CN102735500A - Passive sampling technology aiming at anionic polar organic pollutant in water - Google Patents
Passive sampling technology aiming at anionic polar organic pollutant in water Download PDFInfo
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- CN102735500A CN102735500A CN2011100830085A CN201110083008A CN102735500A CN 102735500 A CN102735500 A CN 102735500A CN 2011100830085 A CN2011100830085 A CN 2011100830085A CN 201110083008 A CN201110083008 A CN 201110083008A CN 102735500 A CN102735500 A CN 102735500A
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Abstract
The invention discloses a novel passive sampling device and related technology for monitoring anionic polar organic pollutants in water by using an anion exchange resin as a receiving phase. The anion exchange resin is placed between two layers of polyether sulfone membranes, which are fixed by cyclic organic glass flanges and silicone pads. The device can be suspended in the water to carry out passive collection on anionic polar organic pollutants dissolved in the water. After the passive sampling, the sampler is cleaned and treated with freeze drying; then the resin receiving phase is moved out; and the sample is treated with fractional extraction by alkaliferous methanol; and the extracting solution is concentrated and analyzed by instrument. The simulation results show that the sampling device can effectively acquire anionic polar organic pollutants in the aqueous solution. Taking perfluorobutyric acid and perfluorohexanesulfonic acid for example, concentrations of the two substances increase linearly with time in the receiving phase of the sampler in certain period, and concentration in the receiving phase is higher than that of water environment by 3-4 orders of magnitude.
Description
Technical field
The present invention relates to a kind of with anion exchange resins for accepting phase, be used for gathering the passive sampling new equipment and the sample preparation technology of monitoring water body trace anion type polarity organic contaminant.
Technical background
Perfluorochemical in the environment water has destruction to human health and environmental ecology, for satisfying the environmental legislation requirement, ensureing human health and environmental ecology, must detect this pollutant in the environment water.Taking back the laboratory behind the spot sampling, to carry out the enrichment analysis be the most frequently used method of traditional environment water quality monitoring.Yet tradition initiatively sampling monitoring method is subject to many limitations, and like complex steps, expensive, and analysis result can only represent the moment situation, is not suitable for the bigger pollutant of concentration changes with time is monitored, for the easy omission of burst Pollution accident etc.The passive sampling technology can be collected monitored target substance under the prerequisite that does not influence mother solution concentration; Thereby the problems referred to above that can avoid tradition initiatively to exist in the sampling monitoring method; According to different collector structural designs, the concentration that is accumulated in the pollutant in the collector can truly reflect its equilibrium concentration or time average concentration in tested systems.The passive sampling technology has a good application prospect in the monitoring of pollutant and environmental process research; But mostly present passive sampling apparatus is that nonpolar organic contaminant or heavy metal pollutant design in order to gather, then actually rare to the passive sampling technical research of polarity organic contaminant.Having the researcher to set up with N-vinylpyrrolidone-divinylbenzene copolymer abroad is the passive sampling apparatus to polar medicine and organo-chlorine pesticide of accepting phase; This type passive sampling device is used the anti-phase principle polarity in the water body and nonpolar organic contaminant is gathered; But cost is comparatively high, and only in the passive sampling research of minority polar contaminants, reports to some extent.At present, still there is not report with the anionic organic contaminant passive sampling technology of ion-exchange mechanism exploitation.
Summary of the invention
It is passive sampling apparatus and the sample preparation technology thereof of accepting phase with anion exchange resins that the present invention aims to provide a kind of, thereby realizes the low-cost effectively passive sampling monitoring of anionic polarity organic contaminant in the water environment.
Anionic polarity organic contaminant passive sampling device structure provided by the invention is following: solid-phase adsorbent places between the two-layer poly (ether sulfone) film.Poly (ether sulfone) film can allow hydrophilic organics hydrophilicity to pass through, thereby it is adsorbed to be adsorbed agent as a semipermeability barrier between adsorbent and the environment, and trapped particles thing, organism and cross-sectional diameter are greater than the big molecule of 100nm simultaneously.Two-layer poly (ether sulfone) film is fixed through organic glass ring flange, silicagel pad and screw, nut seal, to prevent to accept loss mutually.Concrete parameter of this passive sampling apparatus and use and sample preparation mode are following:
1, the used acceptance of sampling thief is the dimethylaminomethyl/polystyrene weak anion exchange resin of Chemical Plant of Nankai Univ.'s production mutually, and the resin particle specific surface area is 500-550m
2/ g.The functional group dimethylaminomethyl of this resin can combine with carboxyl and sulfonic group effectively, thereby such target substance is effectively adsorbed.Resin carries out pre-service before use earlier, and concrete disposal route is following: resin is filled out post, use deionized water successively, and 1mol/L HCl, deionized water and 1mol/L KOH drip washing, the amount of bronsted lowry acids and bases bronsted lowry is 2 times of resin volumes, so triplicate.Use the continuous drip washing of methyl alcohol 3 times of 2 times of volumes again.With the resin oven dry, preserve subsequent use.
2, the used polyethersulfone diaphragm of sampling thief diameter is 47mm.The diaphragm preprocess method is following: place certain volume methyl alcohol to soak on diaphragm; The ratio of methyl alcohol volume and diaphragm quantity is the 20mL/ film, after 24 hours pad is transferred in the new methanol solution of equal volume, and after 24 hours, takes out and dry; Aluminium foil parcel with washed with methanol is crossed refrigerates subsequent use.
3, the used organic glass annular flange of sampling thief dish external diameter 70mm, internal diameter 37mm, disc thickness 3mm, sampling thief effective surface area 13.69cm
2(as shown in Figure 1).The pretreatment mode of ring flange is following: ring flange washes 3 times with tap water and ultrapure water respectively, uses washed with methanol behind the removal surface impurity, dries the back and wraps up subsequent use with aluminium foil.Sampling thief used silica gel pad external diameter 70mm, internal diameter 37mm, spacer thickness 1mm.The pretreatment mode of silica gel pad is following: after pad washes 3 times with tap water and ultrapure water respectively; Place to contain 50% methanol in water and soak, after 24 hours pad is transferred in the pure methanol solution, and after 24 hours, takes out and dry; Aluminium foil parcel with washed with methanol is crossed refrigerates subsequent use.
4, weighing 30mg (dry weight) weak anion exchange resin places between the two-layer polyethersulfone diaphragm, and adopts silica gel pad and ring flange that diaphragm is fixed.The passive sampling apparatus structure that ring flange, pad, poly (ether sulfone) film and resin are formed is as shown in Figure 2.With this device hang on to carry out in the water body of passive sampling monitoring, can realize passive sampling monitoring to anionic polarity organic contaminant in the water body.
5, wash-out: sampling thief is accepted to find that only use methyl alcohol as eluant, eluent, the recovery is lower when upward the anionic target compound of collection carries out wash-out mutually.Wash-out for weak anionic; Often in solvent, add a certain amount of acid or alkali to improve elute effect; Therefore on the basis of selecting methyl alcohol as basic eluant, eluent, examined or check the influence of adding behind weak acid, strong acid, weak base and the highly basic anionic target compound elute effect.Elute effect through more different eluant, eluents finds that the methanol solution that contains 0.5%KOH has good elute effect as eluent.With compound perfluoro caprylic acid and perfluorooctane sulfonate is example, and the methyl alcohol that contains 0.5%KOH can reach more than 88% 3 wash-out recovery of these 2 kinds of target compounds.
Description of drawings
The fixing ring flange synoptic diagram of using of Fig. 1 passive sampling apparatus
Fig. 2 passive sampling apparatus structural representation
Fig. 3 passive sampling apparatus in 7 days to the WS in the collection effect of perfluorobutyric acid (PFBA, concentration 5 μ g/L)
Fig. 4 passive sampling apparatus in 7 days to the WS in the collection effect of the own sulfonic acid of perfluor (PFHxS, concentration 5 μ g/L)
Embodiment
For better understanding content of the present invention, through embodiment the present invention is further described below, but the example of being lifted does not limit protection scope of the present invention.
Embodiment 1: contain perfluorobutyric acid (PFBA) and the own sulfonic acid of perfluor (PFHxS) concentration is respectively in the WS of 5 μ g/L at 4L, put into 1 piece of anion exchange resins passive sampling apparatus, make it to hang on and carry out passive sampling in the WS.Finish sampling after 12 hours, use the flushing with clean water sampling thief, and with the sampling thief freeze drying with the removal residual moisture.After the freeze-drying, open sampling thief, anion exchange resins is accepted phase transfer to the 15mL polypropylene centrifuge tube, and containing the methanol solution 10mL of 0.5%KOH, in 30 ℃ of following constant-temperature shaking wash-outs 3 times, each 1 hour.Collect 3 times eluent, nitrogen blows to nearly dry doubling constant volume.
Recording sampling thief internal object compound concentrations is: 2.6 μ g/g (PFBA) and 2.4 μ g/g (PFHxS).
Embodiment 2: in the system identical with routine 1, carry out 24 hours passive sampling experiment.The sampling thief sample treatment is identical with example 1.Recording sampling thief internal object compound concentrations is: 5.1 μ g/g (PFBA) and 2.6 μ g/g (PFHxS).
Embodiment 3: in the system identical with routine 1, carry out 48 hours passive sampling experiment.The sampling thief sample treatment is identical with example 1.Recording sampling thief internal object compound concentrations is: 10.0 μ g/g (PFBA) and 3.0 μ g/g (PFHxS).
Embodiment 4: in the system identical with routine 1, carry out 96 hours passive sampling experiment.The sampling thief sample treatment is identical with example 1.Recording sampling thief internal object compound concentrations is: 21.0 μ g/g (PFBA) and 5.3 μ g/g (PFHxS).
Embodiment 5: in the system identical with routine 1, carry out 168 hours passive sampling experiment.The sampling thief sample treatment is identical with example 1.Recording sampling thief internal object compound concentrations is: 28.0 μ g/g (PFBA) and 9.5 μ g/g (PFHxS).
More than implementing illustration shows; In this experimental system; Be in linear the rising (Fig. 3) in (96 hours) at preceding 4 days to perfluorobutyric acid (PFBA) quantity, and the own sulfonic acid of perfluor (PFHxS) quantity that the passive sampling device is gathered all was linear ascendant trend (Fig. 4) on the whole in 7 days.For these two kinds of anionic polarity organic contaminants, this passive sampling apparatus can both be realized effective collection.
Claims (4)
1. the invention provides a kind of is passive sampling apparatus and the sampling thief sample treatment of accepting phase with anion exchange resins, and this device and sample treatment can be used for the anionic polarity organic contaminant in the enrichment monitoring water body.
2. the passive sampling device structure in the right 1 is: anion exchange resins is positioned between the two-layer circular polyethersulfone diaphragm, and with ring-type organic glass ring flange and silicagel pad diaphragm is fixed.
3. the passive sampling device structural parameters described in the right 2 are following:
(1) the used acceptance of sampling thief is dimethylaminomethyl/polystyrene weak anion exchange resin mutually, and specific surface area is 500-550m
2/ g, the resin quality that single sampling thief uses is 30mg.
(2) the used polyethersulfone circular film of sampling thief diameter is 47mm.
(3) used organic glass ring flange of sampling thief and silica gel pad are external diameter 70mm, the tubular shape of internal diameter 37mm, and single flange disc thickness is 3mm, the effective surface area of single sampling thief is 13.69cm
2, the ratio of the amount of sampling thief surface area and adsorbent is 456cm
2/ g.
4. the sampling thief sample treatment in the right 1 is: use the methyl alcohol that contains highly basic that the resin of sampling thief is accepted repeatedly to vibrate mutually extraction, analyze after repeatedly the extract merging concentrates.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104729878A (en) * | 2013-12-24 | 2015-06-24 | 南开大学 | Novel passive water body sampling technique based on supported ionic liquid |
| CN105417617A (en) * | 2015-12-21 | 2016-03-23 | 浙江大学 | Passive adsorption sampling device for organic pollutants in water body |
| CN106323689A (en) * | 2016-08-22 | 2017-01-11 | 中国食品发酵工业研究院 | Water quality monitoring-orientated polar organic trace pollutant trap |
| CN107219344A (en) * | 2017-06-02 | 2017-09-29 | 南开大学 | A kind of method for predicting PAHs in soil biological effectiveness |
| CN108507830A (en) * | 2018-07-16 | 2018-09-07 | 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 nonpolar organic pollutants acquisition in sewer |
| 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 |
| CN108837816A (en) * | 2018-07-16 | 2018-11-20 | 未名环境分子诊断（常熟）有限公司 | A kind of adsorbent material for acquisition polarity organic pollutant in water environment passive sampling |
| 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 |
| CN110108809A (en) * | 2019-04-29 | 2019-08-09 | 南京大学 | A kind of measuring method of essence crudefiber crop drug |
| CN111659358A (en) * | 2020-06-11 | 2020-09-15 | 南京大学 | DGT adsorption membrane, preparation method thereof and method for monitoring perfluoro and polyfluoro compounds based on DGT technology |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104729878A (en) * | 2013-12-24 | 2015-06-24 | 南开大学 | Novel passive water body sampling technique based on supported ionic liquid |
| CN105417617A (en) * | 2015-12-21 | 2016-03-23 | 浙江大学 | Passive adsorption sampling device for organic pollutants in water body |
| CN105417617B (en) * | 2015-12-21 | 2018-05-29 | 浙江大学 | A kind of passive adsorption sampling apparatus for Organic Pollutants In Water |
| CN106323689A (en) * | 2016-08-22 | 2017-01-11 | 中国食品发酵工业研究院 | Water quality monitoring-orientated polar organic trace pollutant trap |
| CN106323689B (en) * | 2016-08-22 | 2020-02-21 | 中国食品发酵工业研究院有限公司 | Trace polar organic pollutant trap with water quality monitoring as guide |
| CN107219344A (en) * | 2017-06-02 | 2017-09-29 | 南开大学 | A kind of method for predicting PAHs in soil biological effectiveness |
| 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 |
| CN108837816A (en) * | 2018-07-16 | 2018-11-20 | 未名环境分子诊断（常熟）有限公司 | A kind of adsorbent material for acquisition polarity organic pollutant in water environment passive sampling |
| CN108507830A (en) * | 2018-07-16 | 2018-09-07 | 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 nonpolar organic pollutants acquisition in sewer |
| CN108837816B (en) * | 2018-07-16 | 2020-11-20 | 未名环境分子诊断（常熟）有限公司 | Adsorbing material for collecting polar organic pollutants in passive sampling of water environment |
| CN108507830B (en) * | 2018-07-16 | 2024-03-26 | 未名环境分子诊断（常熟）有限公司 | Passive sampler and sampling method for collecting nonpolar organic pollutants in sewer |
| 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 |
| CN110108809A (en) * | 2019-04-29 | 2019-08-09 | 南京大学 | A kind of measuring method of essence crudefiber crop drug |
| CN110108809B (en) * | 2019-04-29 | 2021-09-28 | 南京大学 | Method for measuring fine sesame drugs |
| CN111659358A (en) * | 2020-06-11 | 2020-09-15 | 南京大学 | DGT adsorption membrane, preparation method thereof and method for monitoring perfluoro and polyfluoro compounds based on DGT technology |
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Application publication date: 20121017 |