CN106323689A - Water quality monitoring-orientated polar organic trace pollutant trap - Google Patents
Water quality monitoring-orientated polar organic trace pollutant trap Download PDFInfo
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- CN106323689A CN106323689A CN201610692412.5A CN201610692412A CN106323689A CN 106323689 A CN106323689 A CN 106323689A CN 201610692412 A CN201610692412 A CN 201610692412A CN 106323689 A CN106323689 A CN 106323689A
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- adsorbent
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- polystyrene
- organic pollution
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/34—Purifying; Cleaning
Abstract
The invention relates to an accumulative sampling device using a composite characteristic adsorbent as a receiving phase and used for monitoring the concentration of polar organic pollutants in water. The accumulative sampling device is based on a synthetic high molecular membrane material and a mixed-mode solid phase extraction adsorbent, the composite adsorbent is placed between two layers of high molecular membranes to form a sampler adopting a sandwich structure, and the accumulative sampling device can enrich a variety of the polar organic pollutants in water at the same time. In allusion to differences among the polar organic pollutants in water, the accumulative sampling device uses five characteristic solid phase extraction adsorbents to form the mixed-mode adsorbent, and has a polarity range-widened reverse phase adsorption effect, a weak anion exchange effect and a weak cation exchange effect at the same time, and has a broad-spectrum adsorption effect on the polar organic pollutants in water; meanwhile, the accumulative sampling device uses a high molecular osmotic membrane with a specific pore size range as an outer membrane, so that free passing of water, compounds in a freely dissolved state and compounds in a colloidal state can be ensured, the adsorption equilibrium time is shortened, and thus the accumulative sampling device can be used as a balanced sampler for monitoring the organic trace pollutants in water and performing biological simulative sampling.
Description
Technical field
The present invention relates to a kind of with compound characteristics adsorbent for receiving phase, be used for being enriched with and monitor polarity organic contamination in water
The acquisition equipment of thing, due to the restriction in outside polymeric membrane aperture, only allows two kinds of forms such as free the dissolved and colloidal attitude
Polarity organic pollution enters its interior and is adsorbed, true reflection polarity organic pollution biologically effective state in water
Concentration, can be used for simulating biological monitoring, the eco-toxicology effects of evaluation polarity pollutant, screens " priority pollutants ", close
The use of reason management polar contaminants and discharge.
Background technology
The present invention relates to a kind of with compound characteristics adsorbent for receiving phase, be used for being enriched with and monitor polarity organic contamination in water
The acquisition equipment of thing, due to the restriction in outside polymeric membrane aperture, only allows two kinds of forms such as free the dissolved and colloidal attitude
Polarity organic pollution enters its interior and is adsorbed, true reflection polarity organic pollution biologically effective state in water
Concentration, can be used for simulating biological monitoring, the eco-toxicology effects of evaluation polarity pollutant, screens " priority pollutants ", close
The use of reason management polar contaminants and discharge.
Active Sampling techniques
Actively Sampling techniques are to collect and the extraction water pollutant residual most common technology of use, and actively Sampling techniques are applied
The gatherer process of sample need additionaling power just can complete sample collecting work.Liquid-liquid extraction and Solid-Phase Extraction are two quasi-representatives
The active method of sampling.The pollutant levels that liquid-liquid extraction is gathered are the total concentrations of chemicals in sample, it is impossible to district accurately
Bioavailable and the biological compound that not may utilize form in time-sharing environment, and organic solvent consumption is big.In order to solve liquid
The defect of liquid extraction, researchers have developed solid phase extraction method, and including solid-phase extracting disk, this method is by sucking filtration or pump
Water body example is passed through the cylindrical container equipped with macromolecular material by the mode of pressure.
If water body example is more muddy when carrying out sample collecting by active Sampling techniques and extract, then sample is the most first wanted
Could pass through adsorbent filler by glass fiber filter after being filtered, this spline filter is the longest.Additionally, target contaminant is at sample
The contaminant loss problem caused due to volatilization, the absorption of storage container walls and chemicals degraded in the storing process of product.And,
The pollutant levels that actively method of sampling obtains can only reflect the pollutant situation of sampling instant, and this sample mode is easily subject to
The impact of pollutant pulsed input.And, trace analysis and parameter in bio kinetic model research need to gather and process large volume
Sample, takes time and effort.Although also there being researcher to have employed large volume Solid-Phase Extraction sampling system, but still there is Solid-Phase Extraction
The inevitable problem of method, and all use large volume sampling system more to take time and effort when multiple sampled point laid by needs,
Cost of investment is high.
Passive type Sampling techniques
Passive type be the most active for, i.e. need not the one of additionaling power or the energy in passive type mode to carry out sample
Gather and the mode of pollutant extraction.Passive type Sampling techniques are based entirely on chemicals from height to acquisition or the concentration of pollutant
The process that gesture or high fugacity spread automatically to low chemical potential or low fugacity, target contaminant can be along chemical potential difference by passive
Diffusion is from being advanced into organic facies.Compare active Sampling techniques, passive type Sampling techniques closer to pollutant at biologic artifact
Interior enrichment mode.
Passive type Sampling techniques develop for many years, currently for the passive type sampling skill of organic pollution in water environment
Art, mainly includes but not limited to semipermeable membrane sampling apparatus (SPMD), solid-phase micro-extracting device (SPME), solid-phase extracting disk
(ED), polyethylene sampling apparatus (PEDs) and polyformaldehyde sampling apparatus (POM) etc..SPMD is at Low Density Polyethylene (LDPE) material
The material compositions such as the semipermeable membrane central filler glycerol trioleate of matter, the organic pollution in water body can pass through semipermeable membrane quilt
Lipid absorption in film, SPMD has been used successfully to the mensuration of hydrophobic organic compound in water environment, and simulated determination aquatile
Biological concentration process.SPME sampling realizes target contaminant on aqueous phase and SPME phase as early as possible typically by the mode of stirring
Reach partition equilibrium, thus realize the extraction process of target contaminant.These passive sample devices are widely used in simulation biology
Predict biological concentration behavior and the biological effectiveness of hydrophobic organic pollutant in surrounding medium.
Enrichment phase in above passive type Sampling techniques and device is macromolecule organic facies, and polarity is the most weak, substantially with
" similar compatibility " principle completes extraction process, and therefore these class passive type Sampling techniques are primarily adapted for use in hydrophobic organic pollutant
Mensuration, be not appropriate for polarity or hydrophilic organic pollution, although also it has been reported that researcher uses it for the organic dirt of polarity
The mensuration of dye thing, but effect is not ideal.In recent years, the research of medicine and personal care articles is increasingly taken seriously, for
The Sampling techniques (such as polarity organic pollution accumulated samples device, POCIS) of these polarity organic pollutions increasingly receive publicity,
And it is commonly used to estrogen in water environment, antibiotic and the monitoring of non-antibiotic class medicine.Polarity organic pollution accumulated samples
Technology has stronger adhesion to polarity organic pollution, can well solve other passive type Sampling techniques and gather and extraction
The problems such as the Enrichment overlong time that faces when taking polarity organic pollution, enriching quantity are not enough.
Traditional microporous hydrophilic film used by POCIS technology is usually the polyether sulfone materials of 0.1 micron pore size, is using
Finding in journey, owing to the aperture of 0.1 micron is less, object resistance when outer membrane is extracted by internal layer enrichment phase is very big, leads
Causing extraction rate less, through the exposure of 28 day time, object is also in linear concentration stage in sampler, not up to divides
Balancing, can bring in actual applications and often occur that during subsequent applications deviation is relatively big, the longest etc. a series of
Problem.The aperture of 0.1 micron only allows free the dissolved polarity organic pollution to enter sampler and cannot gather colloidal attitude pole
Property organic pollution, the colloidal attitude in natural water body is one important existing forms of polarity organic pollution, and it has equally
There is biological effectiveness.Sampling in natural water body additionally, due to long-time, be susceptible to biofouling phenomenon, biomass blocking is adopted
Sample device outer layer polymeric membrane aperture, affects sampling rate, causes sampling to be normally carried out.Used by traditional POCIS sampler
Adsorbent main Oasis HLB adsorbent, application reverse phase absorption principle to the polarity in water body and nonpolar organic pollutants
Being acquired, owing to it takes into account hydrophilic and lipotropy, and be based only on single reverse phase absorption pattern, therefore it is to polarity organic contamination
Adsorption range and the adsorption efficiency of thing are the highest.At present, open with mixing and absorption pattern (reverse phase absorption and ion-exchange absorption are attached) mechanism
The polarity organic pollution passive sampling technology sent out there is no report.
Summary of the invention
The principle of the present invention (the polarity organic pollution accumulated samples technology of economical and efficient) is: by selecting suitable aperture
The hydrophilic macromolecule permeable membrane of scope, as peplos, in conjunction with specific compound adsorbent as enrichment phase, not only ensure that
Sampler is to the enrichment of wide spectrum polarity organic pollution in water environment and extraction, and substantially reduces the sample collecting time, carries
High enriching quantity and sensitivity for analysis, effectively prevent the biofouling phenomenon of sampler, decrease sampling cost, and then can be high
The realization of effect is simulated biological monitoring and carries out ecological risk assessment.
The present invention selects more wide-aperture permeable membrane in terms of hydrophilic film, can effectively be enriched with and extract overwhelming majority distribution
Neutralize the polarity organic pollution in water body gel phase mutually true dissolving, improve sampling rate, make typical case's polar contaminants at 2 weeks
The most i.e. can reach enrichment balance, it is simple to calculate water pollutant concentration.
The present invention selects at the adsorbent of enrichment phase, takes into full account the autgmentability of sampler, range of application, use cost
Etc. factor, have chosen five kinds of solid phase extraction adsorbentses as accepting phase: polystyrene-divinylbenzene resin (is applicable to absorption anti-
Raw elements etc. are at C18Or C18Retain inadequate polar analytes on adsorbent), ketopyrrolidine bonding polystyrene-divinylbenzene
Resin (on the basis of polystyrene/divinylbenzene resins, be bonded ketopyrrolidine, enhanced surface polarity, reach hydrophilic-
Lipophile balance, it is adaptable to extraction polarity and apolar substance), ketopyrrolidine bonding polystyrene-divinylbenzene resin on
Modify anion exchange groups (pH value can be regulated, multiple acid and alkali substance can be extracted), be bonded at ketopyrrolidine
Polystyrene-divinylbenzene resin on modified cation exchange group (enhancing the absorption property to alkalescence material),
Graphon (has the strongest adsorptivity) to polar substances.In order to be able to be sampler during single extraction as much as possible
Absorption various polarity organic pollution, the present invention to above five kinds of filling adsorption agent according to a certain percentage, by certain means mix
Conjunction forms, and is this compound adsorbent reverse phase absorption effect, weak anionic exchange interaction and weak of simultaneously having that polarity scope increases
Cation exchange interaction, it is achieved mixed model Solid-Phase Extraction is adsorbed, and compare single adsorption pattern sampler, has preferably choosing
Selecting property and extraction efficiency.
Beneficial effect
The advantage of the present invention (polarity organic pollution accumulated samples technology and sampler): Sampling techniques principle and sampler make
Simply, afterwards on the basis of research, use the hydrophilic macromolecule permeable membrane of larger aperture, select applied range, economy
Feasible compound characteristics adsorbent, it is achieved mixed model Solid-Phase Extraction is adsorbed, can be to various polarity organic contamination in water environment
Thing all can realize passive type Sampling techniques and the sampler of efficiently concentrating and extraction, and sampler makes and use cost is low, enrichment
Wide with extraction target contaminant scope, enrichment time is short, and bioaccumulation efficiency is high, and sensitivity for analysis is high, effectively prevent sampler
Biofouling.
In Sampling techniques of the present invention, target contaminant can be rapidly achieved partition equilibrium in sampler, and sampler is as flat
Weighing apparatus sampler uses, and is more convenient for calculating the ambient concentration of target stains in tested water body.
Therefore, Sampling techniques of the present invention improve conventional polar organic pollution accumulated samples technology, advantageously in
Come the monitoring of polarity organic pollution in water environment, simulation biological monitoring and evaluate ecological risk, there is bigger scientific meaning.
Accompanying drawing explanation
Fig. 1 is polarity organic pollution catcher structural representation.
Fig. 2 is the polarity organic pollution catcher enrichment power to sulfapyridine in certain Sewage Plant scene exposes experiment
Learn schematic diagram.
Fig. 3 is that the enrichment to sulfamethoxazole in certain Sewage Plant scene exposes experiment of the polarity organic pollution catcher is moved
Mechanics schematic diagram.
Fig. 4 is the polarity organic pollution catcher enrichment kinetics to ketoprofen in certain Sewage Plant scene exposes experiment
Schematic diagram.
Fig. 5 is that the enrichment to Florfenicol in certain Sewage Plant scene exposes experiment of the polarity organic pollution catcher is moved
Mechanics schematic diagram.
Fig. 6 is the polarity organic pollution catcher enrichment power to ofloxacin in certain Sewage Plant scene exposes experiment
Learn schematic diagram.
Detailed description of the invention
For being best understood from present disclosure, in conjunction with accompanying drawing and case study on implementation, the present invention is described further, but institute
The example of act is not limiting as protection scope of the present invention.
The present invention (polarity organic pollution catcher) carries out on-the-spot placement in Shanghai Sewage Plant and tests, and exists respectively
Take out after laying 1 day, 3 days, 5 days, 7 days, 14 days, 21 days and 28 days and carry out elution analysis.The present invention can be with Sync enrichment to ten
Multi-medicament class polar contaminants, and can be enriched to use the active method of sampling (Solid-Phase Extraction) to be enriched to
Organic substance.From the high five kinds of polar medicine sulfapyridines of the recall rate chosen, sulfamethoxazole, ketoprofen, Florfenicol and
The accumulation enriched concentration of ofloxacin it can be seen that this five kinds of pollutant can be the most shorter time in reach rich
Collection balance (referring to Figure of description 2,3,4,5,6).
Embodiment one: polarity organic pollution catcher is to the enrichment dynamic experiment of typical case's PPCPs medicine in water
Select large size city, Shanghai sewage treatment plant, water treatment technology section is laid a some position, by the sampling of the present invention
Device suspends and is placed in water, takes out respectively and carry out elution analysis after laying 1 day, 3 days, 5 days, 7 days, 14 days, 21 days and 28 days.
The present invention can with Sync enrichment to ten multi-medicament class polar contaminants, and can be enriched to use the active method of sampling
The Organic substance that (Solid-Phase Extraction) cannot be enriched to.From five kinds of polar medicine sulfapyridines, sulfalenes that the recall rate chosen is high
The accumulation enriched concentration (Fig. 2,3,4,5,6) of oxazole, ketoprofen, Florfenicol and ofloxacin is it can be seen that this five kinds of dirts
Enrichment balance is reached in the time that dye thing can be the most shorter.
Embodiment two: the broad spectrum activity absorption confirmatory experiment of polarity organic pollution catcher
28th day polarity organic pollution catcher in Example one, analyzes the polarity organic pollution of its absorption, and the
28 days on-the-spot water sampling 5L, use solid phase extraction method to carry out being enriched with, concentrate, measure after transporting laboratory back.And by two kinds of methods
The polarity organic pollution monitored compares.Solid-Phase Extraction and polarity organic pollution catcher method implement step pair
It is as shown in table 1 that when institute's examination goes out pollutant kind contrast difference's result.
The medicine pollutant inventory contrast that the examination of table 1 certain municipal wastewater treatment plant difference monitoring method institute is arrived
As can be seen from the above table, polarity organic pollution catcher sample pretreatment process is the simplest, and the dirt that can detect
Dye species is more.
Claims (4)
1. polarity organic pollution catcher in a water environment, it is characterised in that: this device includes two panels filter membrane, compound characteristics
Adsorbent, two rustless steel pressure rings and STAINLESS STEEL HEX SOCKET CAP SCREWS, described adsorbent is placed between two panels filter membrane, and filter membrane is placed
Between two pressure rings, together with two pressure rings are screwed with two panels filter membrane, form MULTILAYER COMPOSITE sandwich structure, compound
Feature adsorbent is in rustless steel compression ring internal ring middle position and will not flow out between compression ring and loses；Described compound spy
Levy adsorbent by polystyrene-divinylbenzene resin, ketopyrrolidine bonding polystyrene-divinylbenzene resin, at pyrrolidine
Ketonic bond close polystyrene-divinylbenzene resin on modified anion exchange groups, ketopyrrolidine bonding polystyrene-
Modified cation exchange group on divinylbenzene resins and five kinds of solid phase extraction adsorbentses of Graphon configure in proportion and
Become.
2. the polarity organic pollution catcher in water environment as described in claim 1, it is characterised in that: described filter membrane
Use the hydrophilic macromolecule permeable membrane of 0.45-1.0 μm pore diameter range.
3. the polarity organic pollution catcher in water environment as described in claim 1, it is characterised in that: described pressure ring
It is adopted as rustless steel.
4. the polarity organic pollution catcher in water environment as described in claim 1, it is characterised in that: described is compound
Feature adsorbent by polystyrene-divinylbenzene resin, ketopyrrolidine bonding polystyrene-divinylbenzene resin, pyrroles
Anion exchange groups, the polyphenyl second being bonded at ketopyrrolidine has been modified on the polystyrene-divinylbenzene resin of alkanone bonding
Modify cation exchange group on alkene-divinylbenzene resins and five kinds of solid phase extraction fillers of Graphon have been constituted after treatment
Mixed model solid phase extraction adsorbents, is then configured in proportion by the character of institute's monitoring objective pollutant and forms.
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| CN201610692412.5A CN106323689B (en) | 2016-08-22 | 2016-08-22 | Trace polar organic pollutant trap with water quality monitoring as guide |
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|---|---|---|---|
| CN201610692412.5A CN106323689B (en) | 2016-08-22 | 2016-08-22 | Trace polar organic pollutant trap with water quality monitoring as guide |
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| CN106323689B CN106323689B (en) | 2020-02-21 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106770300A (en) * | 2017-03-14 | 2017-05-31 | 常州市人居环境检测防治中心 | The device and monitoring method of underwater in-situ biological monitoring are carried out using various biologies |
| CN108760392A (en) * | 2018-07-16 | 2018-11-06 | 未名环境分子诊断（常熟）有限公司 | A kind of Passive sampler and the method for sampling for the acquisition of hydrophily organic pollution |
| CN109932462A (en) * | 2019-03-20 | 2019-06-25 | 河海大学 | Passive sampler and its method of sampling for polarity organic pollutant in water environment |
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