CN104880520B - Filled type gas chromatographic column and preparation method thereof - Google Patents
Filled type gas chromatographic column and preparation method thereof Download PDFInfo
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- CN104880520B CN104880520B CN201510082100.8A CN201510082100A CN104880520B CN 104880520 B CN104880520 B CN 104880520B CN 201510082100 A CN201510082100 A CN 201510082100A CN 104880520 B CN104880520 B CN 104880520B
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Abstract
The invention provides a kind of filled type gas chromatographic column.The filled type gas chromatographic column includes:First substrate, has micro-channel in its Surface Machining;Second substrate, there is micro-channel in its Surface Machining, the micro-channel is mutually corresponding with the position of the micro-channel on first substrate surface, and after the first substrate and the second substrate be combined with each other sealing, the micro-channel in micro-channel and the second substrate in the first substrate collectively forms the micro- raceway groove of chromatographic column;And chromatograph packing material, it is filled in the micro- raceway groove of the chromatographic column.The present invention is mutually bonded by two kinds of substrates and formed, and the micro- raceway groove of chromatographic column is formed by the micro-channel of surface both, breaches the limitation of corresponding size, and length is longer, and reliability is higher.Based on this, present invention also offers a kind of preparation method of above-mentioned filled type gas chromatographic column.
Description
Technical field
The present invention relates to chromatogram detection technique field, more particularly to a kind of filled type gas chromatographic column and preparation method thereof.
Background technology
It is many for environmental air quality monitoring, intelligent grid and oil exploration in environmental air quality monitoring, equipment etc.
(mainly there are CO, CO in field to contaminated air2、NO2、SO2、H2Low-carbon (LC) hydrocarbon compound such as S, C1~C6 etc.) rapidly and efficiently separate
The active demand of detection, prior art needs miniature gas chromatographic column badly to realize to low carbon compound and permanent gases
Rapidly and efficiently separate.
And at present to CO, CO2、SO2、NO2、H2In the isolation technics and method of the low-carbon (LC) hydrocarbon compound such as S, C1~C6, greatly
Traditional capillary chromatograph and packed column are all used, these traditional chromatographic columns are big due to its volume, and the power consumption of temperature control is high, do not apply to
In field monitoring field.Therefore, it is badly in need of a kind of small volume of invention, temperature control miniaturization gas chromatographic column low in energy consumption substitutes tradition
Capillary chromatograph and packed column.And it is existing be applied to the low-carbon (LC) such as CO, CO2, SO2, H2S, C1~C6 hydrocarbon compound separation
Miniaturization gas-chromatography column technology is very limited.
A kind of micro-scale gas chromatograph post is provided in bibliography 1, as shown in Figure 1.In the raceway groove of the micro-compliant mechanism,
The Minisize pillar of array is set, the effective surface area of chromatographic column raceway groove is increased with this, improve the coated weight of fixing phase, finally
Reach the ability for improving resolution.
But, there is certain defect in above-mentioned micro-scale gas chromatograph post.First, designing the side of Minisize pillar in raceway groove
Method, can no doubt increase the surface area of raceway groove, but also limit the depth of raceway groove, from the graph it can be found that due to process technology
Limitation, chromatogram channel depth is bigger, and the diameter of its Minisize pillar becomes increasingly thinner, when raceway groove reaches 200 microns, has approached
The limit that column is present, then it is deep, column is just easy to fracture;Second, fixing phase film (Al2O3) it is by atomic deposition technique
Fixing phase is coated in raceway groove and leg surface, the thickness of fixing phase film is very limited, only 10nm, much smaller than traditional
The scope of 200nm-20000nm, strongly limit sample capacity, it is difficult to be applicable the separation of complex mixture;Third, passing through atom
The technology coating fixing phase of deposition, paintable stationary phase material species is very limited, this strongly limits it wider
Apply in field.
Bibliography:
1、Hamza Shakeel,Gary W.Rice,Masoud Agah,Semipacked columns with
atomic layer deposited alumina as a stationary phase,Sensors and Actuators B:
Chemical,2014
The content of the invention
(1) technical problem to be solved
In view of above-mentioned technical problem, the invention provides a kind of filled type gas chromatographic column and preparation method thereof, to improve
The sample capacity that can be detected, widens application field.
(2) technical scheme
According to an aspect of the invention, there is provided a kind of filled type gas chromatographic column.The filled type gas chromatographic column bag
Include:First substrate, has micro-channel in its Surface Machining;Second substrate, has micro-channel in its Surface Machining, the micro-channel and first
The position of the micro-channel on substrate surface mutually corresponds to, after the first substrate and the second substrate be combined with each other sealing, the first substrate
On micro-channel and the second substrate on micro-channel collectively form the micro- raceway groove of chromatographic column;And chromatograph packing material, it is filled in chromatographic column
In micro- raceway groove.
According to another aspect of the present invention, a kind of preparation method of above-mentioned filled type gas chromatographic column is additionally provided.Should
Preparation method includes:Step A:Shape and position mutually corresponding micro-channel are formed in the first substrate and the second substrate;Step
C:The side that first substrate and the second substrate are had into micro-channel relatively, carries out bonded seal, and both micro-channels are collectively formed
The micro- raceway groove of chromatographic column;Step D:The packing chromatography filler in the micro- raceway groove of chromatographic column;And step E:To in the micro- raceway groove of chromatographic column
Chromatograph packing material carry out it is aging, so as to prepare filled type gas chromatographic column.
(3) beneficial effect
From above-mentioned technical proposal as can be seen that filled type gas chromatographic column of the present invention and preparation method thereof is with following beneficial
Effect:
(1) it is mutually bonded by two kinds of substrates and is formed, the micro- raceway groove of chromatographic column is formed by the micro-channel of surface both, breaches phase
The limitation of size is answered, longer, more reliable filled type gas chromatographic column can be prepared;
(2) the packing chromatography filler in the micro- raceway groove of chromatographic column, rather than in the way of fixing phase film, greatly improving to fill out
The quantity of chromatograph packing material is filled, so as to increase sample capacity, can be used for the separation of complex mixture;
(3) chromatograph packing material can be the chromatogram of the various characteristics such as CNT, carbon molecular sieve, 5A, Al2O3, Porapak-Q
Filler, greatly improves the range of application of chromatographic system;
(4) bottom of substrate is integrated with microheater one of wherein, micro-compliant mechanism is possessed quick liter in itself
Warm ability, greatly reduces system bulk.
Brief description of the drawings
Fig. 1 is the vertical section schematic diagram of the micro-scale gas chromatograph post of offer in bibliography 1;
Fig. 2A is the vertical section schematic diagram according to embodiment of the present invention filled type gas chromatographic column;
Fig. 2 B are schematic diagram of the filled type gas chromatographic column shown in Fig. 2A along A-A directions cross section;
Fig. 3 is the schematic diagram after packing chromatography filler in micro- raceway groove in filled type gas chromatographic column in Fig. 2A and Fig. 2 B;
Fig. 4 is the schematic diagram of the microheater of filled type gas chromatographic column silicon substrate bottom back side shown in Fig. 2A;
Fig. 5 is the flow chart of the preparation method according to embodiment of the present invention filled type gas chromatographic column.
【Main element】
1- gas accesses;2- gas vents
3- microfilters;The micro- raceway groove of 4- chromatographic columns
5- chromatograph packing materials;6- microheaters
7- substrate of glass.
Specific embodiment
To make the object, technical solutions and advantages of the present invention become more apparent, below in conjunction with specific embodiment, and reference
Accompanying drawing, the present invention is described in more detail.It should be noted that in accompanying drawing or specification description, similar or identical portion
Divide and all use identical figure number.The implementation for not illustrated in accompanying drawing or being described, is those of ordinary skill in art
Known form.In addition, though the demonstration of the parameter comprising particular value can be provided herein, it is to be understood that parameter is without definite etc.
In corresponding value, but corresponding value can be similar in acceptable error margin or design constraint.Mentioned in embodiment
Direction term, for example " on ", D score, "front", "rear", "left", "right" etc., be only the direction of refer to the attached drawing.Therefore, the side for using
It is for illustrating not for limiting the scope of the invention to term.
For application in the urgent need to the present invention proposes a kind of large sample capacity, low-power consumption, the gas phase of miniaturization filled type
Chromatographic column, and there is provided the preparation method of the gas chromatographic column.
In one exemplary embodiment of the present invention, there is provided a kind of filled type gas chromatographic column.Fig. 2A is according to this
The vertical section schematic diagram of inventive embodiments filled type gas chromatographic column.Fig. 2 B are filled type gas chromatographic column shown in Fig. 2A along A-A
The schematic diagram in direction cross section.After Fig. 3 is for packing chromatography filler in micro- raceway groove in filled type gas chromatographic column in Fig. 2A and Fig. 2 B
Schematic diagram.It should be noted that for the sake of clarity, in the raceway groove of the filled type gas chromatographic column in Fig. 2A and Fig. 2 B not
There is addition chromatograph packing material.
Refer to Fig. 2A, Fig. 2 B and Fig. 3, the present embodiment filled type gas chromatographic column includes:Substrate of glass, on its surface
It is machined with micro-channel;Silicon base, micro-channel is equally machined with its surface, the position of the micro-channel in the micro-channel and substrate of glass
Mutually correspondence is put, it is micro- in the micro-channel and silicon base in substrate of glass after substrate of glass and silicon base be combined with each other sealing
Conduit collectively forms the micro- raceway groove 4 of chromatographic column;Chromatograph packing material 5, is filled in the micro- raceway groove of the chromatographic column.
Each part to the present embodiment filled type gas chromatographic column is described in detail individually below.
In the present embodiment, make filled type gas chromatographic column using substrate of glass and silicon base, but the present invention not with
This is limited.In the present invention, other materials, such as quartz substrate, aluminium substrate, copper-based bottom, ceramic bases, plastics base can also be used
Bottom prepares filled type gas chromatographic column, or, while using two pieces of same substrates micro- raceway groove is processed, with reference to structure after sealing
The filled type gas chromatographic column of cost implementation.
Fig. 2A and Fig. 3 is refer to, the micro-channel in substrate of glass and silicon base is serpentine-like, both use bonding pattern reality
In conjunction with sealing.The micro-channel in micro-channel and silicon base in substrate of glass collectively forms the micro- raceway groove 4 of chromatographic column.Preferably,
The circular in cross-section of the micro- raceway groove 4 of the chromatographic column, ellipse, trapezoidal, taper or rectangle.
The physical dimension of the micro- raceway groove 4 of chromatographic column must is fulfilled for certain condition, particularly its width and depth must >=2
~3 times of single chromatograph packing material particle diameter.Wherein, in silicon base and substrate of glass micro-channel depth 0.3mm-0.5mm, it is excellent
Select 0.4mm;Width is 0.4mm-1mm, preferably 0.8mm.After substrate and sealing, the total depth of the micro- raceway groove of chromatographic column is 0.5mm-
1mm, preferably 0.8mm.The raceway groove total length of the micro- raceway groove 4 of chromatographic column is 0.5m-4m, preferably 2m.
For the above-mentioned micro- raceway groove 4 of chromatographic column, it has gas access 1, gas vent 2.Also, in gas vent 2
Position, is to prevent chromatograph packing material from being run out from gas vent 2 with microfilter 3, causes the loss of chromatograph packing material.Wherein,
Chromatograph packing material can be CNT, carbon molecular sieve, 5A (a kind of title of chromatograph packing material), Al2O3, the filler such as Porapak-Q.
The back side of micro-channel is not etched in silicon base, microheater 6 is integrated with.Fig. 4 is filled type gas phase shown in Fig. 2A
The schematic diagram of the microheater of chromatographic column silicon substrate bottom back side.Wherein, the resistance value of microheater is in 5-50 Ω, preferred value 8
Ω.The material of microheater can be Pt, nichrome, tungsten or other metal materials.
It should be noted that the shape of the microheater can be determined by technical staff according to factors such as power, areas,
It is not limited to the microheater pattern shown in Fig. 4.
For the filled type gas chromatographic column of the present embodiment, its operation principle is:Mixed gas to be separated, with carrier gas one
Rise and enter chromatographic column from gas access 1, each component of mixed gas is first filled in fixing phase or color in the micro- raceway groove of chromatographic column
Spectrum filling adsorption, is then desorbed, but absorption due to each component is with to be desorbed the used time different so that each component is from gas in gaseous mixture
Body 2 time out of outlet is also different, it is achieved thereby that the separation of mixed gas.
In another embodiment of the present invention, a kind of preparation method of above-mentioned filled type gas chromatographic column is additionally provided.
Fig. 5 is the flow chart of the preparation method according to embodiment of the present invention filled type gas chromatographic column.As shown in figure 5, the present embodiment is filled out
The preparation method for filling formula gas chromatographic column includes:
Step A:Shape in silicon base and substrate of glass is formed by the method for laser ablation and position is mutually corresponding
Micro-channel;
Wherein, in addition to laser ablation, above-mentioned microflute can also be formed using other methods such as chemical attack, deep etchings
Road.The shape and size of the micro-channel are as previously shown.
Step B:Microheater 6 is formed at the back side of silicon base;
Specifically, in the bottom of silicon base, one layer of Pt is deposited, then using techniques such as photoetching-metal deposit-strippings,
Microheater is produced, as shown in Figure 4.
Step C:The side that silicon base and substrate of glass are had into micro-channel relatively, carries out bonded seal, both microflutes
Road collectively forms the micro- raceway groove 4 of chromatographic column;
Cleaning silicon base and substrate of glass, and be baked to, then by the micro-channel in silicon base and substrate of glass
Micro-channel bonded seal, you can obtain filled type gas chromatographic column chip as shown in Figure 2 A and 2 B.
Step D:The packing chromatography filler 5 in the micro- raceway groove 4 of chromatographic column;
In this step, the gas vent 2 of the micro- raceway groove of chromatographic column is connected encapsulation with one end of wireway first, wireway
The other end is connected with pump;Then the gas access 1 of the micro- raceway groove of chromatographic column is immersed in chromatograph packing material;Open pump, chromatograph packing material
Under the suction of pump, into the micro- raceway groove of chromatographic column and it is sequentially filled in the micro- raceway groove 4 of chromatographic column, treats the micro- ditch of whole chromatographic column
After road is filled up by chromatograph packing material, pump is closed, you can be filled with the miniaturization filled type gas-chromatography of filler as shown in Figure 3
Post chip.
Step E:Chromatograph packing material 5 in the micro- raceway groove of chromatographic column is carried out it is aging, so as to be made filled type gas chromatographic column.
In this step, the gas access 1 of the micro- raceway groove of chromatographic column is connected encapsulation with wireway, is passed through to the micro- raceway groove of chromatographic column
N2;Filled type gas chromatographic column is placed in baking oven, temperature is stepped up, and it is aging one hour at 120 DEG C respectively, and 220 DEG C are old
Change 4 hours, temperature is then cooled to room temperature again, complete the aging of chromatograph packing material, can bring carries out separation test immediately.Its
In, the N being passed through in advance2Effect be protect the micro- raceway groove of chromatographic column in chromatograph packing material it is not oxidized, wherein N2Can be with indifferent gas
Body replaces.Also, above-mentioned aging temperature can be adjusted as needed, generally, chromatograph packing material is carried out always
Being divided into two stages is carried out, and in first stage, between 80-120 DEG C, the time is between 0.5~2 hour for temperature;
In second stage, between 180-280 DEG C, the time is between 0.5~2 hour for temperature.Those skilled in the art can basis
Above range combination actual scene selects aging temperature and time.
So far, combined accompanying drawing has been described in detail to two embodiments of the invention.According to above description, this area
Technical staff should have to filled type gas chromatographic column of the present invention and preparation method thereof and clearly recognize.
Additionally, the above-mentioned definition to each element and method is not limited in embodiment various concrete structures, the shape mentioned
Shape or mode, those of ordinary skill in the art can simply be changed or be replaced to it, for example:Needs are separated according to gas,
Can be with the different chromatograph packing material of subsection filling in the micro- raceway groove of chromatographic column, two kinds or more, different chromatograph packing materials can also be pressed
After ratio mixing, refill in the micro- raceway groove of chromatographic column;Or it is not provided with microheater or in silicon base and substrate of glass
The back side forms microheater simultaneously.
In sum, the present invention is mutually bonded by two kinds of substrates and formed, and it is micro- to form chromatographic column by the micro-channel of surface both
Raceway groove, breaches the limitation of corresponding size, can prepare longer, more reliable filled type gas chromatographic column.Meanwhile, in chromatographic column
Packing chromatography filler in micro- raceway groove, not only improve can packing chromatography filler quantity, also, be applicable the species of chromatograph packing material
There is great extension.Filled type gas chromatographic column of the invention can be widely applied to environmental air quality monitoring, equipment inner ring
Border air quality monitoring, intelligent grid and oil exploration etc. are multi-field, with application value higher.
Particular embodiments described above, has been carried out further in detail to the purpose of the present invention, technical scheme and beneficial effect
Describe in detail bright, should be understood that and the foregoing is only specific embodiment of the invention, be not intended to limit the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution and improvements done etc., should be included in guarantor of the invention
Within the scope of shield.
Claims (8)
1. a kind of filled type gas chromatographic column, it is characterised in that including:
First substrate, has micro-channel in its Surface Machining;
Second substrate, has micro-channel in its Surface Machining, the position of the micro-channel on the micro-channel and first substrate surface
It is mutually corresponding, after the first substrate and the second substrate be combined with each other sealing, in the micro-channel and the second substrate in the first substrate
Micro-channel collectively forms the micro- raceway groove of chromatographic column (4);And
Chromatograph packing material (5), is filled in the micro- raceway groove of the chromatographic column (4), the chromatograph packing material (5) be one kind in following material or
It is various:CNT, carbon molecular sieve, 5A, Al2O3、Porapak-Q;
Wherein, the end of the micro- raceway groove of the chromatographic column (4) is gas vent (2);The filled type gas chromatographic column also includes:It is micro-
Type filter (3), is arranged at the position of the gas vent (2) of the micro- raceway groove of the chromatographic column, for preventing the chromatograph packing material (5)
The outflow from the micro- raceway groove of chromatographic column (4);The length of the micro- raceway groove of chromatographic column (4) between 0.5m-4m, depth between
Between 0.5mm-1mm, width is between 0.4mm-1mm;
Wherein, first substrate is substrate of glass, and second substrate is silicon base.
2. filled type gas chromatographic column according to claim 1, it is characterised in that:
Micro-channel in first substrate and the second substrate is snakelike;
The circular in cross-section of the micro- raceway groove of chromatographic column (4), ellipse, trapezoidal, taper or rectangle.
3. filled type gas chromatographic column according to claim 1, it is characterised in that the width of the micro- raceway groove of chromatographic column (4)
The single chromatograph packing material particle diameter of degree and depth more than or equal to 2~3 times.
4. filled type gas chromatographic column according to claim 1, it is characterised in that also include:
Microheater (6), is formed at first substrate and/or the second substrate does not etch the back side of micro-channel, for checking colors
Chromatograph packing material (5) in the spectrum micro- raceway groove of post is heated.
5. filled type gas chromatographic column according to claim 4, it is characterised in that the microheater (6) is plane
Heater, between 5-50 Ω, its material is Pt, nichrome or tungsten to its resistance.
6. the preparation method of filled type gas chromatographic column any one of a kind of claim 1 to 5, it is characterised in that including:
Step A:Shape and position mutually corresponding micro-channel are formed in the first substrate and the second substrate;
Step B:Microheater (6) is formed at the back side of silicon base;
Step C:The side that first substrate and the second substrate are had into micro-channel relatively, carries out bonded seal, and both is micro-
Conduit collectively forms the micro- raceway groove of chromatographic column (4);
Step D:In the interior packing chromatography filler (5) of the micro- raceway groove of the chromatographic column (4);And
Step E:Chromatograph packing material (5) in the micro- raceway groove of chromatographic column is carried out it is aging, so as to prepare filled type gas chromatographic column.
7. preparation method according to claim 6, it is characterised in that the step D includes:
The gas vent (2) of the micro- raceway groove of chromatographic column is connected encapsulation with one end of wireway, the other end of wireway is connected with pump;
The gas access (1) of the micro- raceway groove of chromatographic column is immersed in chromatograph packing material;
Pump is opened, chromatograph packing material into the micro- raceway groove of chromatographic column and is sequentially filled in the micro- raceway groove of chromatographic column under the suction of pump
(4) in;And
After treating that the micro- raceway groove of whole chromatographic column (4) is filled up by chromatograph packing material, pump is closed.
8. preparation method according to claim 6, it is characterised in that the step E includes:
The gas access (1) of the micro- raceway groove of chromatographic column is connected encapsulation with wireway, protective gas is passed through to the micro- raceway groove of chromatographic column;
Filled type gas chromatographic column is placed in baking oven, temperature is stepped up, and it is default in the first preset temperature and second respectively
At a temperature of burin-in process is carried out to chromatograph packing material;And
Temperature is cooled to room temperature, chromatograph packing material is aging in the completion micro- raceway groove of chromatographic column;
Wherein, the first preset temperature is between 80-120 DEG C;Second preset temperature is between 180-280 DEG C.
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CN105126387B (en) * | 2015-09-11 | 2017-01-25 | 电子科技大学 | Micro wavy gas chromatographic column and preparation method thereof |
CN108333283A (en) * | 2017-01-20 | 2018-07-27 | 中国科学院上海微***与信息技术研究所 | A kind of microfluidic chromatography column and preparation method thereof containing streamlined oval micro-pillar array |
CN107014666B (en) * | 2017-03-21 | 2019-06-11 | 西安交通大学 | A kind of micro gas enricher and preparation method thereof |
CN108254465B (en) * | 2018-01-16 | 2021-04-09 | 中国科学院电子学研究所 | Density distribution type micro chromatographic column chip and manufacturing method thereof |
CN108490104B (en) * | 2018-03-05 | 2020-10-30 | 苏州感闻环境科技有限公司 | Miniature gas chromatographic column chip and preparation method thereof |
CN109613150B (en) * | 2018-11-09 | 2021-05-28 | 兰州中科安泰分析科技有限责任公司 | PLOT-Al2O3Chromatographic column high-pressure dynamic method coating process |
CN111855877B (en) * | 2019-04-30 | 2024-05-24 | 中国科学院上海微***与信息技术研究所 | MEMS-based multi-stationary-phase miniature packed column structure and preparation method thereof |
CN111999408B (en) * | 2020-08-27 | 2022-02-08 | 电子科技大学 | Flexible micro chromatographic column with thin-layer metal lining and preparation method thereof |
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 |
CN116429957A (en) * | 2023-06-09 | 2023-07-14 | 精智未来(广州)智能科技有限公司 | Miniature gas chromatographic column chip and manufacturing process thereof |
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