CN102297800A - Microchannel membrane sample introduction device - Google Patents
Microchannel membrane sample introduction device Download PDFInfo
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- CN102297800A CN102297800A CN2011102059487A CN201110205948A CN102297800A CN 102297800 A CN102297800 A CN 102297800A CN 2011102059487 A CN2011102059487 A CN 2011102059487A CN 201110205948 A CN201110205948 A CN 201110205948A CN 102297800 A CN102297800 A CN 102297800A
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Abstract
A microchannel membrane sample introduction device relates to a sample introduction device of a sample analysis apparatus. A microchannel membrane sample introduction device is provided which is mainly used with a sample analysis apparatus, is applicable to sample introduction of gaseous or liquid samples, can ensure the strength of the membrane sample introduction device, can greatly increase the actual working surface area of the membrane, and can increase the separation and concentration efficiency of the membrane. The device is provided with a microchannel membrane, a substrate, a supporting sheet, two sample-introducing pipes, and a sampling pipe; a double-helix groove is disposed on a surface of the microchannel membrane; the surface of the microchannel membrane is covered by the substrate; a double-helix channel is formed between the microchannel membrane and the substrate; two ends of one of the helical channel in the double-helix channel are respectively communicated with one end of the two sample-introducing pipes; the helical channel is a sample-introducing channel; both the two sample-introducing pipes extends out of the substrate; the bottom surface of the microchannel membrane is covered by the supporting sheet; the other helical channel in the double-helix channel is communicated with the sampling pipe; the helical channel is a sampling channel; the sampling pipe extends out of the supporting sheet.
Description
Technical field
The present invention relates to the sample feeding device of sample analysis instrument, especially relate to a kind of microchannel film sampling device that is mainly used in gaseous state or liquid biased sample.
Background technology
Common sample injection method for gas analysis is micropore sample introduction and capillary sample inlet.Because the diameter of micropore is generally all at tens～hundreds of micron, mechanical processing difficulty requires high.Though the structure of capillary sample inlet is simple relatively, can select the ready-made on the market different inner diameters and the kapillary of length as required.But these two kinds of sample injection methods all are to dilution of sample sample introduction (by volume) in fact, do not have pre-separation and inrichment at all, have therefore also limited the sensitivity of subsequent analysis instrument.
It is to occur in 20 beginnings of the century the earliest that film separates sampling technique, a special kind of skill of rapid stubborn after the sixties in 20th century.It is utilize a special manufacturing, have and select diactinic film, in the pressure differential of film both sides as under the powered, the each component sample is owing to the infiltration rate to film there are differences in the potpourri, through behind the certain hour, the component sample that infiltration rate is big will obtain at the opposite side of film separating, purifies and concentrate.
The film sampling device is simple in structure, need not sample pre-treatments, not only has the dual-use function of pre-separation and enrichment simultaneously, and the response time of ultrathin membrane is also very short, can satisfy the needs that online express-analysis detects, and can directly dock with analytical instrument.Compare micropore (or slit) sample introduction and capillary sample inlet mode, the film sample introduction is the highest can to improve 2～3 orders of magnitude of sensitivity.
The transmission course of potpourri in film can be described by the FICK law:
In the formula (1):
I
SsThe infiltration rate (mol/s) of-testing sample in film;
Effective surface area (the cm of A-film
2);
D-coefficient of diffusion (cm
2/ s);
The thickness of L-film (cm);
Solubility coefficient (the mol/Pacm of S-sample in film
3);
P
sThe pressure of-membrane sample side (Pa).
From formula (1), can learn, after the material of film is selected, the infiltration rate of sample in film only with the effective surface area A of film and the pressure P of membrane sample side
sBe directly proportional, be inversely proportional to the thickness L of film.
In addition, the response time of film separation can be calculated by the FICK law:
Can learn that from formula (2) after the material of film was selected, the time of sample separation degree from 10% to 90% and the thickness L of film square were inversely proportional to.Therefore, when design film sampling device, should increase the separating area of film as far as possible, and reduce the area of film.
At present, the conventional film sampling device that docks with analytical instrument generally adopts diameter 2～5mm, and the polymeric membrane of thickness 10～100 μ m is a driving force with the pressure differential.The both sides of film are respectively sample pressure (equaling atmospheric pressure or malleation) and negative pressure of vacuum, and itself is not only separating component film, also will bear vacuum isolation function simultaneously.Therefore, just there are serious problems in this film sampling device: because the thickness of polymeric membrane is extremely thin, so its physical strength is very poor, and the real work surface area is severely limited, and has only the dozens of square millimeter, has influenced the separating effect of film; If want to increase the worksheet area, just must increase the thickness of polymeric membrane, sample analysis time is increased with quadratic relationship, reduce separation efficiency.
Chinese patent CN 2700877Y provides film sample introduction and the vacuum ultraviolet ionized device in a kind of portable mass spectrometer, and it is exactly the wafer-type film that film sampling device wherein adopts; Article (the Characterization of a sheet membrane interface for sample introduction into a time-of-flight mass spectrometer that delivers at Kwon-Sik Oh, International Journal of Mass Spectrometry 253 (2006) 65-70), introduction also is to adopt conventional wafer-type film.This normal film sampling device generally adopt the disk shape, diameter 2～5mm, the polymeric membrane of thickness 10～100 μ m is a driving force with the pressure differential.The both sides of film are respectively sample pressure (equaling atmospheric pressure or malleation) and negative pressure of vacuum, and itself is not only separating component film, also will bear vacuum isolation function simultaneously.Therefore, just there are serious problems in this wafer-type film sampling device: because the thickness of polymeric membrane is extremely thin, so its physical strength is very poor, and the real work surface area is severely limited, and has only the dozens of square millimeter, has influenced the separating effect of film; If want to increase the worksheet area, just must increase the thickness of polymeric membrane, sample analysis time is increased with quadratic relationship, reduce separation efficiency.
Summary of the invention
The purpose of this invention is to provide a kind of main and sample analysis instrument adapted, be suitable for gaseous state or liquid sample sample introduction, can guarantee the intensity of film sampling device, can significantly improve the real work surface area of film, improve the separation of film and the microchannel film sampling device of bioaccumulation efficiency.
The present invention is provided with microchannel film, substrate, supporting spring, 2 samples introducing conduits and 1 sample conduit;
Film surface, microchannel is provided with the double helix groove, substrate is covered in film surface, microchannel, form the double helix passage between microchannel film and the substrate, the two ends of wherein 1 helical duct in the double helix passage are introduced conduit one end with 2 samples respectively and are communicated with, this helical duct is a sample intake passage, 2 samples are introduced conduit and are all exposed substrate, supporting spring is covered in film bottom surface, microchannel, 1 helical duct in addition in the double helix passage is communicated with sample conduit one end, this helical duct is a sampling channel, and sample conduit is exposed supporting spring.
Described microchannel film can be the high molecular polymerization film, as teflon, cellulose, dimethyl silicone polymer and tygon etc.
Described substrate can be sheet metal substrate, glass sheet substrate or silicon chip substrate, and substrate thickness can be 1～2mm;
Arrange 2 helical duct spaces in the described double helix passage, and phase differential can be 180 °.Article 2, the width of helical duct can be 50～200 μ m, and channel wall thickness can be 10～100 μ m.Article 2, the shape of the little shape passage of double helix can be rectangle or other shape.
Described supporting spring can be sheet metal supporting spring, glass sheet supporting spring or silicon chip supporting spring, and supporting spring thickness can be 1～2mm.
Described sample is introduced conduit and sample conduit can be metal tube or nonmetallic pipe; The bore that sample is introduced conduit and sample conduit can be 200～500 μ m, and pipe thickness can be 1mm.
Principle of work of the present invention is as follows:
When sample flow during through sample intake passage, with the thin layer conduit wall between the little shape passage of double helix as diffusion barrier, according to different component samples seeing through of film had optionally principle, they will be according to different transmitances from sample intake passage, be penetrated in the sampling channel by thin-walled, thereby obtain the sample component after pre-separation and the enrichment, be drawn out in the analytical instrument of subordinate by sample conduit at last.
Compare with existing film sampling device, the present invention has following outstanding advantage:
Adopt the little shape channel membrane of double helix structure, as diffusion barrier, solved the strength problem of conventional film sampling device preferably with the thin layer conduit wall between the little shape passage of double helix.Can significantly improve the real work surface area of film, improve the separation and the bioaccumulation efficiency of film.Can directly carry out pre-separation and enrichment, after analysis instruments such as mass spectrometer, chromatograph and spectrometer dock coupling, can significantly improve the detection sensitivity (can improve 100～1000 times) of these analytical instrument the volatile matter in gas or the liquid mixing sample.Effect is very remarkable.
Description of drawings
Fig. 1 is the structural representation of the embodiment of the invention 1.
Fig. 2 is the microchannel film schematic surface of the embodiment of the invention 1.
Embodiment
The invention will be further described below in conjunction with drawings and Examples.
Referring to Fig. 1 and 2, the present invention is provided with microchannel film 3, substrate 2,4,2 samples introducing conduits 1 of supporting spring and sample conduit 5.
Described microchannel film 3 is the high molecular polymerization film, adopts teflon high molecular polymerization film (also can adopt high molecular polymerization films such as cellulose, dimethyl silicone polymer and tygon).
Described substrate 2 is sheet metal substrate (also can be glass sheet substrate or silicon chip substrate), and substrate 2 thickness are that 1.5mm (can preferred 1～2mm).
Arrange 2 helical ducts 31 in the described double helix passage and 32 spaces, and phase differential is 180 °.Article 2, helical duct 31 and 32 width are 100 μ m (can preferred 50～200 μ m), and 2 helical ducts 31 and 32 wall thickness are 50 μ m (can preferred 10～100 μ m).Article 2, little shape passage 31 of double helix and 32 shape are rectangle (also can be other shape).
Described supporting spring 4 is sheet metal supporting spring (also can be glass sheet supporting spring or silicon chip supporting spring), and supporting spring thickness is that 1.5mm (can preferred 1～2mm).
Conduit 1 introduced by described 2 samples and sample conduit 5 is metal tube (also can be nonmetallic pipe).The bore that 2 samples are introduced conduit 1 and sample conduit 5 is 300 μ m (can preferred 200～500 μ m), and pipe thickness is 1mm.
The manufacturing process of little shape channel membrane 3 is as follows: earlier with photoetching or wet carving method silicon chip surface is formed the raceway groove of double helix shape, the width range of raceway groove is at 10～100 μ m, and the raceway groove wall thickness range is at 0.1～0.5mm; Then with this silicon chip as anode membrane, at its surperficial centrifugal spraying one deck teflon high molecular polymerization film, thickness is at 1～2mm; Next again the silicon chip anode membrane is eroded; At last that remaining teflon high molecular polymerization film and substrate is bonding, so just formed a kind of double helix passage, channel width 0.1～0.5mm, channel wall thickness 10～100 μ m.One of them passage is a sample feeding passage 31, and another passage is a sampling channel 32.Sample intake passage 31 two ends have small sircle hole 311 and 312,2 samples introduce conduit 1 respectively with 2 small sircle holes 311 and 312 bonding connections; The sealing of sampling channel 32 1 ends, the other end has small sircle hole 321 equally, and sample conduit 5 is bonding with it, sample conduit 5 and analytical instrument butt joint.This little shape channel membrane 3 not only can adopt wet etching to make, and also can process for example laser or particle beams processing with other micro-processing method.The course of work of microchannel film sampling device is: when gaseous state or liquid biased sample are flowed through after sample introduces conduit 1 and enter sample intake passage 31, because different component samples have selectivity to seeing through of film, they will be penetrated in the sampling channel 32 by the thin-walled between two passages with different transmitances, thereby obtain the sample component after pre-separation and the enrichment, these components detect through the analytical instrument that sample conduit 5 enters into the back at last.
The actual effectively separating area A of microchannel film 3 can calculate with following formula:
A＝h(d+np)(n-1)π (3)
In the formula (3): the height of h---conduit wall;
D---helix base circle diameter (BCD);
P---helix base circle diameter (BCD);
N---all numbers.
From taking all factors into consideration, the film parameter tentatively is decided to be: h=0.1mm, d=1mm, p=0.15mm, n=53.Therefore the actual effectively separating area of film can reach 146mm
2, and conventional 50 μ m are thick, the membrane area of diameter 5mm is less than 20mm
2, can improve more than 7 times.
Claims (8)
1. a microchannel film sampling device is characterized in that being provided with microchannel film, substrate, supporting spring, sample introducing conduit, sample extraction catheter and sample conduit;
Film surface, microchannel is provided with the double helix groove, substrate is covered in film surface, microchannel, form the double helix passage between microchannel film and the substrate, the two ends of wherein 1 helical duct in the double helix passage introduce conduit one end with sample respectively and sample extraction catheter one end is communicated with, this helical duct is a sample intake passage, sample is introduced conduit and the sample extraction catheter all exposes substrate, supporting spring is covered in film bottom surface, microchannel, wherein other 1 helical duct in the double helix passage is communicated with sample conduit one end, this helical duct is a sampling channel, and sample conduit is exposed supporting spring.
2. a kind of microchannel as claimed in claim 1 film sampling device is characterized in that described microchannel film is the high molecular polymerization film.
3. a kind of microchannel as claimed in claim 2 film sampling device is characterized in that described high molecular polymerization film is teflon high molecular polymerization film, cellulose high molecular polymerization film, dimethyl silicone polymer high molecular polymerization film or vinyl polymer polymeric membrane.
4. a kind of microchannel as claimed in claim 1 film sampling device is characterized in that described substrate is sheet metal substrate, glass sheet substrate or silicon chip substrate, and substrate thickness is 1～2mm.
5. a kind of microchannel as claimed in claim 1 film sampling device is characterized in that 2 helical duct spaces in the described double helix passage are arranged, and phase differential is 180 °.
6. as claim 1 or 5 described a kind of microchannel film sampling devices, it is characterized in that the width of 2 helical ducts is 50～200 μ m, the wall thickness of 2 helical ducts is 10～100 μ m, and the shape of 2 little shape passages of double helix is rectangle.
7. a kind of microchannel as claimed in claim 1 film sampling device is characterized in that described supporting spring is sheet metal supporting spring, glass sheet supporting spring or silicon chip supporting spring, and supporting spring thickness is 1～2mm.
8. a kind of microchannel as claimed in claim 1 film sampling device is characterized in that described sample introducing conduit, sample extraction catheter and sample conduit are metal tube; The bore that sample is introduced conduit, sample extraction catheter and sample conduit is 200～500 μ m, and pipe thickness is 1mm.
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| CN2011102059487A CN102297800A (en) | 2011-07-21 | 2011-07-21 | Microchannel membrane sample introduction device |
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|---|---|---|---|
| CN2011102059487A CN102297800A (en) | 2011-07-21 | 2011-07-21 | Microchannel membrane sample introduction device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104716005A (en) * | 2013-12-15 | 2015-06-17 | 中国科学院大连化学物理研究所 | Sample feeding device for spiral pipe-shaped film in ionization source |
| CN113926402A (en) * | 2020-06-29 | 2022-01-14 | 中国石油化工股份有限公司 | Micro-channel reactor and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20030211629A1 (en) * | 1996-09-13 | 2003-11-13 | James Baumgardner | Membrane countercurrent exchanger and membrane inlet mass spectrometer for the analysis of gas partial pressure in liquid samples |
| CN202166564U (en) * | 2011-07-21 | 2012-03-14 | 厦门大学 | Microchannel membrane sampling device |
-
2011
- 2011-07-21 CN CN2011102059487A patent/CN102297800A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20030211629A1 (en) * | 1996-09-13 | 2003-11-13 | James Baumgardner | Membrane countercurrent exchanger and membrane inlet mass spectrometer for the analysis of gas partial pressure in liquid samples |
| CN202166564U (en) * | 2011-07-21 | 2012-03-14 | 厦门大学 | Microchannel membrane sampling device |
Non-Patent Citations (4)
| Title |
|---|
| DANIEL T. CHIU 等: "Patterned deposition of cells and proteins onto surfaces by using three-dimensional microfluidic systems", 《PROCEEDINGS OF THE NATIONAL ACADEMY OF SCIENCES》 * |
| JAMES E. BAUMGARDNER 等: "Countercurrent Extraction of Sparingly Soluble Gases for Membrane Introduction Mass Spectrometry", 《ANNALS OF BIOMEDICAL ENGINEERING》 * |
| JEONGGI SEO 等: "Membrane-free microfiltration by asymmetric inertial migration", 《APPLIED PHYSICS LETTERS》 * |
| POOJA RAMESH: "《Graduate Theses and Dissertations》", 1 January 2010 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104716005A (en) * | 2013-12-15 | 2015-06-17 | 中国科学院大连化学物理研究所 | Sample feeding device for spiral pipe-shaped film in ionization source |
| CN104716005B (en) * | 2013-12-15 | 2017-01-25 | 中国科学院大连化学物理研究所 | Sample feeding device for spiral pipe-shaped film in ionization source |
| CN113926402A (en) * | 2020-06-29 | 2022-01-14 | 中国石油化工股份有限公司 | Micro-channel reactor and application thereof |
| CN113926402B (en) * | 2020-06-29 | 2023-04-07 | 中国石油化工股份有限公司 | Micro-channel reactor and application thereof |
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Application publication date: 20111228 |