TWM568366U - Gas chromatography device - Google Patents

Abstract

A gas chromatography apparatus includes a gas route system, a sample injecting system, a separating system, a temperature controlling system, a detecting system, and a recording system. The separating system includes a separating flow route, and the separating flow route is formed by stacking plural flow route units manufactured by semiconductor manufacturing process. Each flow route unit is produced by forming a forming layer on a bottom substrate, followed by stacking the upper substrate on the forming layer, wherein a continuous, extended, circulated and connected gas-guiding passage forms in the forming layer. A filling material is disposed in the gas-guiding passage, thereby a to-be-tested sample flowing into the separating flow route is drawn by an adsorption force of the filling material. Since the adsorption force between the filling material and the different compounds are different, each compound contained in the to-be-tested sample has a specific flow speed, which is different from the others. Consequently, the compounds contained in the to-be-tested sample are gradually separated from the others within the separating flow route.

Description

Gas chromatography equipment

The present invention relates to a gas chromatography apparatus, and more particularly to a gas chromatography apparatus for separating and analyzing a compound which is easy to volatilize without decomposition in organic chemistry.

Gas chromatography (GC) In organic chemistry, a technique for separating and purifying volatile, thermally stable compounds, both by mobile phase and stationary phase. Interactions allow the components of the mixture to have different flow rates within the system for separation purposes.

However, there are many types and types of gas chromatographs. Although their shapes and structures are different, they are usually composed of the following six basic systems: (1) pneumatic system, (2) sample injection system, and (3) Separation system, (4) temperature control system, (5) detection system and (6) recording system, thus forming a large-scale instrumentation, because in the separation system, it is necessary to rely on a column (column) Separation of the components of the sample is performed. The column is the heart of a gas chromatograph because the efficiency of the column is related to the length of the column, the inner diameter, and the film thickness. The longer the length of the column, the smaller the inner diameter and the film thickness, the better the analysis effect, so the chromatographic column of the gas chromatograph generally adopts a very long setting. However, since the chromatography column needs to be placed in the temperature control system to maintain the constant temperature operation, the length of the chromatography column will affect the volume setting of the temperature control system, so the current chromatography column adopts a plurality of winding ring settings. Reduce the length and minimize the size of the temperature control system. However, the current chromatographic column setup of the gas chromatograph is still quite large.

In view of this, how to solve the problem of the length setting of the chromatographic column of the gas chromatograph, and effectively achieve the purpose of gas chromatography separation, is the subject of research and development in this case.

The main purpose of the present invention is to provide a gas chromatography apparatus for manufacturing a separation system by a semiconductor process, and the separation system is constructed by a plurality of flow path units to form a gas passage of a continuously extending loop, and a filling is provided in the gas guiding passage. Material, so that when the sample with a large number of compounds passes through the gas guiding path, the adsorption force of the filler is different for the compounds of different components of the sample to be tested, and the compound with high adsorption force will be slower and slower, and the adsorption force is lower. The tendency of the compound flow rate to decrease is small, and the different flow rates will gradually separate the different compounds to achieve the purpose of gas chromatography separation, and then analyze the composition and concentration of each sample to be separated through a detector. In this way, through the miniaturized semiconductor process, the separation system is miniaturized, and the separation speed of the sample to be tested is increased by the micro pump, thereby improving the detection effect and efficiency.

A generalized embodiment of the present invention is a gas chromatography apparatus comprising: a gas path system, a carrier gas supply source and a constant voltage constant current device are connected through a pipeline to derive a carrier gas having a stable flow rate; a system for extracting a sample to be tested by an injection device through the pipeline connection of the pneumatic system; a separation system comprising a separation flow path and a filler material, the separation flow path connecting the pipeline of the pneumatic system And the separation flow path is composed of a plurality of flow path unit stacks prepared by a semiconductor process, each flow path unit is formed by forming a forming layer on a bottom substrate and then stacking an upper substrate, and forming the upper layer. Forming a continuous extension loop in communication with the gas guiding passage, the upper substrate generates an air guiding inlet, communicates with one end of the air guiding passage, and the bottom substrate generates an air guiding outlet, and communicates with the air guiding passage The other end, and the flow path unit of the bottom layer stacks the flow path unit of the upper layer, so that the air guide outlet of the flow path unit located in the upper layer communicates with the air guide passage of the flow path unit located at the bottom layer, thereby causing each of the stacked channels The air guiding passages of the road unit are connected to each other, and the filling material is disposed in the air guiding passage of the separating flow path; a temperature control system is provided for the separating system to maintain an operating temperature of the separating system And controlling the separation operation of the sample to be tested at a certain temperature. a detection system, the detection system includes a detection chamber and a detector, the detection chamber is connected to the air outlet of the separation system, and the detector is disposed in the detection chamber; System, the recording system is connected to the detector of the detection system for performing gas layer phase processing analysis by collecting the signal of the detector; thereby, the carrier gas of the gas path system and the sample injection system are injected The sample to be tested is led out of the pipeline, and then introduced into the gas guide passage through the gas guide inlet, and the component compounds in the sample to be tested are filled by the gas guide passage. The adsorption of the material causes the components of the test sample to be exported to the gas outlet at different speeds and into the detection chamber of the detection system, and the detector of the detection system is the sample to be tested. Each component compound derived at different speeds is detected, and finally the signal of the detector is collected by the recording system to perform measurement analysis and recording of the sample to be tested.

Some exemplary embodiments embodying the features and advantages of the present invention are described in detail in the following description. It is to be understood that the present invention is capable of various modifications in various embodiments, and is not intended to limit the scope of the invention.

Figure 1 is a schematic view of a gas chromatography apparatus of the present invention. As shown in FIG. 1, the present invention provides a gas chromatography apparatus comprising 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 make the setting of the separation system 3 miniaturized and not affect the volume setting of the entire equipment, the present invention is to manufacture the separation system 3 in a semiconductor process to solve the chromatographic column of the conventional gas chromatograph. The problem of length setting can also achieve the purpose of gas chromatography separation, which will be explained below.

The gas path system 1 includes a carrier gas supply source 11, a constant voltage constant current device 12, a pipeline 13 and a pump 14, the carrier gas supply source 11 is a source for providing a carrier gas, and the pump 14 is disposed in the tube. In the path 13, the carrier gas supply source 11 and the constant voltage constant current device 12 are connected through the pipeline 13, and the carrier gas supplied from the carrier gas supply source 11 is guided by the pump 14 connected to the pipeline 13, wherein the carrier gas The carrier gas supplied from the supply source 11 must be chemically inert. The usual carrier gases are nitrogen (N ₂ ), argon (Ar), helium (He), hydrogen (H ₂ ), and carbon dioxide (CO ₂ ). The carrier gas is generally determined by the detector 52 of the detection system 5, and the carrier gas supply source 11 is generally a high-pressure cylinder. Since the flow rate of the carrier gas is one of the important parameters affecting chromatographic separation and qualitative analysis, Therefore, in order to stabilize the flow rate of the carrier gas stream, the carrier gas supply source 11 needs to use the constant voltage constant current device 12 for decompression and constant current to maintain the flow rate stable. The constant voltage constant current device 12 includes a pressure regulator 121 and a flow control valve 122 for regulating the carrier gas supplied from the carrier gas supply source 11 to maintain a stable flow rate in the pipeline 13, and then pumping the pipeline 13 to the pipeline 13 A carrier gas having a stable flow rate is derived.

Figure 7 is a schematic diagram of pump decomposition of the gas chromatography apparatus of the present invention. Referring to Fig. 7, the gas chromatography apparatus of the present invention is characterized in that the volume of the separation system 3 can be reduced, one of the reasons is that since the pump 14 uses a miniaturized pump 14, the pumping 14 is a gas. The pump includes a gas jet sheet 141, a cavity frame 142, an actuating body 143, an insulating frame 144, and a conductive frame 145 which are sequentially stacked. The air vent 141 includes a plurality of brackets 141a, a suspension piece 141b and a hollow hole 141c. The suspension piece 141b is flexibly vibrated, and the plurality of brackets 141a are adjacent to the circumference of the suspension piece 141b. In this embodiment, the number of the brackets 141a is There are four, respectively, adjacent to the four corners of the suspension piece 141b, but not limited thereto, and the hollow hole 141c is formed at the center position of the suspension piece 141b; the cavity frame 142 is carried on the suspension piece 141b, and the actuating body The 143 is stacked on the cavity frame 142 and includes a piezoelectric carrier 143a, an adjustment resonator 143b, and a piezoelectric plate 143c. The piezoelectric carrier 143a is stacked on the cavity frame 142. The adjustment resonance plate 143b is carried on the piezoelectric carrier 143a, and the piezoelectric plate 143c is placed on the adjustment resonance plate 143b, and is deformed after applying a voltage to drive the piezoelectric carrier 143a and the adjustment resonance plate 143b to reciprocate. Bending vibration; the insulating frame 144 is carried on the piezoelectric carrier 143a stacked on the actuating body 143, and the conductive frame 145 is stacked on the insulating frame 144, wherein the actuating body 143, the cavity frame 142 and the suspension Form a total between the pieces 141b The vibration chamber 146, wherein the thickness of the adjustment resonance plate 143b is larger than the thickness of the piezoelectric carrier 143a.

Referring again to FIGS. 8A to 8C, FIG. 8A is a schematic cross-sectional view of the pump of FIG. 7, and FIG. 8B and FIG. 8C are diagrams showing the operation of the pump 14 of the present invention shown in FIG. 8A. Referring to FIG. 8A, the pump 14 is disposed in the pipeline 13 through the bracket 141a, and the airflow chamber 147 is formed between the air vent 141 and the pipeline 13; please refer to FIG. 8B. When a voltage is applied to the piezoelectric plate 143c of the actuator 143, the piezoelectric plate 143c starts to deform due to the piezoelectric effect and simultaneously drives the adjustment resonator plate 143b and the piezoelectric carrier 143a. At this time, the gas orifice plate 141 is caused by Helm. The Helmholtz resonance principle is driven together so that the actuating body 143 moves upward. Due to the upward displacement of the actuating body 143, the volume of the airflow chamber 147 between the air venting fins 141 and the conduit 13 is increased, the internal air pressure thereof forms a negative pressure, and the gas outside the pump 14 will be due to the pressure gradient by the air venting fins. The gap between the bracket 141a of the 141 and the conduit 13 enters the airflow chamber 147 and is concentrated; finally, referring to Fig. 8C, the gas continuously enters the airflow chamber 147, causing the air pressure in the airflow chamber 147 to form a positive pressure. At this time, the actuating body 143 is driven downward by the voltage, compresses the volume of the airflow chamber 147, and pushes the gas in the airflow chamber 147 to allow the gas to begin to be transported.

The pump 14 is a gas pump. Of course, the pump 14 of the present invention can also be a microelectromechanical system gas pump produced by a microelectromechanical process, wherein the gas vent 141, the cavity frame 142, and the actuation The body 143, the insulating frame 144 and the conductive frame 145 are all made by surface micromachining technology to reduce the volume of the pump 14.

The sample injection system 2 described above is calibrated by an injection device (not shown, which is a common micro-injection crucible (including a gasification chamber), so it will not be described here) through the pipeline 13 of the pneumatic system 1 to quantify the sample. The ground is rapidly injected and instantaneously vaporized to facilitate the carrier gas carrying the sample to be tested into the separation system 3. The sample to be tested refers to a multi-component compound to be injected into the gas chromatograph apparatus of the present invention for separation and measurement.

Referring again to FIGS. 2A and 2B, FIG. 2A is a cross-sectional view of the separation system of FIG. 1, and FIG. 2B is a schematic diagram of the fluid unit of the separation system of FIG. As shown in FIGS. 2A and 2B, the above-described separation system 3 includes a separation flow path P composed of a plurality of semiconductor flow path units 31, and each flow path unit 31 is formed from a base substrate 311. A forming layer 312 is further formed by stacking an upper substrate 313, and a continuous extending loop-connecting gas guiding passage 314 is formed in the forming layer 312, and the upper substrate 313 is formed to form a gas guiding inlet 313a for communicating with the gas guiding gas. One end of the passage 314 and the bottom substrate 311 form a gas outlet 311a communicating with the other end of the gas guide passage 314, and the flow path unit 31 of the bottom layer is stacked with the flow path unit 31 of the upper layer to guide the flow path unit 31 located at the upper layer. The gas outlet 311a communicates with the gas inlet 313a of the flow path unit 31 located at the bottom layer, and causes the gas guide passages 314 of each flow path unit 31 of the stack to communicate with each other to constitute the separation flow path P, and the separation flow path P includes A filler material 32 is disposed in the gas guiding passage 314 to form a gas chromatography flow path.

3 to 5 are schematic views showing different implementations of the filling material of the separation system of the present invention disposed in the gas guiding passage. As shown in FIG. 3, the filler 32 described above may be an adsorbent porous polymer 32A, or the filler 32 may be an adsorbent molecular sieve material 32B and disposed in the gas guiding passage 314 in a filling manner. . In addition, as shown in FIG. 4, the filling material 32 may be a fixed liquid film 32C which is uniformly covered with a filling function on the filling carrier 32D, and the filling carrier 32D is filled and disposed in the air guiding passage 314, and the filling carrier 32D may be a crucible. The oxide has a hydroxyl group (-OH) on its surface to implant the fixed liquid film 32C. As shown in FIG. 5, the filler 32 may be attached to the inner wall surface of the air guiding passage 314 via a coating method, or may be disposed in a sputtering manner. The inner wall surface of the air guiding passage 314 is attached.

The above temperature control system 4 is provided for the separation system 3 to maintain an operating temperature for the separation system 3 and to control the separation operation of the sample to be tested at 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 ° C to 200 ° C to enhance the separation gas effect.

The detection system 5 includes a detection chamber 51 and a detector 52. The detection chamber 51 is connected to the air outlet 311a of the separation system 3.

The above-mentioned recording system 6 is connected to the detector 52 of the detection system 5 for collecting the signals of the detector 52 for gas layer phase processing analysis.

Figure 6 is a schematic diagram of chromatographic separation of the separation system of the present invention. It is known from the above description that the gas chromatography apparatus of the present invention produces the separation system 3 by a semiconductor process, the gas path system 1 introduces the carrier gas into the line 13 at a steady flow rate, and the sample injection system 2 is tested. The sample is metered into the rapid injection line 13, and the line 13 is connected to the gas inlet 313a of the separation system 3, and the carrier gas is supplied from the pump 14 and the sample to be tested is introduced into the gas inlet 313a to flow through the gas guiding passage 314. As shown in Fig. 6, the mixed gas of the sample to be tested and the carrier gas will be (by flowing in the direction of the arrow as shown) by the filler 32 on the gas guiding passage 314, since the filler 32 is tested The adsorption capacity of each compound in the sample is different, so the speed of different compounds in the gas guiding passage 314 will be different, the compound with larger adsorption force is slower, and the compound with smaller adsorption force is faster. Therefore, when the component compounds contained in the sample to be tested flow in the gas guiding passage 314, they are gradually separated by the adsorption of the filler 32, so that the compounds of the components contained in the sample to be tested are derived at different rates. The gas outlet 311a enters the detection chamber 51 of the detection system 5, and the detector 52 of the detection system 5 detects the different export rate of each component of the sample to be tested, and finally the recording system 6 Collecting the signal of the detector 52 to perform the measurement analysis and recording of the gas chromatographic processing of the sample to be used for detecting the separated gas, and analyzing the gas composition and concentration contained in each gas in the sample to be tested. The separation system 3 is produced by a semiconductor process, which can not only be miniaturized, but also solve the problem of setting the length of the chromatography column of the conventional gas chromatograph, replacing the chromatography column, and achieving the purpose of gas chromatography separation. For industrial use.

The detector 52 can be a heat conduction detector (TCD), a flame ionization detector (FID), an electron capture detector (ECD), a flame quantity detector (FPD), and thermal ionization detection. (TSD), infrared detector (IR), mass spectrometer (MS) or nuclear magnetic resonance spectrometer (NMR), etc., can separate the components and concentration changes of the sample to be separated from the separation system 3 Turn into a measurable electronic signal for information on qualitative and quantitative analysis.

In summary, the gas chromatography apparatus provided in the present invention uses a semiconductor process to produce a separation system, and the separation system is constructed by a plurality of flow path units to form a gas passage of a continuous extension loop, and the gas passage is disposed in the gas passage. The filling material enables the sample having a large amount of compound to have a different adsorption force for the compound containing different components of the sample to be tested when passing through the gas guiding passage, that is, the flow rate of the compound having a high adsorption force is slower and slower. The tendency of the lower adsorption rate of the compound with lower adsorption force is smaller. Different flow rates will gradually separate different compounds, and the purpose of gas chromatography separation is achieved, and then the components of the tested samples separated from each other are analyzed by a detector. Its concentration. In this way, through the miniaturized semiconductor process, the separation system is miniaturized, and the separation speed of the sample to be tested is increased by the micro pump, thereby improving the detection effect and efficiency.

This case has been modified by people who are familiar with the technology, but it is not intended to be protected by the scope of the patent application.

1‧‧‧ pneumatic system

11‧‧‧ Carrier gas supply

12‧‧‧Constant constant current device

121‧‧‧pressure regulator

122‧‧‧Flow control valve

13‧‧‧ pipeline

14‧‧‧ pump

141‧‧ ‧Hoop film

141a‧‧‧ bracket

141b‧‧‧suspension tablets

141c‧‧‧ hollow holes

142‧‧‧ cavity frame

143‧‧‧Acoustic body

143a‧‧‧Piezo carrier

143b‧‧‧Adjusting the resonance plate

143c‧‧ ‧thin plate

144‧‧‧Insulation frame

145‧‧‧Electrical frame

146‧‧‧Resonance chamber

147‧‧‧Airflow chamber

2‧‧‧ Sample Injection System

3‧‧‧Separation system

P‧‧‧Separate flow path

31‧‧‧Flow unit

311‧‧‧ bottom substrate

311a‧‧‧Air outlet

312‧‧‧ Forming layer

313‧‧‧Upper substrate

313a‧‧‧ gas inlet

314‧‧‧Gas Guide

32‧‧‧Filling materials

32A‧‧‧Porous polymer

32B‧‧‧Molecular sieve materials

32C‧‧‧Fixed film

32D‧‧‧filled carrier

4‧‧‧temperature control system

5‧‧‧Detection system

51‧‧‧Detection chamber

52‧‧‧Detector

6‧‧‧record system

Figure 1 is a schematic view of a gas chromatography apparatus of the present invention. Figure 2A is a schematic cross-sectional view of the separation system of Figure 1. Figure 2B is a schematic diagram of the fluid unit of the separation system of Figure 1. 3 to 5 are schematic views showing different implementations of the filling material of the separation system of the present invention disposed in the gas guiding passage. Figure 6 is a schematic diagram of chromatographic separation of the separation system of the present invention. Figure 7 is a schematic diagram of pump decomposition of the gas chromatography apparatus of the present invention. Fig. 8A is a schematic cross-sectional view of the pump of Fig. 7. Fig. 8B and Fig. 8C are schematic diagrams showing the operation of the pump of Fig. 8A.

Claims (21)

A gas chromatography apparatus comprising: a gas path system, wherein a carrier gas supply source and a constant voltage constant current device are connected through a pipeline to derive a flow rate stable carrier gas; a sample injection system is passed through an injection device The pipeline of the gas path system is connected to derive a sample to be tested; a separation system includes a separation flow path and a filler material, the separation flow path is connected to the pipeline of the gas path system, and the separation flow path is The plurality of flow path units are formed by a semiconductor process, and each flow path unit is formed by forming a forming layer on a base substrate and then stacking an upper substrate, and forming a continuous extending ring in the forming layer. a conductive gas passage connected to the substrate, the upper substrate generates a gas guiding inlet, communicates with one end of the gas guiding passage, and the bottom substrate generates an air guiding outlet, communicates with the other end of the air guiding passage, and the bottom layer The flow path unit of the upper layer of the flow path unit is connected to the air guide passage of the flow path unit at the bottom layer by the air guide outlet of the flow path unit located at the upper layer, thereby promoting the guide of each flow path unit of the stack Gas pass Being in communication with each other, and the filler material is disposed in the gas guiding passage of the separation flow path; a temperature control system is provided for the separation system to maintain an operating temperature of the separation system and controlled at a certain temperature Performing a separation operation of the sample to be tested; a detection system comprising a detection chamber and a detector, the detection chamber being connected to the air outlet of the separation system, the detector setting In the detection chamber, a recording system is connected to the detector of the detection system for performing gas layer phase processing analysis by collecting signals of the detector; thereby, the gas path system The carrier gas and the sample to be injected injected by the sample injection system are led out from the pipeline, and then introduced into the gas guide passage through the gas guide inlet, and the component compounds in the sample to be tested are Adsorbed by the filler material in the gas guiding passage, causing the components of the test sample to be derived at the gas outlet and entering at different speeds. In the detection chamber of the detection system, the detector of the detection system detects the component compounds derived from the sample at different speeds, and finally the detector system collects the detectors. The signal is analyzed and recorded for the measurement of the sample to be tested. The gas chromatography apparatus according to claim 1, wherein the filler is a porous polymer having adsorptivity, and the filling is disposed in the gas guiding passage. The gas chromatography apparatus according to claim 1, wherein the filler is an adsorbent molecular sieve material, and the filling is disposed in the gas guiding passage. The gas chromatography apparatus according to claim 1, wherein the filler material is a fixed liquid film covering the uniformity of the filling carrier and having an adsorption function, and the filling is disposed in the gas guiding passage. The gas chromatography apparatus according to claim 4, wherein the filled carrier is an oxide of cerium, and a hydrocarbon group is provided on the surface to implant the fixed liquid film. The gas chromatography apparatus according to claim 1, wherein the filler material is directly adhered to a surface of the inner wall of the gas guiding passage of the separation flow path. The gas chromatography apparatus according to claim 1, wherein the filler material is directly adhered to the inner wall surface of the gas guiding passage of the separation flow path. The gas chromatography apparatus according to claim 1, wherein the gas path system comprises a pump disposed in the pipeline to control the flow rate of the carrier gas and the sample to be separated into the separation. The gas path of the flow path. The gas chromatography apparatus of claim 1, wherein the injection device of the injection system is configured to quantitatively inject the sample to be measured and instantaneously vaporize. The gas chromatography apparatus of claim 8, wherein the pump is a MEMS pump. The gas chromatography apparatus of claim 8, wherein the pump is a gas pump, comprising: a gas jet sheet comprising a plurality of brackets, a suspension sheet and a hollow hole, the suspension sheet Flexibly vibrating, the plurality of brackets are adjacent to the periphery of the suspension sheet and provide elastic support of the suspension sheet, and the hollow holes are formed at a center position of the suspension sheet, and the air vent sheet is positioned in the pipeline through a plurality of brackets, and Forming an air flow chamber with the air guide inlet, and at least one gap is formed between the plurality of brackets and the suspension piece; a cavity frame is stacked on the suspension piece; the movable body is stacked Reciprocatingly bending vibration is generated on the cavity frame by receiving a voltage; an insulating frame is stacked on the actuating body; and a conductive frame is disposed on the insulating frame; wherein the actuating frame Forming a resonant cavity between the body, the cavity frame and the suspension piece, driving the actuating body to drive the air venting piece to resonate, causing the suspension piece of the air venting piece to reciprocally vibrate and displace The carrier gas and the sample to be tested enter the gas flow chamber through the at least one gap to realize the transport flow of the carrier gas and the sample to be tested. The gas chromatography apparatus of claim 11, wherein the actuating body comprises: a piezoelectric carrier plate stacked on the cavity frame; an adjustment resonance plate, the carrier is stacked on the pressure And a piezoelectric plate stacked on the adjustment resonator plate to receive the voltage to drive the piezoelectric carrier and the adjustment resonator plate to generate reciprocating bending vibration. The gas chromatography apparatus of claim 12, wherein the thickness of the adjustment resonator plate is greater than the thickness of the piezoelectric carrier. The gas chromatography apparatus of claim 1, wherein the detector is a heat conduction detector. The gas chromatography apparatus of claim 1, wherein the detector is a flame ionization detector. The gas chromatography apparatus according to claim 1, wherein the detector is an electron capture Detector. The gas chromatography apparatus of claim 1, wherein the detector is a flame quantity detector. The gas chromatography apparatus of claim 1, wherein the detector is a thermal ionization detector. The gas chromatography apparatus of claim 1, wherein the detector is an infrared detector. The gas chromatography apparatus of claim 1, wherein the detector is a mass spectrometer. The gas chromatography apparatus according to claim 1, wherein the detector is a nuclear magnetic resonance spectrometer.