CN110441101B - Separation system of gas chromatography equipment - Google Patents
Separation system of gas chromatography equipment Download PDFInfo
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- CN110441101B CN110441101B CN201810418914.8A CN201810418914A CN110441101B CN 110441101 B CN110441101 B CN 110441101B CN 201810418914 A CN201810418914 A CN 201810418914A CN 110441101 B CN110441101 B CN 110441101B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
- B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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Abstract
A separation system of gas chromatography equipment comprises a separation flow path, which is formed by stacking a plurality of flow path units manufactured by a semiconductor process, wherein each flow path unit is formed by manufacturing a forming layer on a bottom substrate and then stacking an upper substrate, and a gas guide passage communicated with a continuous extension loop is formed on the forming layer. The air guide passage is internally provided with the filling material, so that a tested sample entering the separation flow path is dragged by the adsorption force of the filling material, the adsorption force of different compounds contained in the tested sample is different, and different compounds contained in the tested sample are dragged by different adsorption forces to generate different flow velocities in the separation flow path, so that different compounds contained in an untested sample are gradually separated in the separation flow path.
Description
Technical Field
The present invention relates to a separation system of a gas chromatography apparatus, and more particularly, to a gas separation system for separating and analyzing compounds that are easily volatilized without decomposition in organic chemistry.
Background
Gas Chromatography (GC), a technique used in organic chemistry for separating and purifying volatile compounds with good thermal stability, is achieved by interacting a mobile phase and a static phase to allow the components contained in the mixture to have different flow rates in the system, thereby achieving the purpose of separation.
However, there are many types and kinds of gas chromatographs, and the gas chromatographs are different in shape and structure, but generally consist of the following 6 basic systems: (1) the gas path system, (2) the sample injection system, (3) the separation system, (4) the temperature control system, (5) the detection system and (6) the recording system constitute a large-sized apparatus, because the separation system needs a chromatography column (column) to separate each component of the sample, which is the heart of the gas chromatograph. Because chromatography tubular column efficiency and tubular column length, internal diameter are thick relevant with the membrane, the length of tubular column is longer, the internal diameter is thick with the membrane is less, the analysis effect is better, so the chromatography tubular column of general gas chromatography appearance adopts very long setting, however because the chromatography tubular column need place in the temperature control system in order to keep the temperature requirement of constant temperature operation, so chromatography tubular column length will influence the volume setting of temperature control system, so the chromatography tubular column adopts the setting of a plurality of winding rings in order to reduce the volume setting of temperature control system as far as possible with reduction length at present. However, the current chromatographic column arrangement of the gas chromatograph is still quite large and space-consuming.
In view of the above, how to solve the problem of setting the length of the chromatography column of the gas chromatograph and effectively achieve the purpose of gas chromatography separation is an object to be developed by the present application.
Disclosure of Invention
The main object of the present invention is to provide a separation system of gas chromatography equipment, which is configured with a plurality of flow path units of the separation system by a semiconductor process to form a gas guide path of a continuous extended loop, and the filling material is arranged in the air guide passage, so that when a tested sample with a large amount of mixture passes through the air guide passage, the different adsorption forces of the filling material on the compounds with different components of the tested sample are utilized, the flow velocity of the compound with high adsorption force is slower and slower, the flow velocity of the compound with lower adsorption force is less in the trend of reducing, different compounds are gradually separated at different flow velocities, the purpose of gas chromatographic separation is achieved, and then the components and the concentration of each separated tested sample are analyzed through the detector, therefore, through the miniaturized semiconductor manufacturing process, the separation system is miniaturized, and the separation speed of the tested sample is increased through the miniature pump, so that the detection effect and efficiency can be improved.
In one broad aspect, the present disclosure provides a separation system for a gas chromatography apparatus, comprising: a separation flow path, which is formed by stacking a plurality of flow path units made by a semiconductor process, wherein each flow path unit is formed by manufacturing a forming layer on a bottom substrate and then stacking an upper substrate, a continuous extending loop communicated air guide path is generated on the forming layer, an air guide inlet is generated on the upper substrate and communicated with one end of the air guide path, an air guide outlet is generated on the bottom substrate and communicated with the other end of the air guide path, the flow path units on the bottom layer are stacked on the flow path units on the upper layer, the air guide outlet of the flow path unit on the upper layer is communicated with the air guide path of the flow path unit on the bottom layer, and the air guide paths of each stacked flow path unit are enabled to be communicated with each other; and a filler material disposed in the air guide passage of the separation flow path; therefore, the tested sample is led into the air guide passage which flows through the separation flow passage from the air guide inlet, the tested sample is adsorbed and separated by the filling material on the air guide passage, and the formed compounds of each component in the tested sample are led out from the air guide outlet at different speeds for measurement, analysis and recording.
Drawings
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below, wherein:
FIG. 1 is a schematic view of the gas chromatography apparatus of the present application.
Fig. 2A is a schematic cross-sectional view of the separation system of fig. 1.
Fig. 2B is a schematic view of a fluidic unit of the separation system of fig. 1.
Fig. 3 to 5 are schematic diagrams of different embodiments of the separation system according to the present invention, in which the filler is disposed in the air guide passage.
Fig. 6 is a schematic view of the chromatographic separation of the separation system of the present invention.
FIG. 7 is an exploded view of the gas chromatography apparatus of the present invention.
Fig. 8A is a cross-sectional schematic view of the pump of fig. 7.
Fig. 8B and 8C are schematic operation diagrams of the pump of fig. 8A.
Description of the reference numerals
1: gas circuit system
11: carrier gas supply source
12: voltage-stabilizing constant-current device
121: pressure regulator
122: flow control valve
13: pipeline
14: pump and method of operating the same
141: air injection hole sheet
141 a: support frame
141 b: suspension plate
141 c: hollow hole
142: cavity frame
143: actuating body
143 a: piezoelectric carrier plate
143 b: tuning the resonator plate
143 c: piezoelectric plate
144: insulating frame
145: conductive frame
146: resonance chamber
147: airflow chamber
2: sample injection system
3: separation system
P: separation flow path
31: flow path unit
311: base substrate
311 a: air outlet
312: shaping layer
313: upper base material
313 a: gas inlet
314: air guide passage
32: filler material
32A: porous polymer
32B: molecular sieve materials
32C: fixed liquid film
32D: filling carrier
4: temperature control system
5: detection system
51: detection chamber
52: detector
6: recording system
Detailed Description
Exemplary embodiments that embody features and advantages of this disclosure are described in detail below in the detailed description. It will be understood that the present disclosure is capable of various modifications without departing from the scope of the disclosure, and that the description and drawings are to be regarded as illustrative in nature, and not as restrictive.
As shown in FIG. 1, a gas chromatography apparatus is provided, which comprises a gas path system 1, a sample injection system 2, a separation system 3, a temperature control system 4, a detection system 5 and a recording system 6. In order to miniaturize the separation system 3 and prevent the volume of the whole apparatus from being affected, the separation system 3 is manufactured by a semiconductor process, so as to solve the problem of the length setting of the chromatography column of the known gas chromatograph and achieve the purpose of gas chromatography separation, which will be described below.
The gas circuit system 1 is formed by connecting a carrier gas supply source 11 and a pressure-stabilizing constant flow device 12 through a pipeline 13, and then leading out carrier gas with stable flow rate by a pump 14 connected to the pipeline 13, wherein the carrier gas provided by the carrier gas supply source 11 must be chemically inert, and the common carrier gas is nitrogen (N)2) Argon (Ar), helium (He), hydrogen (H)2) And carbon dioxide (CO)2) And the like. As to which carrier gas is selected is usually determined by the detector 52 of the detection system 5, and the carrier gas supply source 11 is usually a high pressure steel cylinder, since the flow rate of the carrier gas is one of the important parameters affecting the chromatographic separation and qualitative analysis, in order to require the flow rate of the carrier gas to be stable, the carrier gas supply source 11 needs to use the pressure-stabilizing constant-flow device 12 to reduce the pressure and maintain the flow rate at a constant flow, and the pressure-stabilizing constant-flow device 12 includes a pressure regulator 121 and a flow control valve 122 to regulate the carrier gas supplied by the carrier gas supply source 11 to maintain the flow rate at a constant flow in the pipeline 13, and then the carrier gas with a constant flow rate is led out by the pump 14 connected to the pipeline 13.
Referring to fig. 7 to 8C, the gas chromatography apparatus is characterized in that the volume of the separation system 3 can be reduced, one reason for this is that the pump 14 is a miniaturized pump 14, and the pump 14 is a gas pump including a gas injection hole plate 141, a cavity frame 142, an actuator 143, an insulating frame 144 and a conductive frame 145 which are stacked in sequence. The air injection hole plate 141 includes a plurality of supports 141a, a suspension plate 141b and a hollow hole 141c, the suspension plate 141b can be bent and vibrated, the plurality of supports 141a are adjacent to the periphery of the suspension plate 141b, in the embodiment, the number of the supports 141a is 4, and the supports 141a are respectively adjacent to 4 corners of the suspension plate 141b, but not limited thereto, and the hollow hole 141c is formed at the center of the suspension plate 141 b; the cavity frame 142 is supported and stacked on the suspension plate 141b, the actuator 143 is supported and stacked on the cavity frame 142, and includes a piezoelectric carrier plate 143a, an adjusting resonator plate 143b, and a piezoelectric plate 143c, wherein the piezoelectric carrier plate 143a is supported and stacked on the cavity frame 142, the adjusting resonator plate 143b is supported and stacked on the piezoelectric carrier plate 143a, and the piezoelectric plate 143c is supported and stacked on the adjusting resonator plate 143b, and is deformed to drive the piezoelectric carrier plate 143a and the adjusting resonator plate 143b to perform reciprocating bending vibration after voltage is applied; the insulating frame 144 is supported on the piezoelectric carrier plate 143a stacked on the actuating body 143, and the conductive frame 145 is supported on the insulating frame 144, wherein a resonant cavity 146 is formed between the actuating body 143, the cavity frame 142 and the suspension plate 141b, and the thickness of the resonant cavity 143b is adjusted to be greater than that of the piezoelectric carrier plate 143 a.
Referring to fig. 8A to 8C, fig. 8B and 8C are schematic operation diagrams of the pump 14 shown in fig. 8A. Referring to fig. 8A, the pump 14 is disposed in the pipeline 13 through the bracket 141a by the pump 14, and an airflow chamber 147 is formed between the air injection hole plate 141 and the pipeline 13; referring to fig. 8B, when a voltage is applied to the piezoelectric plate 143c of the actuating body 143, the piezoelectric plate 143c begins to deform due to the piezoelectric effect and synchronously drives the adjustment resonator plate 143B and the piezoelectric carrier plate 143a, at this time, the air injection hole piece 141 is driven by Helmholtz resonance (Helmholtz resonance) principle, so that the actuating body 143 moves upward, and as the actuating body 143 moves upward, the volume of the airflow chamber 147 between the air injection hole piece 141 and the pipeline 13 is increased, the internal air pressure forms a negative pressure, and the air outside the pump 14 enters the airflow chamber 147 from the gap between the bracket 141a of the air injection hole piece 141 and the pipeline 13 due to the pressure gradient and performs pressure collection; finally, referring to fig. 8C, the gas continuously enters the gas flow chamber 147 to form a positive pressure in the gas flow chamber 147, and the actuating body 143 is driven by the voltage to move downward, thereby compressing the volume of the gas flow chamber 147 and pushing the gas in the gas flow chamber 147 to start the gas delivery.
The pump 14 is a gas pump, but the pump 14 may also be a mems gas pump manufactured by a mems process, wherein the orifice plate 141, the cavity frame 142, the actuator 143, the insulating frame 144 and the conductive frame 145 may all be manufactured by a surface micromachining technology to reduce the volume of the pump 14.
The sample injection system 2 is connected to an injection device (not shown, which is a common micro injection port (including a gasification chamber, so it is not described here) through a pipeline 13 of the gas path system 1 to inject the sample quantitatively and rapidly, and gasify the sample instantly, so that the carrier gas carries the sample to be tested into the separation system 3. The sample to be tested is a multi-component compound to be separated and measured by injecting the multi-component compound into the gas chromatography equipment.
Referring to fig. 2A and 2B, the separation system 3 includes a separation flow path P formed by stacking a plurality of flow path units 31 made of semiconductor, each flow path unit 31 is formed by forming a shaping layer 312 on a bottom substrate 311 and stacking an upper substrate 313 on the shaping layer 312, and forming a continuously extending air guide path 314 in loop communication with the shaping layer 312, the upper substrate 313 forms an air guide inlet 313a communicated with one end of the air guide path 314, and the bottom substrate 311 forms an air guide outlet 311a communicated with the other end of the air guide path 314, and the flow path units 31 on the bottom layer stack the flow path units 31 on the upper layer, and the air guide outlet 311a of the flow path unit 31 on the upper layer is communicated with the air guide inlet 313a of the flow path unit 31 on the bottom layer, so that the air guide paths 314 of each stacked flow path unit 31 are communicated with each other to form the separation flow path P, and the separation flow path P includes a filler flow path 32, positioned in the gas guide passageway 314 to form a gas chromatography flow path.
As shown in fig. 3, the filling material 32 may be an adsorptive porous polymer 32A, or the filling material 32 may be an adsorptive molecular sieve material 32B, and is disposed in the air guide path 314 in a filling manner. In addition, as shown in fig. 4, the filling material 32 may also be a fixed liquid film 32C uniformly covered on a filling carrier 32D, the filling carrier 32D is filled in the air guide channel 314, the filling carrier 32D may be an oxide of silicon, and the surface of the filling carrier has hydroxyl (-OH) to implant the fixed liquid film 32C thereon. As shown in fig. 5, the filling material 32 may be attached by coating (coating) the fixed liquid film 32C on the inner wall surface of the air guide path 314, or may be attached by sputtering (sputtering) the fixed liquid film on the inner wall surface of the air guide path 314.
The temperature control system 4 is provided for the separation system 3 to maintain an operation temperature for the separation system 3 and control the separation operation of the sample under a certain temperature. In addition, the temperature control system 4 can also be used to gradually increase the temperature during the gas separation operation, such as gradually increasing the temperature from 20 ℃ to 200 ℃ to improve the gas separation effect.
The detection system 5 includes a detection chamber 51 and a detector 52, wherein the detection chamber 51 is connected to the gas outlet 311a of the separation system 3.
The recording system 6 is connected to the detector 52 of the detecting system 5 for collecting the signal from the detector 52 for gas layer phase processing analysis.
As can be seen from the above description, the gas chromatography apparatus of the present invention is manufactured by a semiconductor process using a separation system 3, wherein a gas path system 1 introduces a carrier gas into a pipeline 13 at a stable flow rate, and a sample injection system 2 quantitatively and rapidly injects a sample to be tested into the pipeline 13, the pipeline 13 is connected to a gas inlet 313a of the separation system 3, and the carrier gas and the sample to be tested are introduced into the gas inlet 313a by a pump 14 and flow in a gas guide path 314, as shown in fig. 6, a mixed gas of the sample to be tested and the carrier gas (when flowing along the direction of the arrow shown in the figure) is adsorbed and separated by a filler 32 on the gas guide path 314, and since the adsorbents 32 have different adsorbances for each compound in the sample to be tested, the velocities of different compounds in the gas guide path 314 are different, and the velocity of the compound with the larger adsorbance is slower, the compound with low adsorption force has a fast speed, so that the compound contained in the sample to be tested is gradually separated by the adsorption of the compound of each component by the filling material 32 when flowing through the gas guide channel 314, so that the compound of each component contained in the sample to be tested is led out from the gas guide outlet 311a at different speeds and enters the detection chamber 51 of the detection system 5, the compound of each component of the sample to be tested is led out at different speeds by the detector 52 of the detection system 5 for detection, and finally, the signal of the detector 52 is collected by the recording system 6 for measurement analysis recording of the gas chromatography processing of the sample to be tested, so that the separated gas is detected for analyzing the gas components and the concentration contained in each gas in the sample to be tested. The separation system 3 is manufactured by a semiconductor process, can be miniaturized, solves the problem of the length arrangement of a chromatographic column of the known gas chromatograph, replaces the chromatographic column, can achieve the purpose of gas chromatographic separation, and is used in industry.
The detector 52 may be any one of a Thermal Conductivity Detector (TCD), a Flame Ionization Detector (FID), an Electron Capture Detector (ECD), a flame light detector (FPD), a thermal ionization detector (TSD), an infrared detector (IR), a Mass Spectrometer (MS), or a nuclear magnetic resonance spectrometer (NMR), and can convert data such as the separation component and concentration variation of the sample to be measured flowing out from the separation system 3 into measurable electronic signals, which are used as qualitative and quantitative analysis information.
In summary, the separation system for gas chromatography provided by the present application utilizes a gas guide path of a continuous extension loop constructed by a plurality of flow path units of the separation system manufactured by a semiconductor process, and a filler is disposed in the gas guide path, so that when a sample to be detected having a large amount of mixture passes through the gas guide path, the filler has different adsorbabilities to compounds having different components contained in the sample to be detected, the flow rate of the compound having a high adsorbability is gradually slow, the tendency of the compound having a low adsorbability to decrease is small, different compounds are gradually separated at different flow rates, and the purpose of gas chromatography separation is achieved, and then a detector is used to analyze the components and the concentrations of each separated sample to be detected. Therefore, through the miniaturized semiconductor manufacturing process, the separation system is miniaturized, and the separation speed of the tested sample is increased through the miniature pump, so that the detection effect and efficiency can be improved.
Various modifications may be made by those skilled in the art without departing from the scope of the invention as defined by the appended claims.
Although the present invention has been described with respect to the preferred embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (22)
1. A separation system for a gas chromatography apparatus, comprising:
a separation flow path, which is formed by stacking a plurality of flow path units manufactured by a semiconductor process, wherein each flow path unit is formed by manufacturing a forming layer on a bottom substrate and then stacking an upper substrate, a gas guide path communicated with a continuous extension loop is generated on the forming layer, a gas guide inlet is generated on the upper substrate and communicated with one end of the gas guide path, and a gas guide outlet is generated on the bottom substrate and communicated with the other end of the gas guide path, and the gas guide outlet of the flow path unit positioned on the upper layer is communicated with the gas guide inlet of the flow path unit positioned on the bottom layer, so that the gas guide paths of each stacked flow path unit are mutually communicated; and
a filler material arranged in the air guide passage of the separation flow path;
therefore, a tested sample is led into the air guide passage which flows through the separation flow passage from the air guide inlet, the tested sample is adsorbed and separated by the filling material on the air guide passage, and the compounds of each component in the tested sample are led out of the air guide outlet at different speeds for measurement analysis and recording.
2. The separation system of a gas chromatography apparatus as claimed in claim 1, wherein the packing material is a porous polymer having adsorptivity, and is filled in the gas guide passage.
3. The separation system of gas chromatography apparatus of claim 1, wherein the packing material is a molecular sieve material having adsorbability, and is filled in the gas guide passage.
4. The separation system of gas chromatography apparatus as claimed in claim 1, wherein the packing material is a fixed liquid film uniformly coated on a packing carrier and having an adsorption function, and is filled in the gas guide passage.
5. The separation system of a gas chromatography apparatus as claimed in claim 4, wherein the packed carrier is an oxide of silicon having hydroxyl groups on the surface thereof to allow the stationary liquid film to be planted thereon.
6. The separation system of a gas chromatography apparatus as claimed in claim 1, wherein the packing material is attached by coating a fixed liquid film directly on the inner wall surface of the gas guide passage of the separation flow path.
7. The separation system of a gas chromatography apparatus as claimed in claim 1, wherein the packing material is a fixed liquid film directly sputtered on the inner wall surface of the gas guide passage of the separation flow path.
8. The separation system of gas chromatography apparatus as claimed in claim 1, wherein the gas inlet of the separation flow path is connected to a pump, the pump is connected to a gas path system and a sample injection system through a pipeline, the gas path system is connected to a carrier gas supply source and a constant pressure and flow rate device through the pipeline, and a carrier gas with a stable flow rate is introduced into the gas guide path of the separation flow path by the pump, and the sample injection system is connected to the sample injection system through the pipeline by an injection device, so that the sample to be tested is injected by the injection device and then is introduced into the gas guide path of the separation flow path by the pump.
9. The separation system of a gas chromatography apparatus of claim 8, wherein the pump is a mems pump.
10. The separation system of gas chromatography apparatus of claim 8, wherein the pump is a gas pump comprising:
the air injection hole piece comprises a plurality of supports, a suspension piece and a hollow hole, the suspension piece can be bent and vibrated, the supports are adjacent to the periphery of the suspension piece, the hollow hole is formed in the central position of the suspension piece, the pipeline is positioned through the supports, the suspension piece is elastically supported, an air flow chamber is formed between the air injection hole piece and the pipeline, and at least one gap is formed between the supports and the suspension piece;
a cavity frame bearing and superposed on the suspension plate;
an actuating body bearing and overlapping on the cavity frame to receive voltage to generate reciprocating bending vibration;
an insulating frame bearing and superposed on the actuating body; and
a conductive frame, which is arranged on the insulating frame in a bearing and stacking manner; wherein, a resonance chamber is formed among the actuating body, the cavity frame and the suspension sheet, the actuating body is driven to drive the air injection hole sheet to generate resonance, so that the suspension sheet of the air injection hole sheet generates reciprocating vibration displacement, the carrier gas and the tested sample enter the air flow chamber through the at least one gap and are discharged through the gas flow channel, and the transmission flow of the carrier gas and the tested sample is realized.
11. The separation system of a gas chromatography apparatus of claim 10, wherein the actuator comprises:
a piezoelectric carrier plate bearing and superposed on the cavity frame;
the adjusting resonance plate is loaded and stacked on the piezoelectric carrier plate; and
and the piezoelectric plate is loaded and stacked on the adjusting resonance plate to receive voltage to drive the piezoelectric carrier plate and the adjusting resonance plate to generate reciprocating bending vibration.
12. The separation system of a gas chromatography apparatus according to claim 11, wherein the thickness of the tuned resonance plate is larger than the thickness of the piezoelectric carrier plate.
13. The separation system of claim 1, wherein the separation system is disposed in a temperature control system for maintaining an operating temperature of the separation system and controlling the separation operation of the sample under test at a certain temperature.
14. The system of claim 1, wherein the separation system is connected to a detection system and a recording system, the detection system comprises a detection chamber and a detector, the detection chamber is connected to the gas outlet of the separation system, the component compounds contained in the sample are guided out of the gas outlet at different speeds for detection by the detector, and the recording system is connected to the detector of the detection system for collecting signals of the detector to perform analysis and recording of the gas chromatography process of the sample.
15. The separation system of a gas chromatography apparatus of claim 14, wherein the detector is a thermal conductivity detector.
16. The separation system of a gas chromatography apparatus as claimed in claim 14, wherein the detector is a flame ionization detector.
17. The separation system of a gas chromatography apparatus of claim 14, wherein the detector is an electron capture detector.
18. The separation system of a gas chromatography apparatus as claimed in claim 14, wherein the detector is a flame light detector.
19. The separation system of a gas chromatography apparatus of claim 14, wherein the detector is a thermal ionization detector.
20. The separation system of a gas chromatography apparatus according to claim 14, wherein the detector is an infrared detector.
21. The separation system of a gas chromatography apparatus of claim 14, wherein the detector is a mass spectrometer.
22. The separation system of a gas chromatography apparatus as claimed in claim 14, wherein the detector is a nuclear magnetic resonance spectrometer.
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