TWI677682B - Separating system of gas chromatography device - Google Patents

Abstract

A separation system of a gas chromatography device includes a separation flow path, which is composed of a plurality of flow path unit stacks made by a semiconductor process. Each flow path unit is made of a forming layer on a base substrate and then stacked one The upper base material is formed, and a continuous air circulation path is formed in the forming layer. Filling material is provided in the air guide path, so that the test sample entering the separation flow path is pulled by the adsorption force of the filling material, and different compounds contained in the test sample have different adsorption forces. It is drawn by different adsorption forces, so that different compounds contained in the test sample generate different flow rates in the separation flow path, so that different compounds contained in the test sample are gradually separated in the separation flow path.

Description

Separation system of gas chromatography equipment

This case relates to a separation system for a gas chromatography device, and in particular to a gas separation system that separates and analyzes compounds that are volatile without decomposition in organic chemistry.

Gas chromatography (GC) is a technique used in organic chemistry to separate and purify volatile and thermally stable compounds, both through the mobile phase and the stationary phase. Interaction, so that the components contained in the mixture have different flow rates in the system to achieve the purpose of separation.

However, there are currently many types and types of gas chromatographs. Although their appearance and structure are different, they usually consist of the following 6 basic systems: (1) gas path system, (2) sample injection system, (3) The separation system, (4) temperature control system, (5) detection system and (6) recording system constitute a relatively large volume of equipment. This is because a chromatography column is required in the separation system. To separate the components of a sample, a chromatography column is the heart of a gas chromatograph. Because the efficiency of a chromatography 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 chromatography column of the general gas chromatography It is a very long setting. However, because the chromatography column needs to be placed in a temperature control system to maintain the temperature requirements of constant temperature operation, the length of the chromatography column will affect the volume setting of the temperature control system. Set multiple loops to reduce the length to minimize the size of the temperature control system. However, at present, the column arrangement of gas chromatography is still quite large.

In view of this, 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 actually the subject of this case.

The main purpose of this case is to provide a separation system for a gas chromatography device. A continuous extension loop gas guide path is constructed by a plurality of flow path units of the separation system made by a semiconductor process, and a filling material is provided in the gas guide path. Therefore, when a test sample with a large amount of mixture passes through the air-conducting path, the adsorption force of the filler on the compounds of different components of the test sample is different, and the flow rate of the compound with higher adsorption force will become slower and slower, The decreasing trend of the compound flow rate is small. Different flow rates will gradually separate different compounds to achieve the purpose of gas chromatography separation. Then the detector analyzes the components and concentrations of the separated test samples. The semiconductor process can miniaturize the separation system, and then increase the separation speed of the sample under test through a miniature pump, which can improve the detection effect and efficiency.

A broad implementation of this case is a separation system for a gas chromatography device, including: a separation flow path, which is composed of a stack of a plurality of flow path units made by a semiconductor process, and each flow path unit consists of a substrate A forming layer is formed on the material, and an upper substrate is stacked, and a continuous extending air circulation path is formed on the forming layer. The upper substrate generates a gas conduction inlet and communicates with the gas conduction. One end of the passage and the bottom substrate generate a gas-conducting outlet, which is connected to the other end of the gas-conducting passage, and the bottom flow path unit is stacked with the upper flow path unit to locate the gas flow in the upper flow path unit. The outlet communicates with the air conduction path of the flow path unit on the bottom layer, so that the air conduction paths of each flow path unit in the stack can communicate with each other; and a filling material is provided in the air conduction path of the separation flow path; Thereby, the test sample is introduced from the air guide inlet into the air guide passage flowing through the separation flow path, and the test sample is formed by the filling material on the air guide passage for adsorption and separation of compounds of various components. Each component compound contained in the tested sample is exported to the gas conducting outlet at different speeds for measurement and analysis records.

1‧‧‧pneumatic system

11‧‧‧ Carrier gas supply source

12‧‧‧ constant voltage and constant current device

121‧‧‧pressure regulator

122‧‧‧Flow Control Valve

13‧‧‧pipe

14‧‧‧Pump

141‧‧‧air hole film

141a‧‧‧bracket

141b‧‧‧ Suspension tablet

141c‧‧‧Hollow

142‧‧‧cavity frame

143‧‧‧actuator

143a‧‧‧piezoelectric carrier

143b‧‧‧Adjust resonance plate

143c‧‧‧Piezoelectric plate

144‧‧‧Insulated frame

145‧‧‧ conductive frame

146‧‧‧Resonant Chamber

147‧‧‧Airflow chamber

2‧‧‧ sample injection system

3‧‧‧ separation system

P‧‧‧ Separated flow path

31‧‧‧flow unit

311‧‧‧ substrate

311a‧‧‧Air outlet

312‧‧‧forming layer

313‧‧‧upper substrate

313a‧‧‧Air inlet

314‧‧‧Air conduction pathway

32‧‧‧filler

32A‧‧‧Porous polymer

32B‧‧‧ molecular sieve material

32C‧‧‧Fixed liquid film

32D‧‧‧filled carrier

4‧‧‧Temperature Control System

5‧‧‧ Detection System

51‧‧‧detection chamber

52‧‧‧ Detector

6‧‧‧Recording System

Figure 1 is a schematic diagram of the gas chromatography equipment of this case.

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 diagrams of different implementations in which the filling material of the separation system of the present invention is arranged in the air guide passage.

Figure 6 shows the chromatographic separation of the separation system in this case.

FIG. 7 is a pump breakdown diagram of the gas chromatography apparatus of the case.

Figure 8A is a schematic cross-sectional view of the pump of Figure 7.

Figures 8B and 8C are schematic diagrams of the operation of the pump in Figure 8A.

Some typical embodiments embodying the features and advantages of this case will be described in detail in the description in the subsequent paragraphs. It should be understood that the present case can have various changes in different aspects, all of which do not depart from the scope of the present case, and the descriptions and diagrams therein are essentially for the purpose of illustration, rather than limiting the case.

As shown in FIG. 1, this case provides a gas chromatography device including 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 setting of the separation system 3 so that it does not affect the volume setting of the entire equipment, this case is made by using the semiconductor process to separate the layers of the conventional gas chromatograph. The problem of setting the length of the analytical column and achieving the purpose of gas chromatography separation will be explained below.

The above-mentioned gas path system 1 is connected by a carrier gas supply source 11 and a constant-voltage constant-current device 12 through a pipeline 13, and a pump 14 connected to the pipeline 13 leads to a carrier gas with a stable flow rate. The carrier gas provided by the gas supply source 11 must be chemically inert. Common carrier gases are nitrogen (N2), argon (Ar), helium (He), hydrogen (H2), and carbon dioxide (CO2). As for the choice of carrier gas, the detector 52 of the detection system 5 is usually used to determine the carrier gas. The carrier gas supply source 11 is usually a high-pressure steel cylinder. The velocity of the carrier gas is one of the important parameters affecting chromatographic separation and qualitative analysis. Therefore, in order to maintain a stable flow rate of the carrier gas, the carrier gas supply source 11 needs to use a constant voltage and constant current device 12 to reduce pressure and maintain a constant flow rate. The constant voltage and constant current device 12 includes a pressure regulator 121 and a flow control valve 122. In order to adjust the carrier gas provided by the carrier gas supply source 11 to maintain a stable flow rate in the pipeline 13, the pump 14 connected to the pipeline 13 leads to a stable flow velocity of the carrier gas.

Please refer to Fig. 7 to Fig. 8C. The feature of the gas chromatography equipment in this case is that it can reduce the volume of the separation system 3. One of the reasons is that the above-mentioned pump 14 uses a miniaturized pump 14. This pump 14 is a gas pump, which includes an air jet hole 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 jet hole sheet 141 includes a plurality of brackets 141a, a suspension sheet 141b, and a hollow hole 141c. The suspension sheet 141b can be flexibly vibrated, and the plurality of brackets 141a are adjacent to the periphery of the suspension sheet 141b. In this embodiment, the number of the brackets 141a There are four, which are respectively adjacent to the four corners of the suspension sheet 141b, but not limited to this, and a hollow hole 141c is formed at the center position of the suspension sheet 141b; the cavity frame 142 is carried on the suspension sheet 141b to actuate the body The 143 carrier is stacked on the cavity frame 142, and includes a piezoelectric carrier plate 143a, an adjustment resonance plate 143b, and a piezoelectric plate 143c. The piezoelectric carrier 143a is stacked on the cavity frame 142. The adjusting resonance plate 143b is stacked on the piezoelectric carrier plate 143a, and the piezoelectric plate 143c is stacked on the adjusting resonance plate 143b, and is deformed after the voltage is applied to drive the piezoelectric carrier plate 143a and the adjustment resonance plate 143b for reciprocation. bending Vibration; the insulating frame 144 is carried on the piezoelectric carrier plate 143a stacked on the actuating body 143, and the conductive frame 145 is carried on the insulating frame 144, wherein the actuating body 143, the cavity frame 142 and the suspension sheet A resonance cavity 146 is formed between 141b, wherein the thickness of the adjustment resonance plate 143b is greater than the thickness of the piezoelectric carrier plate 143a.

Please refer to FIGS. 8A to 8C again. FIGS. 8B and 8C are schematic diagrams of the operation of the pump 14 in the present case shown in FIG. 8A. Please refer to FIG. 8A first, the pump 14 is arranged in the pipeline 13 through the bracket 141a, and the air flow cavity 147 is formed between the air jet orifice 141 and the pipeline 13; please refer to FIG. 8B again, when When a voltage is applied to the piezoelectric plate 143c of the actuator 143, the piezoelectric plate 143c begins to deform due to the piezoelectric effect and synchronously drives the adjustment of the resonant plate 143b and the piezoelectric carrier plate 143a. The principle of Helmholtz resonance is driven together, which causes the actuating body 143 to move upward. Due to the upward displacement of the actuating body 143, the volume of the air flow chamber 147 between the air jet hole 141 and the pipe 13 increases, and the interior The air pressure forms a negative pressure, and the gas outside the pump 14 will enter the air flow chamber 147 and collect pressure from the gap between the bracket 141a of the air jet orifice plate 141 and the pipeline 13 due to the pressure gradient; finally, refer to FIG. 8C, the gas Continuously enter the airflow chamber 147, so that the air pressure in the airflow chamber 147 forms a positive pressure. At this time, the actuator 143 is driven downward by the voltage to move, compress the volume of the airflow chamber 147, and push the airflow chamber. 147 gas, so that gas can begin to be transported.

The above-mentioned pump 14 is a gas pump. Of course, the pump 14 in this case may also be a micro-electro-mechanical system gas pump manufactured by a micro-electro-mechanical process. Among them, the air jet hole sheet 141, the cavity frame 142, The body 143, the insulating frame 144, and the conductive frame 145 can be made by surface micromachining technology to reduce the volume of the pump 14.

The sample injection system 2 described above is quantified by an injection device (not shown, which is a common micro-injection port (including a gasification chamber), so it will not be repeated here) through the pipeline 13 of the gas path system 1 Ground fast injection and instantaneous gasification to facilitate carrier gas to carry the test sample into the separation system 3. The test sample refers to the multi-component compounds to be injected and separated in the gas chromatography equipment of this case.

Please refer to FIG. 2A and FIG. 2B again. The above separation system 3 includes a separation flow path P, which is formed by stacking a plurality of flow path units 31 made of semiconductor, and each flow path unit 31 is composed of a bottom substrate. A forming layer 312 is formed on 311, and an upper substrate 313 is stacked, and a continuous extending gas passage 314 is formed on the forming layer 312. The upper substrate 313 generates a gas guiding inlet 313a, which communicates with An air-conducting outlet 311a is generated at one end of the air-conducting path 314 and the bottom substrate 311, and communicates with the other end of the air-conducting path 314. The air-conducting outlet 311a of 31 communicates with the air-conducting inlet 313a of the flow path unit 31 located at the bottom layer, so that the air-conducting path 314 of each flow path unit 31 in the stack can communicate with each other to form the separation flow path P, and the separation flow path P contains a filling material 32 and is positioned in the gas guide passage 314 to form a gas chromatography flow path.

As shown in FIG. 3, the above-mentioned filling material 32 may be an adsorbent porous polymer 32A, or the filling material 32 may be an adsorbent molecular sieve material 32B, and is provided in the air guiding path 314 in a filling manner. . In addition, as shown in FIG. 4, the filling material 32 can also be a fixed carrier 32D covered with a fixed liquid film 32C having an adsorption function uniformly. The filling carrier 32D is filled in the air guiding path 314, and the filling carrier 32D can be silicon. The oxide has a hydroxyl group (-OH) on its surface so that the fixed liquid film 32C can be planted. As shown in FIG. 5, the filling material 32 may be a fixed liquid film 32C attached to the inner wall surface of the air guide passage 314 through a coating method, or may be provided by a sputtering method. The air guide passage 314 is attached to the inner wall surface.

The temperature control system 4 described above is provided for the separation system 3 to maintain an operating temperature for the separation system 3 and control the separation operation of the test sample 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 improve the effect of separating the gas.

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

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

It is known from the above description that the gas chromatography device in this case is produced by using a semiconductor process for the separation system 3. The gas path system 1 introduces a carrier gas into the pipeline 13 at a stable flow rate, and the sample injection system 2 will be tested. The sample is quantitatively injected into the pipeline 13 quickly, and the pipeline 13 is connected to the gas guide inlet 313a of the separation system 3, and the carrier gas is sent by the pump 14 and the test sample is introduced into the gas guide inlet 313a and circulates in the gas guide passage 314. As shown in Fig. 6, the mixed gas of the test sample and the carrier gas (when flowing in the direction of the arrow shown in the figure) is subjected to the adsorption and separation of the compounds of each component by the filling material 32 on the gas conducting path 314. The adsorption force of the material 32 for each compound in the test sample is different, so the speed of different compounds in the air guide path 314 will vary. The compound with the higher adsorption force has a slower speed and the compound with the lower adsorption force. Its speed is fast, so when the compounds contained in the test sample flow through the air guide path 314, they will be gradually separated by the adsorption of the compounds of the various components by the filler 32, so that the The contained compounds are exported at different rates to the air-conducting outlet 311a and entered into the detection chamber 51 of the detection system 5. The detector 52 of the detection system 5 Different rates are used for detection. Finally, the signal from the detector 52 is collected by the recording system 6 for the measurement and analysis of the gas chromatographic processing of the test sample in order to detect the separated gas and analyze each gas in the test sample. The gas composition and concentration contained in it. In this way, the separation system 3 is produced by a semiconductor process, which can not only miniaturize, solve the problem of the length of the chromatography column of the conventional gas chromatography, replace the chromatography column, but also achieve the purpose of gas chromatography separation. For industrial use.

The above-mentioned detector 52 may be a thermal conductivity detector (TCD), a flame ionization detector (FID), an electronic capture detector (ECD), a flame light detector (FPD), and a thermal ionization detector. Any device such as a TSD, infrared detector (IR), mass spectrometer (MS), or nuclear magnetic resonance spectrometer (NMR) can separate data such as the composition and concentration change of the test sample flowing out of the separation system 3. Transformed into measurable electronic signals for qualitative and quantitative analysis.

To sum up, the separation system for gas chromatography equipment provided in this case utilizes a plurality of flow path units produced by a semiconductor process to construct a continuous extended loop of a gas conducting path, and the gas conducting path The filling material is set inside, so that when the test sample with a large amount of mixture passes through the air conduction path, the filling material has different adsorption power to the compounds of different components contained in the test sample. The lower the flow rate of the compounds with a lower force, the smaller the tendency. The different flow rates will gradually separate the different compounds to achieve the purpose of gas chromatography separation, and then use the detector to analyze the components and concentrations of the separated test samples. . In this way, through the miniaturization of the semiconductor process, the separation system is miniaturized, and then the separation speed of the test sample is increased by the miniature pump, which can improve the detection effect and efficiency.

This case can be modified by anyone who is familiar with this technology, but it is not as bad as the protection of the scope of patent application.

Claims (22)

A separation system for a gas chromatography device includes: a separation flow path, which is composed of a stack of a plurality of flow path units made by a semiconductor process, and each flow path unit is made of a forming layer on a bottom substrate and then An upper substrate is stacked, and a continuous gas path is formed in the forming layer. The upper substrate generates a gas inlet, which is connected to one end of the gas channel and the base. A gas-conducting outlet is connected to the other end of the gas-conducting path, and the gas-conducting outlet of the flow path unit on the upper layer communicates with the gas-conducting inlet of the flow path unit on the bottom layer, which promotes each of the flow paths in the stack. The gas conducting paths of the unit can communicate with each other; and a filling material is provided in the gas conducting path of the separation flow path; thereby, a test sample is introduced from the gas guiding inlet into the flow path of the separation flow path. In the air passage, the test sample is adsorbed and separated by the filling material on the air conduction passage for the compounds of various components, and the component compounds contained in the test sample are exported at different speeds to the air conduction outlet for measurement analysis and analysis. . The separation system of the gas chromatography device according to item 1 of the scope of the patent application, wherein the filling material is a porous polymer having an adsorption property, and the filling material is arranged in the gas conducting path. The separation system of the gas chromatography device according to item 1 of the scope of the patent application, wherein the filling material is an adsorbent molecular sieve material, and the filling material is arranged in the gas conducting path. The separation system of the gas chromatography device according to item 1 of the scope of application for patent, wherein the filling material is a fixed liquid film covered with a uniform and adsorption function on a filled carrier, and filled in the air conducting path. The separation system of a gas chromatography device according to item 4 of the application, wherein the filled carrier is an oxide of silicon and the surface has a hydroxyl group so that the fixed liquid film is planted. The separation system of the gas chromatography device according to item 1 of the scope of the patent application, wherein the filling material is a fixed liquid film directly coated on the inner wall surface of the air conduction path of the separation flow path and attached. The separation system of the gas chromatography device according to item 1 of the scope of the patent application, wherein the filling material is a fixed liquid film directly sputtered on the inner wall surface of the gas conduction path of the separation flow path. The separation system of a gas chromatography device according to item 1 of the scope of the patent application, wherein the gas inlet of the separation flow path is connected to a pump, and the pump communicates with a gas path system and a sample injection system through a pipeline. The gas path system is connected by a carrier gas supply source and a constant-voltage constant-current device through the pipeline and is discharged by the pump. A carrier gas having a stable flow rate enters the gas conduction path of the separation flow path, and the sample is injected. The system is connected by an injection device through the pipeline, so that after the test sample is injected from the injection device, it is introduced by the pump into the air conduction path of the separation flow path. The separation system for a gas chromatography device according to item 8 of the application, wherein the pump is a MEMS pump. The separation system of a gas chromatography device according to item 8 of the scope of the patent application, wherein the pump is a gas pump, which includes: an air jet hole sheet, including a plurality of brackets, a suspension sheet, and a hollow hole, The suspension sheet can be bent and vibrated, the plurality of brackets are adjacent to the periphery of the suspension sheet, and the hollow hole is formed at the center position of the suspension sheet. The plurality of brackets are arranged to locate the pipeline and provide elastic support for the suspension sheet. An air flow cavity is formed between the air jet hole piece and the pipeline, and at least one gap is formed between the plurality of brackets and the suspension piece; a cavity frame is carried on the suspension piece; A bearing stack is placed on the cavity frame to receive a voltage to generate reciprocating bending vibration; an insulating frame is placed on the actuating body; and a conductive frame is provided on the insulating frame; wherein A resonance chamber is formed between the actuating body, the cavity frame and the suspension sheet. By driving the actuating body to drive the air jet hole sheet to generate resonance, the suspension sheet of the air jet hole sheet is generated. Double the vibration displacement to cause the carrier gas and the sample tested by the at least one void of the gas stream entering the chamber, and then discharged from the gas flow path, and said carrier gas to achieve the transfer of the sample measured by the flow. The separation system for a gas chromatography device according to item 10 of the patent application scope, wherein the actuating body comprises: a piezoelectric carrier plate, which is stacked on the cavity frame; an adjustment resonance plate, which is stacked On the piezoelectric carrier plate; and a piezoelectric plate carrying a stack on the adjustment resonance plate to receive the voltage to drive the piezoelectric carrier plate and the adjustment resonance plate to generate reciprocating bending vibration. The separation system of the gas chromatography device according to item 11 of the scope of the patent application, wherein the thickness of the adjusting resonance plate is greater than the thickness of the piezoelectric carrier plate. The separation system of the gas chromatography device as described in the first item of the patent application scope, wherein the separation system is set in a temperature control system for the separation system to maintain an operating temperature and to control the process at a certain temperature. Separation of test samples. The separation system of a gas chromatography device according to item 1 of the scope of patent application, wherein the separation system is connected to a detection system and a recording system, and the detection system includes a detection chamber and a detector. The detection chamber is respectively connected to the gas conducting outlet of the separation system, and each component compound contained in the test sample is exported to the gas conducting outlet at different speeds for detection by the detector, and the recording system is connected to the detection The detector of the system is used to collect the signal of the detector for measurement analysis and recording of the gas chromatography of the test sample. The separation system of a gas chromatography device according to item 14 of the scope of application for a patent, wherein the detector is a heat conduction detector. The separation system for a gas chromatography device according to item 14 of the scope of application, wherein the detector is a flame ionization detector. The separation system for a gas chromatography device according to item 14 of the scope of the patent application, wherein the detector is an electronic capture detector. The separation system for a gas chromatography device according to item 14 of the scope of application, wherein the detector is a flame light detector. The separation system of a gas chromatography device according to item 14 of the scope of application, wherein the detector is a thermal ionization detector. The separation system of a gas chromatography device according to item 14 of the scope of application, wherein the detector is an infrared detector. The separation system for a gas chromatography device according to item 14 of the scope of application, wherein the detector is a mass spectrometer. The separation system for a gas chromatography device according to item 14 of the scope of application, wherein the detector is a nuclear magnetic resonance spectrometer.