CN108490104B - Miniature gas chromatographic column chip and preparation method thereof - Google Patents
Miniature gas chromatographic column chip and preparation method thereof Download PDFInfo
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- CN108490104B CN108490104B CN201810179691.4A CN201810179691A CN108490104B CN 108490104 B CN108490104 B CN 108490104B CN 201810179691 A CN201810179691 A CN 201810179691A CN 108490104 B CN108490104 B CN 108490104B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/60—Construction of the column
- G01N30/6052—Construction of the column body
- G01N30/606—Construction of the column body with fluid access or exit ports
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The invention provides a micro gas chromatographic column chip and a preparation method thereof. The chip includes: at least two mutually independent chromatographic channels filled with stationary phases of different phases; at least one connecting channel, wherein each connecting channel is connected between two adjacent chromatographic channels and is used for communicating the two adjacent chromatographic channels; and at least one solenoid valve, each solenoid valve is arranged in one of the connecting channels and is used for opening or closing the connecting channel so as to enable gas to flow through the two chromatographic channels communicated with the connecting channel when the connecting channel is opened. According to the scheme of the invention, because the single chromatographic channel or the combined use of a plurality of chromatographic channels can be realized by opening or closing the electromagnetic valve, active selection can be carried out according to the environmental gas, namely, a plurality of stationary phases can be filled in the chromatographic channel, the types of the separated gas are greatly improved, the mixed gas with a complex background does not need to be combined by a plurality of chromatographic columns, and the volume of the system is greatly reduced.
Description
Technical Field
The invention relates to the technical field of gas separation, in particular to a micro gas chromatographic column chip and a preparation method thereof.
Background
Pollution gas such as various VOCs, CO and CO in multiple fields such as environmental air quality, fixed point pollution source, sudden environmental pollution and the like2、SO2And H2Permanent gases such as S all have the requirement of rapid detection. Background gas components are complex and various, and most detectors in the market have the characteristic of poor interference resistance, so that the combination of a chromatographic technology is often needed.
The separation of the mixed polluted gas is realized by utilizing the chromatographic separation technology so as to solve the technical bottleneck of poor resolution of the detector. However, the existing separation chromatography columns have a limited ability to separate gas species due to the limitation of the stationary phase on which they can be immobilized. For multi-component and multi-variety environmental samples with complex backgrounds, a single chromatographic column is adopted, effective separation of most gases in the samples is difficult to realize, multi-chromatographic columns are often required to work in parallel, separation of the gases in the complex environments can be achieved, and therefore the size, power consumption, cost and the like of the system are greatly increased.
Disclosure of Invention
The invention aims to solve the technical problems of large volume and high power consumption of a chromatographic column chip when multi-component and multi-type environmental sample separation is carried out in the prior art.
The invention provides a micro gas chromatographic column chip, comprising:
at least two mutually independent chromatographic channels filled with stationary phases of different phases;
at least one connecting channel, wherein each connecting channel is connected between two adjacent chromatographic channels and is used for communicating the two adjacent chromatographic channels; and
at least one solenoid valve, each solenoid valve is arranged in one of the connecting channels and is used for opening or closing the connecting channel, and when the connecting channel is opened, gas flows through the two chromatographic channels communicated with the connecting channel.
Optionally, the micro gas chromatography column chip further comprises:
the main inlet is communicated with one of the chromatographic channels at the outermost side and is used for introducing gas into the chromatographic channel; and
a main outlet communicating with one of said chromatographic channels outermost at the other end for discharging said gas when said at least one connecting channel is open.
Optionally, the micro gas chromatography column chip further comprises:
and the at least one branch outlet is respectively corresponding to the at least one connecting channel, and each branch outlet is communicated with the corresponding connecting channel and used for discharging the gas from the branch outlet corresponding to the connecting channel when the gas flows to the connecting channel in a closed state.
Optionally, at least two of the chromatographic channels comprise:
a first chromatographic channel filled with a solid stationary phase;
and a second chromatographic channel filled with a liquid or colloidal stationary phase.
Optionally, a plurality of partition walls are arranged in parallel in the second chromatography passage, each partition wall being configured to extend in the direction in which the gas flows.
Optionally, a filter is disposed in the first chromatography channel at a position close to the corresponding branch outlet, for preventing loss of the stationary phase in the first chromatography channel.
Optionally, the material of the stationary phase filled in the first chromatographic channel is selected from one or more of OV-1, OV-101, polydimethylsiloxane, carbon nano-tube and graphene;
the stationary phase filled in the second chromatographic channel is one or a combination of more of polymer microspheres, carbon molecular sieves, graphene and carbon nanotubes.
Optionally, the chromatography channel is serpentine.
Correspondingly, the invention also provides a preparation method of the micro gas chromatographic column chip, which comprises the following steps:
etching at least two mutually independent chromatographic channels on a substrate;
bonding and sealing a glass substrate for sealing with the chromatographic channel;
respectively pumping the configured stationary phases with different phases to at least two chromatographic channels, so that the stationary phases with different phases are respectively filled in the at least two chromatographic channels;
and communicating at least two chromatographic channels through at least one connecting channel, introducing inert gas into the communicated chromatographic channels, and then carrying out aging treatment.
Optionally, after etching at least two mutually independent chromatographic channels on a substrate, the method further comprises the following steps:
etching a total inlet and a total outlet on the substrate, and enabling the total inlet and the total outlet to be respectively communicated with the two outermost chromatographic channels.
According to the scheme of the invention, the single chromatographic channel or the combined use of a plurality of chromatographic channels can be realized by opening or closing the electromagnetic valve, so that active selection can be carried out according to the environmental gas, and the gas separation efficiency is further improved. The chromatographic column chip can be filled with various stationary phases in a chromatographic channel, so that the types of separated gases are greatly improved, the mixed gas with a complex background does not need to be combined by a plurality of chromatographic columns, and the volume of the system is greatly reduced.
The above and other objects, advantages and features of the present invention will become more apparent to those skilled in the art from the following detailed description of specific embodiments thereof, taken in conjunction with the accompanying drawings.
Drawings
Some specific embodiments of the invention will be described in detail hereinafter, by way of illustration and not limitation, with reference to the accompanying drawings. The same reference numbers in the drawings identify the same or similar elements or components. Those skilled in the art will appreciate that the drawings are not necessarily drawn to scale. In the drawings:
FIG. 1 is a schematic structural view of a micro gas chromatography column chip according to a first embodiment of the present invention;
FIG. 2 is a schematic flow chart of a method of fabricating a micro gas chromatography column chip according to one embodiment of the invention.
Reference numerals:
1-micro gas chromatography column chip; 10-a first chromatography channel; 20-a second spectral channel; 201-partition wall; 30-a connecting channel; 40-electromagnetic valve; 50-total inlet; 60-total outlet; 70-a branch outlet; 80-a filter.
Detailed Description
FIG. 1 shows a schematic configuration diagram of a micro gas chromatography column chip 1 according to a first embodiment of the present invention. As shown in FIG. 1, the micro gas chromatography column chip 1 comprises two mutually independent chromatography channels, a connecting channel and a solenoid valve 40. The two chromatographic channels are a first chromatographic channel 10 and a second chromatographic channel 20, respectively. The first chromatographic channel 10 is filled with a solid stationary phase, and the second chromatographic channel 20 is filled with a liquid or colloidal stationary phase. The connecting channel is provided between the first color spectrum channel 10 and the second color spectrum channel 20 for communicating the first color spectrum channel 10 and the second color spectrum channel 20. A solenoid valve 40 is located in the connection passage for opening or closing the connection passage. The micro gas chromatography column chip 1 further comprises a main inlet 50 and a main outlet 60. The main inlet 50 communicates with the first chromatography channel 10 for introducing gas into the first chromatography channel 10. The main outlet 60 communicates with the second chromatography passage 20 for discharging the gas flowing through the second chromatography passage 20 from the first chromatography passage 10 when the solenoid valve 40 is opened. The micro gas chromatography column chip 1 further comprises a branch outlet 70, the branch outlet 70 being in communication with the connection channel and being arranged to discharge the gas of the first chromatography channel 10 when the solenoid valve 40 is closed.
In the above embodiment, when the solenoid valve 40 is opened, the gas enters the first chromatography channel 10 from the main inlet 50, flows through the first chromatography channel 10 and the second chromatography channel 20 in sequence, and is discharged from the main outlet 60. When the solenoid valve 40 is closed, gas enters the first chromatographic channel 10 from the main inlet 50, flows through the first chromatographic channel 10, and is discharged from the branch outlet 70.
According to the scheme of the embodiment of the invention, the electromagnetic valve 40 can be opened or closed to realize the use of a single chromatographic channel or the combined use of a plurality of chromatographic channels, so that the active selection can be carried out according to the ambient gas, and the gas separation efficiency is further improved. The chromatographic column chip can be filled with various stationary phases in a chromatographic channel, so that the types of separated gases are greatly improved, the mixed gas with a complex background does not need to be combined by a plurality of chromatographic columns, and the volume of the system is greatly reduced.
As shown in fig. 1, the first chromatography channel 10 is configured in a serpentine shape and is hollow inside. The material of the stationary phase filled in the composite material is selected from one or more of OV-1, OV-101, polydimethylsiloxane, carbon nano-tube and graphene. In the first chromatographic channel 10, the stationary phase is filled in the channel, or a layer of stationary phase is deposited on the inner wall of the channel by chemical synthesis. A filter 80 is provided at the end of the first chromatography passage 10 near the branch outlet 70 for preventing loss of the fixed phase in the first chromatography passage 10. The second chromatography channel 20 is configured in a serpentine shape. The stationary phase filled in the second chromatographic channel 20 is one or a combination of more of polymer microspheres, carbon molecular sieves, graphene and carbon nanotubes. In the second chromatographic channel 20, the stationary phase is coated on the inner wall of the channel, or a layer of stationary phase is deposited on the inner wall of the channel by chemical synthesis. And a plurality of partition walls 201 are arranged in parallel therein, each partition wall 201 being configured to extend in a direction in which gas flows. Therefore, on the one hand, the effective width of the second chromatographic channel 20 can be reduced, and the depth-to-width ratio can be improved, and on the other hand, the surface area of the chromatographic channel can be greatly increased by arranging a plurality of parallel partition walls 201 in the chromatographic channel, and the area of the coating stationary phase can be further improved.
In a second embodiment, the gas chromatography column chip includes a main inlet 50, a main outlet 60, three mutually independent chromatography channels, two connecting channels, two solenoid valves 40 and two branch outlets 70. Three chromatography channels are arranged side by side on a substrate. The main inlet 50 and the main outlet 60 communicate with the outermost two chromatography channels, respectively, and the main outlet 60 is used to discharge gas flowing through the three chromatography channels when both solenoid valves 40 are open. Wherein each connecting channel is arranged between two adjacent chromatographic channels, and a corresponding solenoid valve 40 is arranged in the connecting channel. The two branch outlets 70 correspond to two chromatographic channels, respectively, and the branch outlets 70 are used for discharging gas from the corresponding branch outlets 70 of a connecting channel when the gas flows to the connecting channel in a closed state. Other features are the same as those in the first embodiment and will not be described herein.
In other embodiments, the micro gas chromatography column chip 1 includes a main inlet 50, a main outlet 60, at least four mutually independent chromatography channels, at least three connecting channels, at least three solenoid valves 40, and at least three branch outlets 70. The main inlet 50 and the main outlet 60 communicate with the outermost two chromatography channels, respectively, and the main outlet 60 is used to discharge gas flowing through at least four chromatography channels when all the solenoid valves 40 are open. At least four chromatographic channels are filled with stationary phases with different phase states. Each connecting channel is connected between two adjacent chromatographic channels and is used for communicating the two adjacent chromatographic channels. Each solenoid valve 40 is provided in one of the connection passages for opening or closing the connection passage to allow gas to flow through the two chromatographic passages communicating with the connection passage when the connection passage is opened. At least three branch outlets 70 respectively corresponding to the at least three connecting channels, each branch outlet 70 being communicated with the corresponding connecting channel for allowing the gas to be discharged from the branch outlet 70 corresponding to the connecting channel when the gas flows through to the connecting channel in a closed state. Other features are the same as those in the first embodiment and will not be described herein.
Particularly, the invention also provides a preparation method of the micro gas chromatographic column chip, which comprises the following steps:
s100, etching at least two mutually independent chromatographic channels on a substrate, etching a main inlet and a main outlet, and respectively communicating the main inlet and the main outlet with two outermost chromatographic channels;
s200, bonding and sealing a glass substrate for sealing with a chromatographic channel;
s300, respectively pumping the configured stationary phases with different phase states to at least two chromatographic channels so as to respectively fill the stationary phases with different phase states in the at least two chromatographic channels;
s400, communicating at least two chromatographic channels through at least one connecting channel, introducing inert gas into the communicated chromatographic channels, and then carrying out aging treatment.
In step S100, the substrate may be, for example, a stainless steel, silicon, copper, or glass substrate. The etching method may be, for example, a laser etching method, but is not limited thereto. There are various methods for obtaining at least two mutually independent chromatographic channels, such as Deep Reactive Ion Etching (DRIE) technology, LiGA technology based on electron beam lithography and PECVD method growth technology. The chromatographic channel prepared by the LiGA technology can improve the aspect ratio of the section of the micro-channel. The chromatographic channel prepared by the DRIE technology has high column efficiency. The long semicircular micro-channel is prepared on the chip by using a PECVD method, and the column efficiency is large. The chromatographic channel prepared by adopting the laser etching technology can be used for producing chromatographic column chips in batches and has low production cost.
And the length of the chromatographic channel is 0.2m-5m, preferably 3 m. The width of the chromatographic channel is 0.2mm to 1mm, preferably 0.5 mm. The depth of the chromatographic channel is 0.3mm to 1.0mm, preferably 0.6 mm. The length of the chromatographic channel determines the length of the gas running time and thus the level of the column pressure. The length, width and depth of the chromatographic channel are too small, the running time of gas in the chromatographic channel is short, the column pressure is low, the length, width and depth of the chromatographic channel are too large, the running time of gas in the chromatographic channel is too long, and the column pressure is too high.
In step S200, the substrate and the glass substrate are cleaned before bonding and sealing the glass substrate with the chromatography channel. When the substrate is a metal substrate such as a stainless steel substrate, after cleaning and drying, it is necessary to cover a soft gasket on the surface thereof and to press-seal it with another metal sheet with a screw.
Before step S300, it is further required to seal the main outlet and the first end of the chromatography channel communicated with the main outlet with a gas-guide tube respectively, and connect the gas-guide tube with the pump. The first end of the chromatographic channel is the end in communication with another adjacent chromatographic channel, which is labeled as the third chromatographic channel. It is also necessary to seal the main inlet and the second end of the chromatography channel communicating with the main inlet to a gas-conducting tube, and to connect the gas-conducting tube to the pump. The second end of the chromatographic channel is the end in communication with another adjacent chromatographic channel, which is labeled as the fourth chromatographic channel.
In step S300, the total outlet is immersed in the stationary phase solution, the stationary phase solution is pumped to the third chromatography channel, after the whole third chromatography channel is filled with the stationary phase solution, the air duct is closed, and the pump is made to slowly suck the solution in the stationary phase solution closed in the third chromatography channel, so as to leave an even stationary phase on the inner wall of the channel in the third chromatography channel. And then the main inlet is immersed in the stationary phase filler, the stationary phase filler is pumped into the fourth chromatographic channel, and the pump is closed after the whole fourth chromatographic channel is filled with the stationary phase filler.
In step S400, the inert gas may be, for example, nitrogen. And introducing nitrogen into the chromatographic channel, placing the chromatographic channel in an oven, gradually increasing the temperature, aging at 120 ℃ for 1h, aging at 220 ℃ for 4h, and then cooling to room temperature to finish aging.
In one embodiment, a heater may be integrated into the prepared chip of the column, or a commercial micro heater plate or rod may be used and connected to a temperature controller to heat the column to a constant temperature.
Thus, it should be appreciated by those skilled in the art that while a number of exemplary embodiments of the invention have been illustrated and described in detail herein, many other variations or modifications consistent with the principles of the invention may be directly determined or derived from the disclosure of the present invention without departing from the spirit and scope of the invention. Accordingly, the scope of the invention should be understood and interpreted to cover all such other variations or modifications.
Claims (8)
1. A micro gas chromatography column chip, comprising:
at least two mutually independent chromatographic channels etched on a substrate are filled with stationary phases with different phase states; the length of the chromatographic channel is 0.2-5 m, the width of the chromatographic channel is 0.2-1 mm, and the depth of the chromatographic channel is 0.3-1.0 mm;
at least one connecting channel, wherein each connecting channel is connected between two adjacent chromatographic channels and is used for communicating the two adjacent chromatographic channels; and
at least one solenoid valve, each solenoid valve is arranged in one of the connecting channels and is used for opening or closing the connecting channel, and when the connecting channel is opened, gas flows through the two chromatographic channels communicated with the connecting channel;
wherein at least two of the chromatographic channels comprise:
a first chromatographic channel filled with a solid stationary phase;
a second chromatography channel filled with a liquid or colloidal stationary phase;
a plurality of partition walls are arranged in parallel in the second chromatography passage, each of the partition walls being configured to extend in the direction in which the gas flows.
2. The micro gas chromatography column chip of claim 1, further comprising:
the main inlet is communicated with one of the chromatographic channels at the outermost side and is used for introducing gas into the chromatographic channel; and
a main outlet communicating with one of said chromatographic channels outermost at the other end for discharging said gas when said at least one connecting channel is open.
3. The micro gas chromatography column chip of claim 2, further comprising:
and the at least one branch outlet is respectively corresponding to the at least one connecting channel, and each branch outlet is communicated with the corresponding connecting channel and used for discharging the gas from the branch outlet corresponding to the connecting channel when the gas flows to the connecting channel in a closed state.
4. The micro gas chromatography column chip of claim 3, wherein a filter is disposed in the first chromatography channel at a position near the corresponding branch outlet for preventing loss of the stationary phase in the first chromatography channel.
5. The micro gas chromatography column chip of claim 1, wherein the material of the stationary phase filled in the first chromatography channel is selected from one or more of OV-1, OV-101, polydimethylsiloxane, carbon nanotube and graphene;
the stationary phase filled in the second chromatographic channel is one or a combination of more of polymer microspheres, carbon molecular sieves, graphene and carbon nanotubes.
6. The micro gas chromatography column chip of any of claims 1-5, wherein the chromatography channel is serpentine.
7. A preparation method of a micro gas chromatography column chip is characterized by comprising the following steps:
etching at least two mutually independent chromatographic channels on a substrate; the length of the chromatographic channel is 0.2-5 m, the width of the chromatographic channel is 0.2-1 mm, and the depth of the chromatographic channel is 0.3-1.0 mm;
bonding and sealing a glass substrate for sealing with the chromatographic channel;
respectively pumping the configured stationary phases with different phases to the at least two chromatographic channels, so that the stationary phases with different phases are respectively filled in the at least two chromatographic channels;
communicating the at least two chromatographic channels through at least one connecting channel, introducing inert gas into the communicated chromatographic channels, and then carrying out aging treatment;
wherein at least two of the chromatographic channels comprise:
a first chromatographic channel filled with a solid stationary phase;
a second chromatography channel filled with a liquid or colloidal stationary phase;
a plurality of partitions are arranged in parallel in the second chromatography passage, each of the partitions being configured to extend in a direction in which the gas flows.
8. A method according to claim 7, wherein after etching at least two mutually independent chromatographic channels on a substrate, further comprising the steps of:
etching a total inlet and a total outlet on the substrate, and enabling the total inlet and the total outlet to be respectively communicated with the two outermost chromatographic channels.
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| CN113804810A (en) * | 2020-06-15 | 2021-12-17 | 浙江科技学院 | Chromatographic separation column and method for detecting VOCs gas chromatography |
| CN111999422B (en) * | 2020-08-27 | 2022-01-25 | 电子科技大学 | Double-side heating flexible composite substrate micro chromatographic column and preparation method thereof |
| CN112255358A (en) * | 2020-09-20 | 2021-01-22 | 杭州谱育科技发展有限公司 | Multicomponent detecting system based on single column |
| CN113281424A (en) * | 2021-03-31 | 2021-08-20 | 天津大学 | Miniature chromatographic column, coating method thereof and miniature gas chromatograph |
| CN113567600B (en) * | 2021-07-22 | 2023-06-27 | 中国科学院空天信息创新研究院 | Multi-channel miniature gas chromatographic column chip and preparation method thereof |
| CN114019038B (en) * | 2021-10-09 | 2024-01-02 | 长鑫存储技术有限公司 | Device and method for monitoring organic matters in environmental gas |
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