the second quantitative pipe, the Q4 interface, the Q5 interface, the second chromatographic column and the first detector are communicated in sequence, and the carrier gas A pushes the sample gas in the second quantitative pipe to enter the second chromatographic column, and then enters the first detector after being separated by the second chromatographic column.
In one possible design, in the balancing stage and the sampling stage, the first carrier gas pipe, the P7 interface, the P6 interface and the first detection device are communicated in sequence to form a gas flow channel for the carrier gas a to purge the first detection device;
the second carrier gas pipe, the P4 interface, the P5 interface, the first chromatographic column, the P9 interface and the P8 interface are communicated in sequence to form a gas flow channel for the carrier gas A to purge the first chromatographic column;
the third carrier gas pipe, the Q6 interface, the Q5 interface, the second chromatographic column and the first detection device are communicated in sequence to form a gas flow channel for the carrier gas A to purge the second chromatographic column.
In one possible design, a Z1 interface, a Z2 interface, a Z3 interface and a Z4 interface which are positioned between a Q3 interface and a Q4 interface are added on the pneumatic reversing valve, the Z1 interface, the Z2 interface, the Z3 interface and the Z4 interface are sequentially arranged along the first direction, and the Z1 interface is positioned close to the Q3 interface;
the gas chromatograph also comprises a second carrier gas leading-in device, a third chromatographic column, a third quantitative tube and a second detection device;
the second carrier gas introducing device is used for introducing carrier gas B, and is connected to the Z3 interface;
one end of the third quantitative pipe is connected to the Z1 interface, and the other end of the third quantitative pipe is connected to the Z4 interface;
one end of the third chromatographic column is connected to the Z2 interface, and the other end of the third chromatographic column is connected to the second detection device;
in the sampling phase, the S2 interface, the S3 interface, the P1 interface, the P10 interface, the first quantitative tube, the P3 interface, the P2 interface, the Q2 interface, the Q1 interface, the second quantitative tube, the Q4 interface, the Z4 interface, the third quantitative tube, the Z1 interface, the Q3 interface, the S6 interface, the S1 interface, and the sample gas outlet are sequentially communicated with each other to form a sample gas channel for flowing a sample gas, so that the sample gas fills the first quantitative tube, the second quantitative tube, and the third quantitative tube;
the six-way pneumatic valve is switched to enable the gas chromatograph to enter a balance phase from a sampling phase;
in the balancing stage, the evacuation port, the S4 interface, the S3 interface, the P1 interface, the P10 interface, the first quantitative pipe, the P3 interface, the P2 interface, the Q2 interface, the Q1 interface, the second quantitative pipe, the Q4 interface, the Z4 interface, the third quantitative pipe, the Z1 interface, the Q3 interface, the S6 interface, and the S5 interface are sequentially communicated, so that the sample gas pressure in the first quantitative pipe, the second quantitative pipe, and the third quantitative pipe is kept balanced with the ambient atmospheric pressure, and the S2 interface is connected to the S1 interface;
the ten-way vent valve and the pneumatic reversing valve are used for switching the valve, so that the gas chromatograph enters the sample injection stage from the balance stage;
in the sample introduction stage, the second carrier gas pipe, the P4 interface, the P3 interface, the first quantitative pipe, the P10 interface, the P9 interface, the first chromatographic column, the P5 interface, the P6 interface, and the first detection device are sequentially communicated, and the carrier gas a pushes the sample gas in the first quantitative pipe to enter the first chromatographic column, and enters the first detection device after being separated by the first chromatographic column;
the third carrier gas pipe, the Q6 interface, the Q1 interface, the second quantitative pipe, the Q4 interface, the Q5 interface, the second chromatographic column, the Q4 interface, the Q5 interface, and the first detector are sequentially communicated, the first carrier gas pushes the sample gas in the second quantitative pipe to enter the second chromatographic column, and the sample gas enters the first detector after being separated by the second chromatographic column;
the second carrier gas introducing device, the Z3 interface, the Z4 interface, the third quantifying pipe, the Z1 interface, the Z2 interface, the third chromatographic column and the second detection device are sequentially communicated, and the carrier gas B pushes the sample gas in the third quantifying pipe to enter the third chromatographic column and enter the second detection device after being separated by the third chromatographic column.
In one possible design, during the sampling phase and the balancing phase, the first carrier gas pipe, the P7 interface, the P6 interface, and the first detection device are communicated to form a gas flow channel for the carrier gas a to purge the first detection device;
the second carrier gas pipe, the P4 interface, the P5 interface, the first chromatographic column, the P9 interface and the P8 interface are communicated in sequence to form a gas flow channel for the carrier gas A to purge the first chromatographic column;
the third carrier gas pipe, the Q6 interface, the Q5 interface, the second chromatographic column and the first detection device are communicated in sequence to form a gas flow channel for the carrier gas A to purge the second chromatographic column;
the second carrier gas introducing device, the Z3 interface, the Z2 interface, the third chromatographic column and the second detection device are sequentially communicated, so that an airflow channel for the carrier gas B to purge the third chromatographic column and the second detection device is formed.
In one possible design, the second detection device is any one of an electron capture detector, a hydrogen flame ionization detector, a flame photometric detector, a photoionization detector, and a thermal conductivity detector.
In one possible design, the carrier gas a and the carrier gas B are any one of hydrogen, helium, nitrogen, argon, carbon dioxide.
In one possible design, the second carrier gas introduction device is configured as a branch of the first carrier gas introduction device; alternatively, the first carrier gas introduction means and the second carrier gas introduction means may operate independently of each other.
In one possible design, the gas chromatograph further includes a first gas-resistance tube, a second gas-resistance tube, and a third gas-resistance tube for increasing gas flow resistance;
wherein the first gas-resistance tube is arranged between the first carrier gas tube and the P7 interface, the second gas-resistance tube is arranged between the P6 interface and the first detection device, and the third gas-resistance tube is arranged between the second chromatographic column and the first detection device.
In one possible design, the first and second gas-resistance tubes are capillary tubes or damper tubes.
In one possible design, the first detection device is any one of an electron capture detector, a hydrogen flame ionization detector, a flame photometric detector, a photoionization detector, and a thermal conductivity detector.
Compared with the prior art, the invention has the beneficial effects that:
through the technical scheme, the switching of the air path can be controlled through the six-way pneumatic valve, the ten-way pneumatic valve and the pneumatic reversing valve, so that the pneumatic reversing valve is suitable for a high-temperature working environment. And in the balancing stage, the six-way pneumatic valve can keep the whole gas circuit in a better balanced state relative to the ambient atmospheric pressure, and the accuracy of the later detection result is improved beneficially.
In the invention, the first chromatographic column and the second chromatographic column can be simultaneously analyzed, for example, the analysis of methane and total hydrocarbon can be simultaneously realized, so that the content of different types of gases can be accurately obtained, and the content of non-methane total hydrocarbon can be accurately obtained after calculation.
In addition, the gas chromatograph is used for one-time sample injection, so that system errors caused by multiple sample injections are effectively reduced, and the accuracy of data is ensured.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only show some embodiments of the present invention, and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
Fig. 1 is a gas diagram of a gas chromatograph according to an embodiment of the present invention, wherein the gas chromatograph is in a sampling phase;
fig. 2 is a gas diagram of a gas chromatograph in an embodiment of the present invention, wherein the gas chromatograph is in an equilibrium stage;
FIG. 3 is a gas diagram of a gas chromatograph in an embodiment of the present invention, wherein the gas chromatograph is in a sample injection stage;
fig. 4 is a gas diagram of a gas chromatograph according to another embodiment of the present invention, wherein the gas chromatograph is in a sampling phase;
fig. 5 is a gas diagram of a gas chromatograph according to another embodiment of the present invention, wherein the gas chromatograph is in an equilibrium stage;
fig. 6 is a gas circuit diagram of a gas chromatograph according to another embodiment of the present invention, wherein the gas chromatograph is in a sample injection stage.
In the above drawings, the meaning of each reference numeral is:
11-a six-way pneumatic valve, 12-a ten-way pneumatic valve, 13-a pneumatic reversing valve, 2-a stop valve, 3-a sampling device, 41-a first air resistance pipe, 42-a second air resistance pipe, 43-a third air resistance pipe, 51-a first chromatographic column, 52-a second chromatographic column, 53-a third chromatographic column, 61-a first quantitative pipe, 62-a second quantitative pipe, 63-a third quantitative pipe, 71-a first carrier gas leading-in device, 72-a second carrier gas leading-in device, 81-a first detection device, 82-a second detection device, 91-an evacuation port and 92-an exhaust port.
Detailed Description
The invention is further explained below with reference to the drawings and the specific embodiments.
It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. Specific structural and functional details disclosed herein are merely illustrative of example embodiments of the invention. This invention may, however, be embodied in many alternate forms and should not be construed as limited to the embodiments set forth herein.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments of the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises," "comprising," "includes," and/or "including," when used herein, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, numbers, steps, operations, elements, components, and/or groups thereof.
It should also be noted that, in some alternative implementations, the functions/acts noted may occur out of the order noted in the figures. For example, two figures shown in succession may, in fact, be executed substantially concurrently, or the figures may sometimes be executed in the reverse order, depending upon the functionality/acts involved.
In the following description, specific details are provided to facilitate a thorough understanding of example embodiments. However, it will be understood by those of ordinary skill in the art that the example embodiments may be practiced without these specific details. For example, systems may be shown in block diagrams in order not to obscure the examples in unnecessary detail. In other instances, well-known processes, structures and techniques may be shown without unnecessary detail in order to avoid obscuring example embodiments.
According to an embodiment of the present invention, a gas chromatograph is provided. One embodiment of which is shown in fig. 1 to 6.
Referring to fig. 1 to 6, the gas chromatograph includes a six-way air-operated valve 11, a ten-way air-operated valve 12, a pneumatic direction valve 13, a shutoff valve 2, a sampling device 3, a first column 51, a second column 52, a first quantitative tube 61, a second quantitative tube 62, a first carrier gas introduction device 71, and a first detection device 81.
The six-way pneumatic valve 11 has an S1 port, an S2 port, an S3 port, an S4 port, an S5 port and an S6 port which are sequentially arranged in a first direction, the ten-way pneumatic valve 12 has a P1 port, a P2 port, a P3 port, a P4 port, a P5 port, a P6 port, a P7 port, a P8 port, a P9 port and a P10 port which are sequentially arranged in the first direction, and the pneumatic directional valve 13 has a Q1 port, a Q2 port, a Q3 port, a Q4 port, a Q5 port and a Q6 port which are sequentially arranged in the first direction, wherein the first direction is clockwise or counterclockwise.
Referring to fig. 1 to 6, the S1 interface is connected to the sample gas outlet of the sampling device 3, and the S2 interface is connected to the sample gas inlet of the sampling device 3. It should be noted that the sampling devices may be the same device or may be two different devices.
The S3 interface is connected with the P1 interface, the S4 interface is connected with the evacuation port 91, the S5 interface is connected with the stop valve 2, and the S6 interface is connected with the Q3 interface.
The first carrier gas introducing device 71 is used for introducing the carrier gas a, and the first carrier gas introducing device 71 has a first carrier gas pipe, a second carrier gas pipe and a third carrier gas pipe, the first carrier gas pipe is connected to the P7 interface, the second carrier gas pipe is connected to the P4 interface, and the third carrier gas pipe is connected to the Q6 interface.
The P8 port is circumscribed by an exhaust outlet.
One end of the first chromatographic column 51 is connected to the P5 interface, and the other end of the first chromatographic column 51 is connected to the P9 interface; the first detection device 81 is connected to the P6 interface; one end of the second chromatographic column 52 is connected to the first detecting device 81, and the other end of the second chromatographic column 52 is connected to the Q5 interface.
One end of the first quantitative pipe 61 is connected to a P3 interface, and the other end of the first quantitative pipe 61 is connected to a P10 interface; one end of the second fixed quantity pipe 62 is connected to the Q1 port, and the other end of the second fixed quantity pipe 62 is connected to the Q4 port.
The gas chromatograph has a sampling stage, an equilibration stage, and a sample introduction stage.
In the sampling stage, the sample gas inlet, the S2 interface, the S3 interface, the P1 interface, the P10 interface, the first quantitative tube 61, the P3 interface, the P2 interface, the Q2 interface, the Q1 interface, the second quantitative tube 62, the Q4 interface, the Q3 interface, the S6 interface, the S1 interface and the sample gas outlet are sequentially communicated to form a sample gas channel for the sample gas to flow, so that the first quantitative tube 61 and the second quantitative tube 62 are filled with the sample gas.
The six-way pneumatic valve 11 is switched so that the gas chromatograph enters the equilibrium phase from the sampling phase.
In the balancing stage, the evacuation port 91, the S4 interface, the S3 interface, the P1 interface, the P10 interface, the first quantitative pipe 61, the P3 interface, the P2 interface, the Q2 interface, the Q1 interface, the second quantitative pipe 62, the Q4 interface, the Q3 interface, the S6 interface, the S5 interface and the stop valve 2 are sequentially communicated, so that the sample gas pressure in the first quantitative pipe 61 and the second quantitative pipe 62 is balanced with the ambient atmospheric pressure, and the S2 interface is connected to the S1 interface.
The ten air vent valve 12 and the pneumatic reversing valve 13 are opened and closed, so that the gas chromatograph enters the sample injection stage from the balance stage.
In the sample injection stage, the second carrier gas pipe, the P4 interface, the P3 interface, the first quantitative pipe 61, the P10 interface, the P9 interface, the first chromatographic column 51, the P5 interface, the P6 interface and the first detection device 81 are sequentially communicated, and the carrier gas a pushes the sample gas in the first quantitative pipe 61 to enter the first chromatographic column 51, and the sample gas enters the first detection device 81 after being separated by the first chromatographic column 51;
the third carrier gas pipe, the Q6 interface, the Q1 interface, the second quantitative pipe 62, the Q4 interface, the Q5 interface, the second chromatographic column 52 and the first detector are sequentially communicated, and the carrier gas a pushes the sample gas in the second quantitative pipe 62 to enter the second chromatographic column 52, and enters the first detector 81 after being separated by the second chromatographic column 52.
Through the technical scheme, the switching of the air passages can be controlled through the six-way pneumatic valve 11, the ten-way pneumatic valve 12 and the pneumatic reversing valve 13, so that the pneumatic reversing valve is suitable for a high-temperature working environment. And in the balancing stage, the six-way pneumatic valve 11 can keep the whole gas circuit in a better balanced state relative to the ambient atmospheric pressure, which is beneficial to improving the accuracy of the later detection result.
In the present invention, the first chromatographic column 51 and the second chromatographic column 52 can be analyzed simultaneously, for example, the analysis of methane and total hydrocarbons can be realized simultaneously, and not only the contents of different types of gases can be accurately obtained, but also the contents of non-methane total hydrocarbons can be accurately obtained after calculation. Because the gas chromatograph is used for one-time sample injection, the system error caused by multiple sample injections is effectively reduced.
According to the difference of distribution coefficients of all components in the sample gas between the gas phase and the fixed phase in the chromatographic column, when the sample gas is carried into the chromatographic column by the carrier gas to operate, the components are repeatedly distributed (adsorbed-desorbed-discharged) between the two phases. Due to the different adsorption capacities (i.e., different storage effects) of the immobilized phase with respect to the components, the components are separated from each other after a certain column length at different running speeds in the column.
The separated components enter a first detection device 81 according to the sequence of retention time, the first detection device 81 detects the components in sequence according to the physicochemical properties of the components and automatically records detection signals, and the generated signals are amplified and then the chromatographic peaks of the components can be drawn. And finally, carrying out qualitative analysis according to the retention time (peak position) of each component in the sample gas or carrying out quantitative analysis on each component in the sample gas according to the response value (peak height or peak area).
It should be understood that, in the present invention, the first chromatographic column 51, the second chromatographic column 52, the first quantitative tube 61, the second quantitative tube 62, the sampling device 3, the first carrier gas introduction device 71, and the first detection device 81 are all of the prior art. In other words, the person skilled in the art can modify the above components in a conventional manner on the basis of the prior art.
Referring to fig. 1 to 6, in the equilibrium stage and the sampling stage, the first carrier gas pipe, the P7 interface, the P6 interface and the first detection device 81 are sequentially communicated to form a gas flow channel for the carrier gas a to purge the first detection device 81.
The second carrier gas pipe, the P4 interface, the P5 interface, the first chromatographic column 51, the P9 interface and the P8 interface are sequentially communicated to form a gas flow channel for the carrier gas a to purge the first chromatographic column 51.
The third carrier gas pipe, the Q6 interface, the Q5 interface, the second chromatographic column 52 and the first detection device 81 are sequentially communicated to form a gas flow channel for the carrier gas a to purge the second chromatographic column 52.
Therefore, the carrier gas a can carry the gas sample or the gasified sample gas at a certain flow rate to enter the first chromatographic column 51 and the second chromatographic column 52 together for separation, then each separated component is loaded into the first detection device 81 for detection, and finally the carrier gas a flows out of the chromatographic system for emptying or collection.
The pneumatic reversing valve 13 is additionally provided with a Z1 interface, a Z2 interface, a Z3 interface and a Z4 interface which are positioned between the Q3 interface and the Q4 interface, the Z1 interface, the Z2 interface, the Z3 interface and the Z4 interface are sequentially arranged along a first direction, and the Z1 interface is positioned close to the Q3 interface.
The gas chromatograph further includes a second carrier gas introduction device 72, a third chromatographic column 53, a third quantitative tube 63, and a second detection device 82.
The second carrier gas introduction device 72 is for introducing the carrier gas B, and the second carrier gas introduction device 72 is connected to the Z3 port.
One end of the third quantitative tube 63 is connected to the Z1 port, and the other end of the third quantitative tube 63 is connected to the Z4 port.
One end of the third column 53 is connected to the Z2 port and the other end of the third column 53 is connected to the second detection device 82.
In the sampling stage, the interface S2, the interface S3, the interface P1, the interface P10, the interface first quantitative tube 61, the interface P3, the interface P2, the interface Q2, the interface Q1, the interface second quantitative tube 62, the interface Q4, the interface Z4, the interface third quantitative tube 63, the interface Z1, the interface Q3, the interface S6, the interface S1 and the sample gas outlet are sequentially communicated with each other to form a sample gas channel for flowing sample gas, so that the first quantitative tube 61, the second quantitative tube 62 and the third quantitative tube 63 are filled with the sample gas.
The six-way pneumatic valve 11 is switched so that the gas chromatograph enters the equilibrium phase from the sampling phase.
In the balancing stage, the evacuation port 91, the S4 interface, the S3 interface, the P1 interface, the P10 interface, the first quantitative tube 61, the P3 interface, the P2 interface, the Q2 interface, the Q1 interface, the second quantitative tube 62, the Q4 interface, the Z4 interface, the third quantitative tube 63, the Z1 interface, the Q3 interface, the S6 interface and the S5 interface are sequentially communicated, so that the sample gas pressure in the first quantitative tube 61, the second quantitative tube 62 and the third quantitative tube 63 is kept balanced with the ambient atmospheric pressure, and the S2 interface is connected to the S1 interface.
The ten air vent valve 12 and the pneumatic reversing valve 13 are opened and closed, so that the gas chromatograph enters the sample injection stage from the balance stage.
In the sample injection stage, the second carrier gas pipe, the P4 interface, the P3 interface, the first quantitative pipe 61, the P10 interface, the P9 interface, the first chromatographic column 51, the P5 interface, the P6 interface and the first detection device 81 are sequentially communicated, and the carrier gas a pushes the sample gas in the first quantitative pipe 61 to enter the first chromatographic column 51, and the sample gas enters the first detection device 81 after being separated by the first chromatographic column 51.
The third carrier gas pipe, the Q6 interface, the Q1 interface, the second quantitative pipe 62, the Q4 interface, the Q5 interface, the second chromatographic column 52, the Q4 interface, the Q5 interface, and the first detector are sequentially communicated, the first carrier gas pushes the sample gas in the second quantitative pipe 62 to enter the second chromatographic column 52, and the sample gas is separated by the second chromatographic column 52 and then enters the first detector 81.
The second carrier gas introducing device 72, the Z3 interface, the Z4 interface, the third quantifying tube 63, the Z1 interface, the Z2 interface, the third chromatographic column 53 and the second detecting device 82 are sequentially communicated, and the carrier gas B pushes the sample gas in the third quantifying tube 63 to enter the third chromatographic column 53, and enters the second detecting device 82 after being separated by the third chromatographic column 53.
Through the mode, the system gas path is changed by reasonably configuring and switching the six-way pneumatic valve 11, the ten-way pneumatic valve 12 and the pneumatic reversing valve 13, so that any single item or multiple item combination of the first chromatographic column 51, the second chromatographic column 52 and the third chromatographic column 53 is realized, independent analysis is realized, common analysis can also be realized, different detection requirements are met, and the universal detection device has better universality.
For example, the content of methane can be analyzed by the first chromatographic column 51, the content of total hydrocarbons by the second chromatographic column 52, and the content of benzene series by the third chromatographic column 53.
Referring to fig. 1 to 6, in the sampling stage and the balancing stage, the first carrier gas pipe, the P7 interface, the P6 interface, and the first detection device 81 are communicated to form a gas flow channel for the carrier gas a to purge the first detection device 81, so that the first detection device 81 can rapidly and effectively measure the content of the sample gas.
The second carrier gas pipe, the P4 interface, the P5 interface, the first chromatographic column 51, the P9 interface and the P8 interface are sequentially communicated to form a gas flow channel for the carrier gas a to purge the first chromatographic column 51, so that the first chromatographic column 51 separates the target components.
The third carrier gas pipe, the Q6 interface, the Q5 interface, the second chromatographic column 52 and the first detection device 81 are sequentially communicated to form a gas flow channel for the carrier gas a to purge the second chromatographic column 52, so that the first chromatographic column 51 separates the target components.
The second carrier gas introducing device 72, the Z3 interface, the Z2 interface, the third chromatographic column 53 and the second detecting device 82 are sequentially communicated, so that a gas flow channel for the carrier gas B to purge the third chromatographic column 53 and the second detecting device 82 is formed. Thus, the target component can be separated through the third column 53. The second detecting device 82 can sequentially detect the separated components according to the physicochemical properties of the components.
In one embodiment of the present invention, the second detecting device 82 may be any one of an electron capture detector, a hydrogen flame ionization detector, a flame photometric detector, a photoionization detector, and a thermal conductivity detector.
In the present disclosure, the first detecting device 81 is a hydrogen Flame Ionization Detector (FID), which may be externally connected to the first air and the first fuel gas. The second sensing device 82 is a hydrogen Flame Ionization Detector (FID) that also circumscribes the second air and second fuel gas communication.
Specifically, the first detection device and the second detection device may be appropriately selected according to the kind of the sample gas. Such as a Thermal Conductivity Detector (TCD) using thermal conductivity principles, which can be flexibly selected by those skilled in the art according to practical needs, and is not limited by the present disclosure.
In the specific embodiment provided by the present invention, the carrier gas a and the carrier gas B are any one of hydrogen, helium, nitrogen, argon, and carbon dioxide, and those skilled in the art can flexibly select the carrier gas a and B according to the sample gas.
Alternatively, the second carrier gas introduction device 72 may be configured to be branched from the first carrier gas introduction device 71, that is, the carrier gas a introduced by the first carrier gas introduction device 71 and the carrier gas B introduced by the second carrier gas introduction device 72 are both the same type of carrier gas.
Alternatively, the first carrier gas introduction device 71 and the second carrier gas introduction device 72 operate independently of each other. That is, the carrier gas a and the carrier gas B introduced are different types.
In the present invention, the first carrier gas introducing device 71 and the second carrier gas introducing device 72 may be the carrier gas pumps of the related art, or may be the carrier gas pumps of the related art, and the carrier gas introducing device of the present invention may be obtained by performing a conventional modification to the air pumps of the related art, but is not limited thereto.
Referring to fig. 1 to 6, in the present invention, the gas chromatograph further includes a first gas barrier tube 41, a second gas barrier tube 42, and a third gas barrier tube 43 for increasing gas flow resistance. Wherein, the first air-blocking tube 41 is arranged between the first carrier gas tube and the P7 interface, the second air-blocking tube 42 is arranged between the P6 interface and the first detection device 81, and the third air-blocking tube 43 is arranged between the second chromatographic column 52 and the first detection device 81.
In this way, the resistance of the gas in the gas flow passage during circulation can be increased by the first, second, and third gas- resistance tubes 41, 42, and 43, so that the sample gas separation efficiency is improved, and it is also beneficial to improve the analysis speed of the first and/or second detection devices 81 and 82. And the formed chromatographic peak is narrow and symmetrical in peak shape, which is beneficial to accurately reacting the components of the current sample gas.
In the present invention, the first and second air resistance tubes 41 and 42 are capillary tubes or damper tubes. Therefore, those skilled in the art can flexibly select the target according to the actual requirement, and the present invention is not limited to this.
In one embodiment of the present invention, the first detecting device 81 is any one of an electron capture detector, a hydrogen flame ionization detector, a flame photometric detector, a photoionization detector, and a thermal conductivity detector.
The present invention is not limited to the above-described alternative embodiments, and various other embodiments can be obtained by those skilled in the art from the above-described embodiments in any combination, and any other embodiments can be obtained in various forms while still being within the spirit of the present invention. The above detailed description should not be taken as limiting the scope of the invention, which is defined in the claims, and which the description is intended to be interpreted accordingly.

Claims (10)

1. A gas chromatograph is characterized by comprising a six-way air-operated valve (11), a ten-way air-operated valve (12), a pneumatic reversing valve (13), a stop valve (2), a sampling device (3), a first chromatographic column (51), a second chromatographic column (52), a first quantitative tube (61), a second quantitative tube (62), a first carrier gas introduction device (71) and a first detection device (81);
wherein the six-way pneumatic valve (11) has an S1 port, an S2 port, an S3 port, an S4 port, an S5 port and an S6 port arranged in series in a first direction, the ten-way pneumatic valve (12) has a P1 port, a P2 port, a P3 port, a P4 port, a P5 port and a P6 port, a P7 port, a P8 port, a P9 port and a P10 port arranged in series in the first direction, and the pneumatic directional valve (13) has a Q1 port, a Q2 port, a Q3 port, a Q4 port, a Q5 port and a Q6 port arranged in series in the first direction, which is clockwise or counterclockwise;
the S1 interface is connected to a sample gas outlet of the sampling device (3), the S2 interface is connected to a sample gas inlet of the sampling device (3), the S3 interface is connected to the P1 interface, the S4 interface is connected to a drain port (91), the S5 interface is connected to the stop valve (2), and the S6 interface is connected to the Q3 interface;
the first carrier gas introducing device (71) is used for introducing carrier gas A, and the first carrier gas introducing device (71) is provided with a first carrier gas pipe, a second carrier gas pipe and a third carrier gas pipe, wherein the first carrier gas pipe is connected with the P7 interface, the second carrier gas pipe is connected with the P4 interface, and the third carrier gas pipe is connected with the Q6 interface;
the P8 interface is externally connected with an exhaust gas discharge port;
one end of the first chromatographic column (51) is connected to the P5 interface, and the other end of the first chromatographic column (51) is connected to the P9 interface; the first detection device (81) is connected to the P6 interface; one end of the second chromatographic column (52) is connected to the first detection device (81), and the other end of the second chromatographic column (52) is connected to the Q5 interface;
one end of the first quantitative pipe (61) is connected to the P3 interface, and the other end of the first quantitative pipe (61) is connected to the P10 interface; one end of the second quantitative pipe (62) is connected to the Q1 interface, and the other end of the second quantitative pipe (62) is connected to the Q4 interface;
the gas chromatograph is provided with a sampling stage, a balancing stage and a sample introduction stage;
in the sampling phase, the sample gas inlet, the S2 interface, the S3 interface, the P1 interface, the P10 interface, the first quantitative tube (61), the P3 interface, the P2 interface, the Q2 interface, the Q1 interface, the second quantitative tube (62), the Q4 interface, the Q3 interface, the S6 interface, the S1 interface, and the sample gas outlet are sequentially communicated with each other to form a sample gas channel for flowing a sample gas, so that the first quantitative tube (61) and the second quantitative tube (62) are filled with the sample gas;
the six-way pneumatic valve (11) is switched so that the gas chromatograph enters an equilibrium stage from a sampling stage;
in the balancing stage, the evacuation port (91), the S4 interface, the S3 interface, the P1 interface, the P10 interface, the first quantitative pipe (61), the P3 interface, the P2 interface, the Q2 interface, the Q1 interface, the second quantitative pipe (62), the Q4 interface, the Q3 interface, the S6 interface, the S5 interface, and the stop valve (2) are sequentially communicated, so that the sample gas pressure in the first quantitative pipe (61) and the second quantitative pipe (62) is kept balanced with the ambient atmospheric pressure, and the S2 interface is connected to the S1 interface;
the ten-way pneumatic valve (12) and the pneumatic reversing valve (13) are switched to enable the gas chromatograph to enter a sample injection stage from the balance stage;
in the sample injection stage, the second carrier gas pipe, the P4 interface, the P3 interface, the first quantitative pipe (61), the P10 interface, the P9 interface, the first chromatographic column (51), the P5 interface, the P6 interface, and the first detection device (81) are sequentially communicated, and the carrier gas a pushes the sample gas in the first quantitative pipe (61) to enter the first chromatographic column (51), and enters the first detection device (81) after being separated by the first chromatographic column (51);
the third carrier gas pipe, the Q6 interface, the Q1 interface, the second quantitative pipe (62), the Q4 interface, the Q5 interface, the second chromatographic column (52) and the first detector are sequentially communicated, and the carrier gas A pushes the sample gas in the second quantitative pipe (62) to enter the second chromatographic column (52) and enter the first detection device (81) after being separated by the second chromatographic column (52).
2. Gas chromatograph according to claim 1, characterized in that, during the sampling phase and during the balancing phase, said first carrier gas pipe, said P7 interface, said P6 interface and said first detection device (81) are in communication in sequence so as to form a gas flow channel for said carrier gas a to purge said first detection device (81);
the second carrier gas pipe, the P4 interface, the P5 interface, the first chromatographic column (51), the P9 interface and the P8 interface are communicated in sequence to form a gas flow channel for the carrier gas A to purge the first chromatographic column (51);
the third carrier gas pipe, the Q6 interface, the Q5 interface, the second chromatographic column (52) and the first detection device (81) are communicated in sequence to form a gas flow channel for the carrier gas A to purge the second chromatographic column (52).
3. The gas chromatograph according to claim 1, wherein the pneumatic reversing valve (13) is added with a Z1 interface, a Z2 interface, a Z3 interface and a Z4 interface which are positioned between a Q3 interface and a Q4 interface, the Z1 interface, the Z2 interface, the Z3 interface and the Z4 interface are sequentially arranged along the first direction, and the Z1 interface is positioned close to the Q3 interface;
the gas chromatograph further comprises a second carrier gas introducing device (72), a third chromatographic column (53), a third quantifying pipe (63) and a second detecting device (82);
the second carrier gas introducing device (72) is used for introducing carrier gas B, and the second carrier gas introducing device (72) is connected to the Z3 interface;
one end of the third quantitative pipe (63) is connected to the Z1 interface, and the other end of the third quantitative pipe (63) is connected to the Z4 interface;
one end of the third chromatographic column (53) is connected to the Z2 interface, and the other end of the third chromatographic column (53) is connected to the second detection device (82);
in the sampling phase, the S2 interface, the S3 interface, the P1 interface, the P10 interface, the first quantitative tube (61), the P3 interface, the P2 interface, the Q2 interface, the Q1 interface, the second quantitative tube (62), the Q4 interface, the Z4 interface, the third quantitative tube (63), the Z1 interface, the Q3 interface, the S6 interface, the S1 interface, and the sample gas outlet are sequentially communicated with each other to form a sample gas channel for flowing a sample gas, so that the sample gas fills the first quantitative tube (61), the second quantitative tube (62), and the third quantitative tube (63);
the six-way pneumatic valve (11) is switched so that the gas chromatograph enters an equilibrium stage from a sampling stage;
in the balancing stage, the evacuation port (91), the S4 interface, the S3 interface, the P1 interface, the P10 interface, the first quantitative tube (61), the P3 interface, the P2 interface, the Q2 interface, the Q1 interface, the second quantitative tube (62), the Q4 interface, the Z4 interface, the third quantitative tube (63), the Z1 interface, the Q3 interface, the S6 interface, and the S5 interface are sequentially communicated, so that the sample gas pressure in the first quantitative tube (61), the second quantitative tube (62), and the third quantitative tube (63) is balanced with the ambient atmospheric pressure, and the S2 interface is connected to the S1 interface;
the ten-way vent valve (12) and the pneumatic reversing valve (13) are switched so that the gas chromatograph enters the sample injection stage from the equilibrium stage;
in the sample injection stage, the second carrier gas pipe, the P4 interface, the P3 interface, the first quantitative pipe (61), the P10 interface, the P9 interface, the first chromatographic column (51), the P5 interface, the P6 interface, and the first detection device (81) are sequentially communicated, and the carrier gas a pushes the sample gas in the first quantitative pipe (61) to enter the first chromatographic column (51), and enters the first detection device (81) after being separated by the first chromatographic column (51);
the third carrier gas pipe, the Q6 interface, the Q1 interface, the second quantitative pipe (62), the Q4 interface, the Q5 interface, the second chromatographic column (52), the Q4 interface, the Q5 interface, and the first detector are sequentially communicated, the first carrier gas pushes the sample gas in the second quantitative pipe (62) to enter the second chromatographic column (52), and the sample gas enters the first detector (81) after being separated by the second chromatographic column (52);
the second carrier gas introducing device (72), the Z3 interface, the Z4 interface, the third quantitative tube (63), the Z1 interface, the Z2 interface, the third chromatographic column (53) and the second detection device (82) are sequentially communicated, and the carrier gas B pushes the sample gas in the third quantitative tube (63) to enter the third chromatographic column (53) and enter the second detection device (82) after being separated by the third chromatographic column (53).
4. Gas chromatograph according to claim 3, characterized in that, during the sampling phase and during the balancing phase, the first carrier gas pipe, the P7 interface, the P6 interface, the first detection device (81) are in communication so as to form a gas flow channel for the carrier gas A to purge the first detection device (81);
the second carrier gas pipe, the P4 interface, the P5 interface, the first chromatographic column (51), the P9 interface and the P8 interface are communicated in sequence to form a gas flow channel for the carrier gas A to purge the first chromatographic column (51);
the third carrier gas pipe, the Q6 interface, the Q5 interface, the second chromatographic column (52) and the first detection device (81) are communicated in sequence to form a gas flow channel for the carrier gas A to purge the second chromatographic column (52);
the second carrier gas introducing device (72), the Z3 interface, the Z2 interface, the third chromatographic column (53) and the second detection device (82) are sequentially communicated, so that a gas flow channel for the carrier gas B to purge the third chromatographic column (53) and the second detection device (82) is formed.
5. Gas chromatograph according to claim 3, characterized in that said second detection means (82) are any one of an electron capture detector, a hydrogen flame ionization detector, a flame photometric detector, a photoionization detector and a thermal conductivity detector.
6. Gas chromatograph according to claim 3, characterized in that said carrier gas A and said carrier gas B are any one of hydrogen, helium, nitrogen, argon, carbon dioxide.
7. Gas chromatograph according to claim 3, characterized in that said second carrier gas introduction means (72) are configured as branches of said first carrier gas introduction means (71); alternatively, the first carrier gas introduction device (71) and the second carrier gas introduction device (72) are operated independently of each other.
8. Gas chromatograph according to any one of claims 1 to 7, characterized in that it further comprises a first gas-resistance tube (41), a second gas-resistance tube (42) and a third gas-resistance tube (43) for increasing the gas flow resistance;
wherein the first gas-resistance tube (41) is arranged between the first carrier gas tube and the P7 interface, the second gas-resistance tube (42) is arranged between the P6 interface and the first detection device (81), and the third gas-resistance tube (43) is arranged between the second chromatographic column (52) and the first detection device (81).
9. Gas chromatograph according to claim 8, characterized in that said first and second gas-resistance tubes (41, 42) are capillary or damper tubes.
10. Gas chromatograph according to any one of claims 1 to 7, characterized in that said first detection means (81) is any one of an electron capture detector, a hydrogen flame ionization detector, a flame photometric detector, a photoionization detector and a thermal conductivity detector.
CN202110700342.4A 2021-02-02 2021-06-23 Gas chromatograph Withdrawn CN113219108A (en)

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CN2021101454800 2021-02-02

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20210088484A1 (en) * 2019-09-24 2021-03-25 Shimadzu Corporation Gas sampler

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20210088484A1 (en) * 2019-09-24 2021-03-25 Shimadzu Corporation Gas sampler
US11531008B2 (en) * 2019-09-24 2022-12-20 Shimadzu Corporation Gas sampler

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Application publication date: 20210806