CN1257762C - Preparation method of detection filter membrane used for bacteria and virus sampling in air - Google Patents
Preparation method of detection filter membrane used for bacteria and virus sampling in air Download PDFInfo
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- CN1257762C CN1257762C CN 200410025764 CN200410025764A CN1257762C CN 1257762 C CN1257762 C CN 1257762C CN 200410025764 CN200410025764 CN 200410025764 CN 200410025764 A CN200410025764 A CN 200410025764A CN 1257762 C CN1257762 C CN 1257762C
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- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 4
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
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- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
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- Measuring Or Testing Involving Enzymes Or Micro-Organisms (AREA)
Abstract
The present invention discloses a preparation method of a composite membrane used for sampling and detecting microorganisms in air. A support porous membrane is placed on a horizontal glass plate; the height of a membrane preparing knife is regulated; a knife frame moves at a speed of 5cm to 6cm per minute; thereby, membrane preparing liquor is uniformly distributed on a porous membrane for forming a composite membrane skin layer; the reaction temperature is 20 DEG C to 30 DEG C, the humidity is 20 to 50%, and the pressure is negative pressure lower than the atmospheric pressure; then, the heat treatment with 40 DEG C to 80 DEG C is carried out for 1 to 3 hours; simultaneously, the height of the membrane preparing knife is regulated for preparing the composite membrane with different pore diameters. Macromolecular substances in the composite membrane can keep the activity of trapped microorganisms in a certain extent. Compared with other filter membranes, the composite membrane can decrease the formation of filter cakes; compared with other filter membranes with the same pore diameter, the flux is obviously increased under the same detection condition. Simultaneously, used macromolecule coating solution has biological activity and is good for keeping the activity of the microorganisms in a certain extend, which causes that a sample actually displays an air condition; the present invention also keeps the microbial activity when the microorganisms are sampled, and reduces detection errors.
Description
Technical field
The present invention relates to a kind of preparation method who is used for air bacterium and viral sample detecting filter membrane.
Background technology
Utilizing filter membrane method to gather aerosol particle is the most general method of sampling of aerosol.So-called aerosol is meant that solid-state or liquid particulate is suspended in the dispersion in the gas medium.Just begin to gather microbial aerosol as far back as Pasteur in 1861 and Petri in 1888 by filter membrane.It is to collect the simple and inexpensive method of aerosol sample.
In recent years, sampling of aerosol is made in filter membrane method extensive use.Many materials are used to filter membrane material, and most important filter membrane material has fibrous filter and porous membrane type filter material.
Most of fibrous filters all are arranged in and the mobile perpendicular direction of air, and its porosity is 70～99%, and to 100 μ m, the most frequently used is lignose, glass fibre element and plastic optical fibre to the size range of fiber from sub-micron.
What most of porous filter materials were used is cellulose esters, sintering metal, polyvinyl chloride, polytetrafluoroethylene (PTFE) or other materials.
Aerosol often contains many dust, and bacterium even virus are those inhalable particles that are stained with bacterium and virus in the main component of atmosphere pollution, particularly air, very easily suck the lung chamber from respiratory tract, have a strong impact on human health.Therefore set up aerocolloidal sampling and detection system, detect air quality timely and effectively and be of great significance.The normal both at home and abroad at present quality that adopts air pollution index PM10 to characterize air quality, representative and very convenient.Along with progress of science and technology, it is found that real what influence human health is that the air medium power is learned the particulate of diameter less than 2.5 μ m.The U.S. has carried out the PM2.5 standard, China will be before 2008 Olympic Games integrates with the air quality standard of developed country, carry out the PM2.5 standard as early as possible, carry out the development of the air sampling filter membrane relevant with PM2.5, the development that particularly can effectively detect the air sampling film of microorganism in the air (the particularly detection of SARS virus, influenza virus, adenovirus etc.) has crucial meaning.
Along with people pay attention to air-polluting, develop the air sampling rig of multiple different types both at home and abroad, comprising filtering type, impacting type and centrifugal etc. several.Utilizing filtration to gather aerosol particle in these several typical air samplers is the most general method of sampling of aerosol, also is to collect the simple and inexpensive method of aerosol sample.The most important character of filtering type sampler is the filter efficiency height, and it can be retained down particle in the air (particle diameter 〉=aperture or particle diameter are slightly smaller than the aperture).Therefore the filter membrane air sampler is called as absolute sampler, usually is used as the last contrast of other samplers.
Filter membrane material commonly used exists significantly not enough, shows as following two aspects:
1, can not make flux and hold back the useful combination of efficient.Filter membrane material commonly used adopts the filter membrane in 10 μ m apertures mostly, and the aperture is bigger, and not only smaller particles is difficult to hold back, and it is also bigger to detect error.For holding back than small-particle, the aperture of filter membrane material will be less, must adopt the less filter membrane in aperture, and will gather virus, and then the aperture of film will reach nanoscale.Adopt less its flux of film in aperture to want corresponding minimizing, so that the sampler cisco unity malfunction.These deficiencies usually are because the structure of filter membrane itself causes.
2, can not make action of microorganisms and hold back the useful combination of efficient.When sampling of aerosol, often only consider the efficient of holding back of filter membrane, and ignored the biological agent of filter membrane material particulate.When gathering bioaerosol, be activated microorganism owing to what gather, used filtrate is that microorganism is not suppressed or killing action at least.Because filter membrane method is earlier to be trapped in aerosol particle on the filter membrane and then to cultivate, therefore comparatively ideal filter membrane is can keep activation of microorganism to a certain extent to the microorganism of being held back in sampling process.Result of experiment has more reliability like this.And the many effects, particularly some chloride materials that inhibition or killing microorganisms are arranged of filter membrane material commonly used.Though some does not have to suppress or the effect of killing microorganisms, perhaps act on not obviously, do not have which kind of filter membrane material can keep activation of microorganism to a certain extent substantially.
Hence one can see that, and in the Filter film type sampler, key technology is exactly to prepare the filter membrane material that the aperture is controlled, pore-size distribution is narrow, porosity is high.For being used in filter membrane material in the microorganism sampler especially for the sample material of infectious virus such as SARS virus, popular virus, avian influenza virus, also require to have certain biologically active, can in one short period, keep the activation of microorganism of holding back.For from the used filter membrane material of present domestic filtering type sampler, be difficult to solve the aforesaid drawbacks preferably.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method who is used for air bacterium and viral sample detecting filter membrane.
Be positioned on the glass plate of level supporting perforated membrane; regulate the height of system hymenotome; speed follow rest with per minute 5～6cm; make the shitosan preparation liquid be evenly distributed on porous film surface and form the composite membrane cortex; reaction temperature is 20～30 ℃; humidity is 20～50%; pressure is negative pressure;. use 40～80 ℃ of heat treatments 1～3 hour then; make the different composite membrane cortex in aperture by the concentration of regulating the shitosan preparation liquid simultaneously; the mass percent concentration of shitosan preparation liquid is 0.05～3.0%; the preparation method of chitosan solution is: take by weighing deacetylation shitosan 1～5 gram, put into 250ml conical beaker with cover, add 100～250ml deionized water then; use magnetic agitation 2～3 hours down at 40～80 ℃; shitosan is fully dissolved, and suction filtration while hot adds proper quantity of defoaming agent and stirs froth breaking then; filtrate is positioned in the darkroom cools off, and leaves standstill after 1～3 day stand-by.
The present invention is directed to filter membrane material commonly used and can not make, a kind of composite membrane of suitable air microbe sampling is provided action of microorganisms and hold back the useful combination of efficient.This composite membrane is made through the macromolecular substances solution coatings by perforated membrane.Macromolecular complex mass-energy keeps the activation of microorganism of holding back to a certain extent in this composite membrane.This performance of this composite membrane depends on the character of macromolecular substances.
This composite membrane contrasts the formation that other filter membranes can reduce filter cake, and under the same test condition, flux obviously increases than other filter membranes of same apertures.Simultaneously used big molecular coatings solution biologically active, therefore not only can not suppress or killing microorganisms, and can help microorganism to keep active to a certain extent, make the situation of the more real reaction air of sample, the problem that microbial activity keeps when having improved microbe sampling again reduces and detects error.
Description of drawings
Fig. 1 is the Electronic Speculum figure after perforated membrane of the present invention is sampled by the PM2.5 sampler;
Fig. 2 is the particle diameter distribution map of embodiments of the invention 8;
Fig. 3 is the graph of pore diameter distribution of composite membrane of the present invention (coating of 0.5% shitosan preparation liquid makes);
Fig. 4 is a perforated membrane graph of pore diameter distribution of the present invention.
The specific embodiment
Preparation liquid of the present invention is 0.05～3.0% chitosan solution.0.05 the preparation method of～3.0% chitosan solution is: take by weighing deacetylation shitosan 1～5 gram; put into 250ml conical beaker with cover; add 100～250ml deionized water then; use magnetic agitation 2～3 hours down at 40～80 ℃; chitosan solution is fully dissolved, and suction filtration while hot adds proper quantity of defoaming agent and stirs froth breaking then; filtrate is positioned in the darkroom cools off, and leaves standstill after 1～3 day stand-by.
The mass percent concentration of shitosan preparation liquid of the present invention is 0.05～3.0%.The material of perforated membrane is the high-molecular organic material of modified poly (ether-sulfone), polyester, Merlon, Kynoar, perhaps is aluminium oxide, silica, titanium oxide, zirconia.The duct of perforated membrane is column construction or becomes to be communicated with network structure that the aperture is in 0.1～1.0 mu m range, and porosity is between 20～70%.
The good characteristic of this perforated membrane depends on the technology of filter membrane material itself and system film.We have at first carried out primary election to filter membrane material, the filter membrane material after the primary election have been carried out the mensuration of aspects such as flux, mechanical strength and chemical stability.Choose metal oxide and high molecular polymer at last and made the material of preparation perforated membrane.
Embodiment 1
Be positioned on the glass plate of level supporting perforated membrane, the stand-by preparation liquid (0.75% chitosan solution) of preparation is coated on the support porous film surface. regulate the height of system hymenotome, speed follow rest with per minute 5cm, preparation liquid is evenly distributed on supports on the perforated membrane, use 40 ℃ of heat treatments 3 hours then.
Embodiment 2
Be positioned on the glass plate of level supporting perforated membrane, the stand-by preparation liquid (0.75% chitosan solution) of preparation is coated on the support porous film surface. regulate the height of system hymenotome, speed follow rest with per minute 5cm, preparation liquid is evenly distributed on supports on the perforated membrane, use 80 ℃ of heat treatments 1 hour then.
Embodiment 3
Be positioned on the glass plate of level supporting perforated membrane, the stand-by preparation liquid (0.75% chitosan solution) of preparation is coated on the support porous film surface. regulate the height of system hymenotome, speed follow rest with per minute 6cm, preparation liquid is evenly distributed on supports on the perforated membrane, use 40 ℃ of heat treatments 3 hours then.
Embodiment 4
Be positioned on the glass plate of level supporting perforated membrane, the stand-by preparation liquid (0.75% chitosan solution) of preparation is coated on the support porous film surface. regulate the height of system hymenotome, speed follow rest with per minute 6cm, preparation liquid is evenly distributed on supports on the perforated membrane, use 40 ℃ of heat treatments 3 hours then.
Embodiment 5
The concentration that changes preparation liquid in the film-forming process can make the composite membrane in different apertures.The concentration range of preparation liquid from 0.5% to 3%.
Embodiment 6
This example supports composite membrane with the inorganic, metal oxide porous and places the PM2.5 sampler, and the composite membrane diameter is 25mm, is used for the sampling of aerodynamic diameter less than 2.5 μ m particles.Under vacuum 80Kpa condition, sample half an hour, from the PM2.5 sampler, take out filter membrane, carry out the Electronic Speculum of face distribution of particles and measure.
With contrast with other filter membrane variations of flux in aperture.Inorganic, metal oxide perforated membrane flux stabilized.Show that by electromicroscopic photograph sampling particle aerodynamic diameter is basically less than 2.5 μ m.Contrast with other membrane retention amounts with the aperture.Under identical sampling condition, the perforated membrane flux of flowing through is more than big than other several filter membranes.Improved the accuracy of experiment like this.
The sampling of employing composite membrane, molecule (aerodynamic diameter is less than the 50nm) number of escaping in the sampling process as can be known by electron microscope obviously reduces, contrast other filtering types PM2.5 sampler, the sample effect that the PM2.5 sampler of composite membrane is housed obviously improves.
Embodiment 7
This example has been carried out flux mensuration to inorganic, metal oxide perforated membrane and the composite membrane of diameter 25mm and diameter 47mm respectively.The aperture of perforated membrane is about 200nm, and the aperture of composite membrane cortex is a tens nanometer.Under vacuum 80Kpa condition, the gas permeation flux that records diameter 25mm perforated membrane is 802.7m
3/ m
2.h (standard state), the gas permeation flux of diameter 25mm composite membrane is 488.9m
3/ m
2.h (standard state); Under vacuum 20Kpa condition, the gas permeation flux of diameter 47mm perforated membrane is 797.7m
3/ m
2.h (standard state), the gas permeation flux of diameter 47mm composite membrane is 468.6m
3/ m
2.h (standard state).This perforated membrane and composite membrane flux have satisfied the traffic requirement of general sampler, and (flow of the air sampler of low discharge is at 500m
3/ m
2.h about).
Embodiment 8
This example adopts the two-stage air sampler, first order sampler dress inorganic, metal oxide perforated membrane (diameter 25mm, aperture 200nm), and second level sampler assembling composite membrane (diameter 25mm, composite membrane aperture 50nm), two samplers are connected in series.Under vacuum 80Kpa condition, collect the particulate on the secondary sampler, the analysis of weighing is carried out particle size distribution measuring to the particle on the sampling film of the second level simultaneously.Utilize ZATEZSIZER particle diameter distribution instrument that the back particulate held back of composite membrane of sampling has been carried out the particle diameter distribution tests, the particle diameter of surveying as shown in the figure, basically all between 50nm and 200nm.
Embodiment 9
This example adopts the composite membrane of cortex (aperture 200nm, diameter 47mm).As the test of sampling outside the microbial room in the air, sample is by the microorganism culture assays.Zhejiang Center For Disease Control and Prevention's Bacteriology Room provides the (700cfu/m that reports the result
3), with microbe quantity (500～1000cfu/m in the air of Local Units report
3) quite approaching.In the repeatedly sampling analysis of same sampled point, the result shows: total number of bacteria is all at 560cfu/m in the interior air of this sampled point
3To 800cfu/m
3Between, sample detecting mean value is 730cfu/m
3Adopt traditional CAM to carry out parallel sample detecting simultaneously, total number of bacteria is 250cfu/m in the testing result air
3The film of making by two kinds of different materials compares, and composite membrane of the present invention has the effect of certain maintenance microbial activity.
Claims (4)
1. preparation method who is used for air bacterium and viral sample detecting filter membrane; it is characterized in that: will support on the glass plate that perforated membrane is positioned over level; regulate the height of system hymenotome; speed follow rest with per minute 5～6cm; make the shitosan preparation liquid be evenly distributed on porous film surface and form the composite membrane cortex; reaction temperature is 20～30 ℃; humidity is 20～50%; pressure is negative pressure; use 40～80 ℃ of heat treatments 1～3 hour then; make the different composite membrane cortex in aperture by the concentration of regulating the shitosan preparation liquid simultaneously, the mass percent concentration of shitosan preparation liquid is 0.05～3.0%, and the preparation method of shitosan preparation liquid is: take by weighing deacetylation shitosan 1～5 gram; put into 250ml conical beaker with cover; add 100～250ml deionized water then, use magnetic agitation 2～3 hours down, shitosan is fully dissolved at 40～80 ℃; suction filtration while hot then; add proper quantity of defoaming agent and stir froth breaking, filtrate is positioned in the darkroom cools off, and leaves standstill after 1～3 day stand-by.
2. a kind of preparation method who is used for air bacterium and viral sample detecting filter membrane according to claim 1, it is characterized in that: the material of said perforated membrane is the high-molecular organic material of modified poly (ether-sulfone), polyester, Merlon or Kynoar.
3. a kind of preparation method who is used for air bacterium and viral sample detecting filter membrane according to claim 1, it is characterized in that: the material of said perforated membrane is aluminium oxide, silica, titanium oxide or zirconia.
4. a kind of preparation method who is used for air bacterium and viral sample detecting filter membrane according to claim 1 is characterized in that: the duct of said perforated membrane is column construction or becomes to be communicated with network structure that the aperture is 0.1～1.0 μ m, and porosity is 20～70%.
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| CN 200410025764 CN1257762C (en) | 2004-06-29 | 2004-06-29 | Preparation method of detection filter membrane used for bacteria and virus sampling in air |
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|---|---|---|---|
| CN 200410025764 CN1257762C (en) | 2004-06-29 | 2004-06-29 | Preparation method of detection filter membrane used for bacteria and virus sampling in air |
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| CN1257762C true CN1257762C (en) | 2006-05-31 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4194596A1 (en) | 2021-12-10 | 2023-06-14 | Kaunas University of Technology | Nano/micro composite fibrous filter for sampling aerosol particles and production method thereof |
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|---|---|---|---|---|
| CN105296340B (en) * | 2014-09-19 | 2018-03-27 | 青岛市中心医院 | A kind of intestinal contents fractions extraction element |
| WO2022120561A1 (en) * | 2020-12-08 | 2022-06-16 | 深圳先进技术研究院 | Water-soluble gel membrane having virus enrichment function, and preparation method therefor and application thereof |
| CN114272772A (en) * | 2021-12-31 | 2022-04-05 | 杭州科百特过滤器材有限公司 | Asymmetric PES (polyether sulfone) porous membrane for virus removal and preparation method thereof |
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| EP4194596A1 (en) | 2021-12-10 | 2023-06-14 | Kaunas University of Technology | Nano/micro composite fibrous filter for sampling aerosol particles and production method thereof |
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