CN104198221B - Aquatic plant grease-cellulose acetate composite semipermeable membrane type bionic passive sampling device - Google Patents
Aquatic plant grease-cellulose acetate composite semipermeable membrane type bionic passive sampling device Download PDFInfo
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- CN104198221B CN104198221B CN201410287920.6A CN201410287920A CN104198221B CN 104198221 B CN104198221 B CN 104198221B CN 201410287920 A CN201410287920 A CN 201410287920A CN 104198221 B CN104198221 B CN 104198221B
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- cellulose acetate
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Abstract
The invention relates to an aquatic plant grease-cellulose acetate composite semipermeable membrane. Inexpensive and protogenetic aquatic plant grease is used as a main raw material, and highly hydrophilic cellulose acetate is used as an outer membrane material to prepare the aquatic plant grease-containing semipermeable membrane which has the advantages of uniform grease dispersion, large specific area and integrated structure. The balance time required for collection of hydrophobic organic pollutants in a water body can be shortened greatly, and costs of raw materials can be reduced significantly. The invention also provides a preparation tool and a preparation method for preparation of the aquatic plant grease-cellulose acetate composite semipermeable membrane. In addition, the invention provides a supporting external device suitable for in-situ sampling of organic pollutants in lakes, rivers and other water bodies. The simulation of aquatic plants can be realized for in-situ, accurate, convenient and low-cost monitoring of organic pollutants in water bodies.
Description
The application is the divisional application of an application for a patent for invention.The applying date of original application is on October 31st, 2012, Shen
Please number be 201210427132.3, invention and created name be the " water plant fat-bionical quilt of cellulose acetate composite semi-permeable membrane
Dynamic sampling apparatuses ".
Technical field
The invention belongs to field is learned on environmental science, analytical chemistry and ground, it is related to a kind of water plant fat-cellulose acetate
The bionical passive sampling apparatus of composite semi-permeable membrane and correlation technique, are combined particularly to water plant fat-cellulose acetate and partly ooze
Permeable membrane, water plant fat-cellulose acetate composite semi-permeable membrane prepare instrument and be applied to the water bodys such as lake, river
The corollary apparatus of organic pollution in situ sampling.
Background technology
Organic pollution is extensive in the water bodys such as lake, river or even potable water source district, persistently presence, has carcinogenic, cause
The effects such as abnormal, mutagenesis, constitute very big threat to aquatic ecosystem, also can be transmitted, be amplified and enter by aquatic ecosystem
Food chain, is detrimental to health, and causes World Health Organization (WHO)（WHO）And the highest attention of various countries' food, hygiene department.Cause
This it would be highly desirable to strengthen lake, in river especially its water head site organic pollution monitoring, conscientiously ensure drinking water safety and resident
Health.However, the Sampling techniques of current Organic Pollutants In Water be difficult to meet lake, the monitoring of river large area convenient, in situ,
Accurately, the requirement such as continuous, has had a strong impact on accurate evaluation and the drinking water safety guarantee of the ecological risk of organic pollution.
It has been generally acknowledged that the organic pollution being only freely soluble in water body or pore water just by bio-absorbable and can produce
Potential toxic action, and the free the dissolved organic pollution in water body can be with DOM, suspended particulate substance and deposition
Thing etc. combines, and affects the mensure of its actual concentration and the accurate evaluation of ecological risk.Therefore, accurately, in in-situ acquisition water body certainly
It is the key carrying out its monitoring and urban eco landscape forest by the organic pollution of the dissolved.
Active Sampling techniques（As：Chemical leaching test, physical method etc.）It is widely used in organic contamination in water body at present
The collection of thing, wherein chemical leaching test use is more extensive, but needs collection, transport, stores substantial amounts of water sample or deposit sample
Product, waste time and energy, and generally obtain is the instantaneous total concentration of water body or hole organic pollutants（Concentration containing combined state）,
Its ecological risk will be over-evaluated with the biological effectiveness that this concentration reflects organic pollution；Physical method is also applied in water body
The collection of organic pollution, such as：Centrifugation, chromatography, although using higher rotating speed, it is organic that the mode of centrifugation is still difficult to exclusion dissolving
The interference of free the dissolved in confrontation pore water.Although chromatography can preferably be isolatable from by the organic contamination of the dissolved and combined state
Thing, but waste time and energy it is difficult to meet lake water head site high frequency time, high-volume monitoring easily requires.
Passive sampling technology（As：Solid-Phase Extraction, solid-phase microextraction, ion liquid abstraction, semipermeable membrane sampling etc.）Quilt at present
It is widely used in the collection of free the dissolved organic pollution in surrounding medium, the concentration of its collection is that time weight is averagely dense
Degree, reaching sampling balance post-sampling medium in constant concentration constant, have continuous sampling, save solvent, reduce purifying step, do not break
The advantages of bad dielectric structure.Wherein, solid phase micro-extraction technique（SPME）The collection side of free dissolved organic matter in aqueous medium
Face use relatively broad, but less be applied to water body in-situ sampling, need in addition using business-like extracting fiber, experimental cost
Higher it is difficult to meet water head site high frequency time, high-volume monitor low cost requirement；Solid phase extraction techniques are also widely used for water
The collection of organic pollution in sample, but in water sample organic pollutant enrichment to solid-phase extraction column and eluting needs the long period, and
Business-like solid-phase extraction column experimental cost higher it is also difficult to realize the target of water body organism in-situ monitoring；Ionic liquid extracts
Also there is more application in terms of taking the technology collection of Organic substance in water sample in recent years, but be also difficult to meet Organic Pollutants In Water
The requirement of in-situ monitoring.
Early-stage Study and correlational study all show：（1）Biolipid is during biological concentration hydrophobic organic pollutant
Play pivotal role（Water, cellulose, saccharide, protein isopolarity component contribute very little to the enriching quantity of organic pollution）；
（2）Biological（Including animal and plant）To the enrichment of nonionic organic pollution with Passive diffusion as main path；（3）Biological
Film has played molecular sieve effect.Thus can be using the semi-permeable membrane materials simulation biological concentration organic contamination containing biolipid or lipoid
The process of thing.According to this imagination, research in recent years person have developed successively multiple containing fat（Lipoid）Bionical passive sampling material.Its
In, Huckins etc.（Huckins, J. N.; Tubergen, M. W.; Manuweera, G. K. Semipermeable
membrane devices containing model lipid: A new approach to monitoring the
bioavailability of lipophilic contaminants and estimating their
bioconcentration potential.Chemosphere, 1990, 20, 533 - 552.）Three Oleic acid developed are sweet
Grease-Low Density Polyethylene semipermeable membrane devices（SPMD）It is to coat the main of tallow on low density polyethylene films surface
Composition glycerol trioleate.Although SPMD has been achieved with commercialization at present and is widely used in continuous acquisition water body
Organic pollution, but because it is outer membrane material, is assumed " sandwich " using the strong Low Density Polyethylene of hydrophobicity
（Sandwich) structure, thus there is the defects such as uneven, the sampling equilibration time length of fat dispersion.Subsequently, more researcher around
The outer membrane material the sampling apparatuses of semipermeable membrane containing fat is improved, such as：Prince is good for and waits on the basis of SPMD with hydrophilic
Cellulose acetate be outer membrane material, prepared glycerol trioleate cellulose acetate semipermeable membrane sampling apparatuses
（TECAM）（Xu, Y.; Wang, Z.; Ke, R.; Khan, S. Accumulation of organochlorine
pesticides from water using triolein embedded cellulose acetate
membranes.Environ. Sci. Technol., 2005, 39, 1152 - 1157.）, but the three of its commodity in use
Olein, experimental cost is higher.
Water plant is the organic carbon source of a large amount of distributions in the water bodys such as lake, river, and its stem and leaf is flourishing, root system is undeveloped,
Contain more C in vivo16, C18, C24Deng unsaturated fatty acid and its ester, there is to hydrophobic organic pollutant stronger richness
Collection ability, has played important function in terms of purification of water quality（Dhir, B.; Shamila, P.; Saradhi, P. P.
Potential of aquatic macrophytes for removing contaminants from the
environment.Crit.Rev. Env. Sci. Technol., 2009, 39, 754 - 781.）, its internal pollution
Thing concentration can reflect the change of quality of water environment to a certain extent.Compared with aquatic animal, water plant is the organic dirt of water body
The natural in-situ monitoring body of dye thing and accumulation body, have more advantage in terms of organic pollution in-situ monitoring.However, species difference
Greatly, poor reproducibility, the defect such as be difficult to survive constrain application in terms of organic pollutants in water body in-situ monitoring for the water plant.Cause
This, filter out and can dissolve majority hydrophobic organic pollutant and have the primary of higher lipid-water partition coefficients to organic pollution
Water plant fat, being prepared into the bionical semipermeable membrane sampling apparatuses containing vegetable butter is to substitute water plant monitoring, development containing fat
Triolein SPMD technology simultaneously realizes water head site original position, a good thinking of accurate, convenient, inexpensive monitoring.
Content of the invention
The primary and foremost purpose of the present invention is to provide a kind of water plant fat-cellulose acetate composite semi-permeable membrane, for drinking
The great demand of country of water-rock reactions and the Sampling techniques using in the world at present are difficult to meet organic contamination in water head site
The particular/special requirement of thing monitoring, with cheap, primary water plant fat as primary raw material, with cellulose acetate as outer membrane material,
Develop that fat is uniformly dispersed, specific surface area is big, the semipermeable membrane containing water plant fat of one, realizes the water bodys such as lake, river
Especially in water head site, the original position of organic pollution, accurate, convenient, inexpensive monitoring, are in drinking water safety guarantee and water body
The urban eco landscape forest of organic pollution provides technical support.
Second object of the present invention is to provide one kind to be used for preparing above-mentioned water plant fat-cellulose acetate compound half
Extensive preparation and the application preparing instrument, be easy to this composite semi-permeable membrane of permeable membrane.
Third object of the present invention is to provide the preparation of above-mentioned water plant fat-cellulose acetate composite semi-permeable membrane
Method, improves the performance of invented composite semi-permeable membrane.
Fourth object of the present invention is to provide one kind to be applied to the Organic Pollutants In Water in situ sampling such as lake, river
Supporting outer device, internal equipped with above-mentioned water plant fat-cellulose acetate composite semi-permeable membrane, realize in-situ monitoring.
The present invention is achieved through the following technical solutions：
First, a kind of water plant fat-cellulose acetate composite semi-permeable membrane, this composite semi-permeable membrane by cellulose acetate,
Cis- 9,12-, 18 carbon-dienoic acid, anhydrone, acetone and Isosorbide-5-Nitrae-dioxane are made, and the mass ratio of each raw material is successively
For 9：1 ：1 ：40 ：5.
Cis- 9,12-, 18 carbon-dienoic acid is water plant fat, and chemical formula is C18H32O2, structural formula below figure.This is aquatic
Vegetable butter is derived from the protophyte such as lake, river.Water plant is extracted by fat extractor（Little thatch grass, Herba vallisneriae Spiralis, horse
Come Herba potamogetonis distincti, watermifoil, frogbit, floating heart etc.）Internal fat, by semi-preparative liquid chromatograph separation, purification, collects fat
Each component, passes through HPLC-MS instrument, nuclear magnetic resonance analyser and Fourier transform infrared spectrometer etc. further
Instrument, determines chemical molecular formula and the structural formula of each component of lipid.By measure target organic pollution each component of lipid with
Equilibrium distribution coefficient in water, filters out the fat prepared needed for semipermeable membrane.Through screening, in the present invention, fat used is cis-
9,12- 18 carbon-dienoic acid.
2nd, a kind of water plant fat-cellulose acetate composite semi-permeable membrane prepare instrument, including scraper and tempering glass
Glass plate, has a cuboid-type glass groove above armorplate glass, the lower edge of scraper can frame the two of cuboid-type glass groove
On side.
Described scraper is cuboid-type, and lower edge is wedge shape.
Described cuboid-type glass groove is formed by connecting by safety glass bar head and the tail.
The thickness of described safety glass bar is 50-200 μm.
Described cuboid-type glass groove both sides are respectively provided with the safety glass of the cuboid-type parallel to glass groove
Retaining groove.
Described safety glass retaining groove exceeds armorplate glass 0.2-1 cm.
3rd, a kind of method preparing water plant fat-cellulose acetate composite semi-permeable membrane, the method includes following step
Suddenly：
（1）Ratio according to claim 1 weighs various raw materials successively；
（2）Sonic oscillation 1 hour after various raw material stirring mixing；
（3）It is no less than 24 hours with 100 revs/min of constant temperature oscillations under 25 °C, until Casting solution mix homogeneously, clarification,
Bubble-free；
（4）Take out the cuboid-type glass groove that the raw material after a small amount of mixing pours on armorplate glass so as to uniformly
Be separated into strip；
（5）With scraper wedge shape lower edge along cuboid-type glass groove upper limb, using the weight of scraper itself, evenly
Scrape water plant fat-cellulose acetate composite semi-permeable membrane；
（6）Clean fume hood is placed 13 minutes, subsequently puts at room temperature in distilled water and soak 35 points
Clock；
（7）Water plant fat-cellulose acetate the composite semi-permeable membrane of solidification is taken off from cuboid-type glass groove.
4th, a kind of supporting outer device equipped with water plant fat-cellulose acetate composite semi-permeable membrane, including rustless steel
The rustless steel spiral cover at cylinder and two ends, is to threaded between spiral cover and rustless steel cylinder, spiral cover has aperture, internal
It is welded with stainless (steel) wire, the aperture of stainless (steel) wire is 75 150 μm；Rustless steel cylinder is longitudinally divided into two halves, two halves
Between place water plant fat-cellulose acetate composite semi-permeable membrane.
Longitudinally asymmetric on described rustless steel cylinder it is welded with two rustless steel nuts.
Good effect using technique scheme：The composite semi-permeable membrane that the present invention develops employs cellulose acetate generation
Glycerol trioleate-Low Density Polyethylene the semipermeable membrane devices of the developments such as Huckins are replaced（SPMD）The low-density using
Polyethylene outer membrane material, hydrophilic strengthens so that outer membrane material and biolipid, cosolvent etc. are dissolved in one, are uniformly dispersed, and compares table
Area is bigger, greatly shortens the required equilibration time of hydrophobic organic pollutant collection in water body；Simultaneously as develop
It is raw material that composite semi-permeable membrane employs cheap, primary water plant fat, instead of prince be good for etc. research and development three Oleic acid sweet
Grease cellulose acetate semipermeable membrane sampling apparatuses（TECAM）The business-like glycerol trioleate using, greatly reduces
The cost of raw material, and can realize simulating water plant to the original position of the organic pollution in water body, accurate, convenient, low one-tenth
This monitoring；Extensive preparation and the application preparing instrument, be easy to this composite semi-permeable membrane that the present invention develops, and supporting outer device
In-situ monitoring can be realized.
Brief description
Fig. 1 is the structural representation preparing instrument in the present invention；
Fig. 2 is the structural representation of supporting outer device in the present invention；
Fig. 3 is the longitudinal section of supporting outer device in the present invention；
Fig. 4 is the use state schematic diagram of supporting outer device in the present invention.
In figure：1 scraper, 2 armorplate glasses, 3 glass grooves, 4 safety glass bars, 5 safety glass retaining grooves, 6 rustless steel circles
Cylinder, 7 spiral covers, 8 semipermeable membranes, 9 stainless (steel) wires, 10 nuts, 11 ball floats, 12 weights.
Specific embodiment
With reference to embodiment and test example, technical scheme is described further, but should not be construed as right
The restriction of the present invention：
The making preparing instrument of embodiment one water plant fat-cellulose acetate composite semi-permeable membrane
Fig. 1 is the structural representation preparing instrument in the present invention, as shown in the figure：
（1）It is base using smooth armorplate glass 2, using four width in the upper surface of armorplate glass 2 is 5
Mm, thickness are 50 200 μm of thin tempering glass bar 4, head and the tail first tie, structure go out length be 15 cm, width be 12 cm, depth
Spend the cuboid-type glass groove 3 for 50 200 μm, the thickness of semipermeable membrane according to actual needs, corresponding adjustment glass
The depth of groove 3；
（2）The scraper 1 prepared needed for semipermeable membrane is developed using the safety glass or metal material with constant weight,
Scraper 1 is in cuboid-type, and the width of scraper 1 is 12 cm, and highly for 5 10 cm, thickness is 0.5-0.8 cm, scraper 1
Lower edge is wedge shape；The lower edge of scraper 1 can frame on two sides of cuboid-type glass groove 3.
（3）The left and right of glass groove 3 outer is respectively provided with the safety glass gear of the cuboid-type parallel to glass groove 3
Groove 5.Safety glass retaining groove 5 exceeds toughened glass base 0.2 1 cm, is used for preventing scraper in semipermeable membrane preparation process left
Move right.
The preparation of embodiment two water plant fat-cellulose acetate composite semi-permeable membrane
It is 9 according to mass ratio：1 ：1 ：40 ：5 ratio weighs cellulose acetate, cis- 9,12- 18 carbon-two respectively
Olefin(e) acid, anhydrone, acetone and Isosorbide-5-Nitrae-dioxane, shake putting in ultrasonic cleaner after the stirring mixing of various materials
Swing 1 hour, be no less than 24 hours with 100 revs/min of constant temperature oscillations under 25 °C, until Casting solution mix homogeneously, this
When Casting solution clarification, without any bubble and solid impurity.Take out the raw material after a small amount of mixing to pour on armorplate glass 2
Cuboid-type glass groove 3 so as to uniformly be separated into strip, width be 12 cm.Scraper 1 is put into two pieces of left and right
Between safety glass retaining groove 5, scraper 1 wedge shape lower edge is close to above glass groove 3, by the own wt of scraper 1, at the uniform velocity
Scrape semipermeable membrane.Clean fume hood is placed 13 minutes, subsequently puts at room temperature and in distilled water, soak 35
Minute.Water plant fat-cellulose acetate the composite semi-permeable membrane of solidification is taken off from cuboid-type glass groove 3.Treat acetone
After volatilizing completely, in the semipermeable membrane prepared, the content of cis- 9,12-, 18 carbon-dienoic acid is 6.25%, and thickness is 100
M, average density is 30 mg cm-2.Also can cis- 9,12- ten according to the needs of actual samples, in suitable adjustment semipermeable membrane
The content of eight carbon-dienoic acid and the thickness of semipermeable membrane.
Embodiment three is applied to the making of the supporting outer device of the Organic Pollutants In Water in situ sampling such as lake, river
Fig. 2 is the structural representation of supporting outer device in the present invention, and Fig. 3 is that the vertical profile of supporting outer device in the present invention regards
Figure, in conjunction with shown in Fig. 2, Fig. 3, this supporting outer device, including the spiral cover 7 at rustless steel cylinder 6 and two ends, spiral cover 7 with stainless
It is threaded between steel cylinder 6, spiral cover 7 has aperture, inner side is welded with stainless (steel) wire 9, and the aperture of stainless (steel) wire 9 is 75
150 μm, it is easy to water body and flows into and stop biology and particulate matter etc. to disturb.Rustless steel cylinder 6 is longitudinally divided into two halves,
Place water plant fat-cellulose acetate composite semi-permeable membrane 8 between two halves, the organic pollution in water body is enriched with.
The content of the organic pollution in semipermeable membrane 8 after measure collection balance, realize organic pollution original position, accurately,
Convenient, inexpensive monitoring.
Longitudinally asymmetric on rustless steel cylinder 6 it is welded with two rustless steel nuts 10, primarily to solid for sampling tether
Fixed use.
Fig. 4 is the use state schematic diagram of supporting outer device in the present invention, as shown in figure 4, according to rustless steel circle during sampling
The external diameter of cylinder 6 and length, cut out the water plant fat-cellulose acetate composite semi-permeable membrane 8 of correspondingly-sized, will partly ooze
What permeable membrane 8 was smooth is clipped between two panels rustless steel cylinder 6, screw two ends with aperture and be welded with the rotation of stainless (steel) wire 9
Lid 7.Mother Luo 10 fastens nylon rope, and the other end of nylon rope fastens foam ball float 11, according to water depth and the depth to be sampled,
Suitably the distance between adjustment foam ball float and sampling apparatuses can be sampled.Can also be according to water depth and sampling need
Will, it is additionally arranged at the bottom weight 12 in sampling apparatuses, the position of sampling apparatuses is fixed.
Test example one apparatus of the present invention are compared with the sample effect of existing relevant apparatus in the world
（1）Glycerol trioleate-Low Density Polyethylene semipermeable membrane sampling apparatuses with developments such as Huckins（SPMD）
Use Low Density Polyethylene outer membrane material compare, present invention uses hydrophilic cellulose acetate be outer membrane material so that
Outer membrane material and biolipid, cosolvent etc. are dissolved in one, overcome " sandwich " structure of SPMD；Unit bodies adipopexia is disperseed
Evenly（1 mL water plant fat is uniformly dispersed in 15000 cm2Cellulose acetate surface, in significantly larger than SPMD
1 mL glycerol trioleate is dispersed in 450 cm2Low Density Polyethylene surface）So that compared with high hydrophobicity organic pollution in water body
Collection equilibration time shorten in one week, well below the time of month needed for SPMD；The fat that the present invention uses is derived from
In cheap water plant, cost, well below business-like glycerol trioleate, greatly reduces the sampling of semipermeable membrane containing fat
The cost of device field large-scale application；
（2）It is good for etc. the glycerol trioleate-cellulose acetate semipermeable membrane sampling apparatuses of development with prince（TECAM）Phase
The fat that the present invention uses comes from cheap water plant to ratio, and cost, well below business-like glycerol trioleate, drops significantly
The low cost of the sampling apparatuses of semipermeable membrane containing fat field large-scale application, can also simulate water plant to dirt organic in water body
Dye thing carries out in-situ monitoring.
Claims (2)
1. a kind of supporting outer device of organic pollution in situ sampling be applied to lake, river water it is characterised in that：Including
Rustless steel cylinder（6）And the rustless steel spiral cover at two ends（7）, spiral cover（7）With rustless steel cylinder（6）Between for screw thread even
Connect, spiral cover（7）On have aperture, internal welding is connected to stainless (steel) wire（9）, stainless (steel) wire（9）Aperture be 75 150 μm；Rustless steel
Cylinder（6）Longitudinally it is divided into two halves, between two halves, place semipermeable membrane（8）；
Wherein, described semipermeable membrane（8）By cellulose acetate, cis- 9,12- 18 carbon-dienoic acid, anhydrone, third
Ketone and Isosorbide-5-Nitrae-dioxane are made, and the mass ratio of each raw material is followed successively by 9：1 ：1 ：40 ：5.
2. supporting outer device according to claim 1 it is characterised in that：Described rustless steel cylinder（6）Upper axial direction is right
Claim to be welded with two rustless steel nuts（10）.
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| CN201410287920.6A CN104198221B (en) | 2012-10-31 | 2012-10-31 | Aquatic plant grease-cellulose acetate composite semipermeable membrane type bionic passive sampling device |
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| CN201210427132.3A CN102895887B (en) | 2012-10-18 | 2012-10-31 | Aquatic plant grease-cellulose acetate composite semipermeable membrane type bionic passive sampling device |
| CN201410287920.6A CN104198221B (en) | 2012-10-31 | 2012-10-31 | Aquatic plant grease-cellulose acetate composite semipermeable membrane type bionic passive sampling device |
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| CN105334082B (en) * | 2015-11-19 | 2019-03-12 | 中国科学院广州地球化学研究所 | A kind of Passive sampler |
| CN105806645A (en) * | 2016-05-10 | 2016-07-27 | 北京交通大学 | Driven sampling device for organic pollutants of water and bottom mud and use method thereof |
| CN107037193A (en) * | 2017-06-22 | 2017-08-11 | 泉州师范学院 | A kind of water body free state pollutant passive sampling apparatus and the method for sampling |
| CN107462435A (en) * | 2017-08-01 | 2017-12-12 | 南京理工大学 | It is a kind of using cyclodextrin polymeric membrane as the dynamics passive sampling apparatus with reference to phase |
| CN112934187B (en) * | 2021-02-02 | 2023-02-24 | 中国科学院生态环境研究中心 | Bionic passive sampling membrane based on plant lipid, sampling device and application |
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| US6478961B2 (en) * | 2000-09-26 | 2002-11-12 | The United States Of America As Represented By The Secretary Of The Interior | Device for sequestration and concentration of polar organic chemicals from water |
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