CN101900646B - Rapid sampler of micro polycyclic aromatic hydrocarbon in water based on electrospinning nano-fiber membrane - Google Patents
Rapid sampler of micro polycyclic aromatic hydrocarbon in water based on electrospinning nano-fiber membrane Download PDFInfo
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- CN101900646B CN101900646B CN2010102376158A CN201010237615A CN101900646B CN 101900646 B CN101900646 B CN 101900646B CN 2010102376158 A CN2010102376158 A CN 2010102376158A CN 201010237615 A CN201010237615 A CN 201010237615A CN 101900646 B CN101900646 B CN 101900646B
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Abstract
A fast sampler of trace polycyclic aromatic hydrocarbons in water based on an electro spinning nano fiber membrane is disclosed. The invention relates to a water quality monitoring device, provides an adsorption sampler of polycyclic aromatic hydrocarbon based on an electro spinning lactic acid-caprolactone nano fiber membrane. In the sampler, a water collection sleeve is fixed with a membrane supporting sleeve, a check valve is arranged at the lower part of the water collection sleeve and is connected with a sampling needle and the membrane supporting sleeve, the water collection sleeve can be externally connected with a polytetrafluoroethylene sampling tube to discharge water, the outer wall of the membrane supporting sleeve is used for fixing the fiber membrane to adsorb the polycyclic aromatic hydrocarbon in the water, a water diversion bin is arranged at the bottom of the membrane supporting sleeve, the bottom of the membrane supporting sleeve is connected with the check valve, and a pulling piston is used for sucking a water sample and transports the water sample to the water collection sleeve to be contacted with the fiber membrane. The electro spinning lactic acid-caprolactone nano fiber membrane for matching is prepared through a high-voltage electrostatic spinning method. The sampler has the advantages that sampling, adsorption enrichment and solvent desorption are synchronously carried out, and easy to control, water samples before and after enrichment are respectively stored without mutual interference, the manual operation is adopted without matching equipment; the adsorption ability of the fiber membrane is strong, and the selectivity of different pollutants can be realized by changing different fiber membranes, the structure is simple and the operation is convenient, and the fiber membrane is easy to disassemble.
Description
Technical field
The present invention relates to a kind of palycyclic aromatic absorption type sampling thief, belong to micro polluted source environmental monitoring field and laboratory study field based on electrospinning PLA-caprolactone nano fibrous membrane.
Background technology
(Polycyclic Aromatic Hydrocarbons, the volatile hydrocarbon that produces when PAHs) being rough burnings such as coal, oil, timber and macromolecular compound is important environment and food contaminant to palycyclic aromatic.Among more than the 200 kind of PAHs that has found so far, there is quite a few to have carcinogenicity, as benzo [α] pyrene, benzo [α] anthracene etc.PAHs is distributed widely in the environment, and human external environment such as atmosphere all contain various PAHs to some extent in soil and the water.But PAHs is polluted-water also, can constantly accumulate by the food chain of marine alga, shellfish, mollusc and fish composition, and finally shift to human body, causes a series of endocrines to be disturbed and carcinogenic, teratogenesis, mutagenic effect.
Correlative study shows that PAHs's is dense in the water body of growing near city and integrated mill.Even in micro-polluted source water and underground water away from the area, industrial center, PAHs also has certain concentration level.These pollute mainly is because PAHs moves at a distance, the plant of rotting is residual, and organic substance causes in the factors such as effect of soil microorganism.PAHs can not be underestimated as the damaging effect of environmental contaminants in water, and the popularity of its existence has also caused it to remove and improvement becomes an arduous challenge.
In order further the distribution of PAHs, migration to be transformed and treatment technology carries out research and analysis, in the micro-polluted water and the analysis that the PAHs in the simulated wastewater carries out rapidly and efficiently under the laboratory condition be a technical barrier.Also lack efficient effective method for the PAHs sampling in the environmental analysis experiment and in the micro-polluted source water at present.Using at present is a kind of solid phase extraction (Solid-Phase Extraction more widely, SPE), it is developed recently a kind of sample pretreatment technology of getting up, by the development that combines of liquid-solid extraction and liquid chromatography technology, be mainly used in separation, the purifying and concentrated of sample, compare with traditional liquid-liquid extraction method and can improve the recovery of analyte, more effective analyte is separated with interfering component, reduce the sample pretreatment process.The SPE great majority are used for handling liquid samples, extraction, concentrate and purify wherein half volatile and involatile compound.Be mainly used in organic substance analysis in the water at present, agricultural chemicals and herbicide residue analysis in fruit, vegetables and the food, microbiotic analysis, aspects such as clinical medicine analysis.Common SPE device is made up of column jecket, sintering pad, filler, vacuum system, vacuum pump, blow-dry device, inertia source of the gas, high volume sampler and surge flask, complex structure, complex operation.And because SPE column filling complexity, cost of manufacture is higher, need expend a large amount of organic solvents during operation, so economy is not good enough.
In recent years, according to the sampling characteristics innovation and creation of different field multiple Liquid sampler.But owing to can not realize the in-situ treatment of water sample, cause the enrichment and the extraction process of underwater micro-organic matter numerous and diverse, processing cost height, low, the poor reproducibility of efficient.
Summary of the invention
The object of the present invention is to provide a kind of based on electrospinning PLA-caprolactone (P (LA/CL), 7/3) the palycyclic aromatic absorption type sampling thief of nano fibrous membrane, it can realize the in-situ enrichment to palycyclic aromatic in the simulated wastewater under micro-polluted water or the laboratory condition, simple in structure, easy operation, and cheap.
The technical solution adopted in the present invention is:
The micro polycyclic aromatic hydrocarbon sampling thief comprises the sleeve I that catchments, film carrier sleeve II and lifts piston I II; Wherein, the sleeve I open top of catchmenting has internal thread and film carrier sleeve II to fix.The sleeve I bottom of catchmenting is provided with a water inlet retaining valve and connects sampling syringe needle and film carrier sleeve II, and the middle and upper part outer wall is provided with two apopores, and is connected in total water delivering orifice cock with stainless-steel tube, is used for external teflon sampling pipe.Film carrier sleeve II outer wall is used for fixing palycyclic aromatic in the tunica fibrosa planar water.Film carrier sleeve II top has opening, and barrel has the external thread and the sleeve I that catchments to fix.The bottom is provided with watershed storage 8, and watershed storage center upper portion opening directly penetrates the catchment retaining valve of sleeve I of watershed storage 8 and bottom and links to each other.Watershed storage 8 top both-side openings are communicated with the watershed storage outer wall through going out water one-way valve, make the interior water sample of film carrier sleeve II can unidirectionally export the sleeve I that catchments to.Lifting piston I II is used to draw water sample and it is delivered to the sleeve I that catchments and contact with tunica fibrosa.
Wherein, above-mentioned tunica fibrosa is electrospinning PLA-caprolactone (P (LA/CL)) nano fibrous membrane, prepares with the high-voltage electrostatic spinning method.Concrete preparation method is: take by weighing 1.2 gram molecular weights and be PLA-caprolactone (P (LA/CL)) particle of 100,000, be dissolved in the 20 gram methylene chloride, concussion is to dissolving.This solution is inserted the high-voltage electrostatic spinning device, and described electrostatic spinning apparatus comprises DC high-voltage power supply, and spinning head receives flat board, at 12 kilovolts, carries out the operation of electrospinning silk under 15 centimetres of conditions of utmost point target spacing, and the gained tunica fibrosa is deposited on dash receiver.After spinning about 3 hours, stop spinning, tunica fibrosa is taken off standby.
Also can make following various optimal design:
Wherein, the synthetic ratio of PLA and polycaprolactone is 7: 3 in PLA-caprolactone material.
The film carrier sleeve adopts fixedly electricity spinning fibre film of semi-circular magnet.
The tunica fibrosa fibre diameter is distributed between 200～800 nanometers mostly, and film thickness is 0.3 millimeter, is beneficial to palycyclic aromatic in the planar water.
The sleeve that catchments has identical water sample capacity with the film carrier sleeve, but equivalent sucks or emptying.
Catchment sleeve and film carrier sleeve all adopts barrier film micro one-way valve design, prevents that water sample from flowing backwards.
The sleeve that catchments, film carrier sleeve and lift piston and be stainless steel, corrosion-resistant, no adsorptive hindrance influences.
The palycyclic aromatic concentration range is in 1～5 micrograms per litre in the water sample that the sleeve I bottom sampling syringe needle that catchments is drawn.
Compared with prior art, the invention has the advantages that:
1, sampling, adsorption and enrichment, solvent desorption can carry out synchronously;
2, sampling quantity and sample frequency are easy to control;
3, before the enrichment after water sample and the enrichment water sample respectively at storing no phase mutual interference in catchment sleeve and the film carrier sleeve;
4, support equipments such as needing no vacuum pump, power supply, Solid-Phase Extraction support manually can be operated;
5, tunica fibrosa high adsorption capacity is changed different tunica fibrosas and can be realized different pollutant selectivity;
6, simple in structure, easy to operate, be easy to dismounting, tunica fibrosa can be changed rapidly.
Description of drawings
Fig. 1 is a decomposition texture synoptic diagram of the present invention;
Among the figure: the I-sleeve that catchments; II-film carrier sleeve; III-lifts piston; The total water delivering orifice cock of 1-; The 2-internal thread of sleeve that catchments; The 3-retaining valve; The 4-sleeve watershed storage that catchments; 5-film carrier sleeve closing handle; 6-film carrier sleeve external thread; The 7-annular recess; 8-film carrier sleeve watershed storage; 9-lifts the piston handle; 10-lifts the piston scale mark.
Fig. 2 is the assembled state figure of Fig. 1;
Fig. 3 is the operating position synoptic diagram of Fig. 1;
Fig. 4 is the scanning electron microscope image of electrospinning PLA-caprolactone (P (LA/CL)) tunica fibrosa.
Embodiment
The present invention will be further described below in conjunction with accompanying drawing.
As shown in the figure, a possible embodiments of the present invention, the micro polycyclic aromatic hydrocarbon sampling thief has the sleeve of catchmenting I, and the sleeve I open top of catchmenting has internal thread 2 and film carrier sleeve II to fix.The sleeve I bottom of catchmenting is provided with a water inlet retaining valve 3 and connects sampling syringe needle and film carrier sleeve II, and the middle and upper part outer wall is provided with two apopores, and is connected in total water delivering orifice cock 1 with stainless-steel tube, can external teflon sampling pipe.Film carrier sleeve II outer wall has annular recess 7 to be used for fixing palycyclic aromatic in the tunica fibrosa planar water.Open top, barrel have external thread 6 can manually rotate closing handle 5 and the sleeve that catchments is fixed.The bottom is provided with watershed storage 8, and watershed storage 8 center upper portion openings directly penetrate the catchment retaining valve 3 of sleeve I of watershed storage 8 and bottom and link to each other.Watershed storage 8 top both-side openings are communicated with the watershed storage outer wall through going out water one-way valve 3, make the interior water sample of film carrier sleeve II can unidirectionally export the sleeve I that catchments to.Lifting piston I II is used to draw water sample and it is delivered to the sleeve that catchments and contact with tunica fibrosa.Lift piston outer wall and scale mark 10 is arranged with the control sampling volume.
During assembling, earlier 125 millimeters * 170 millimeters tunica fibrosa is coated on film carrier sleeve II outer wall, with four magnetic semicircular ring at annular recess 7 clamped fibers films.Then the outlet at bottom of film carrier sleeve II is aimed at the sleeve I outlet at bottom that catchments, screw internal and external threads with closing handle 5 and be fixed in the sleeve that catchments.To lift piston I II directly inserts in the film carrier sleeve II.Total water delivering orifice cock is the teflon drain pipe fixedly; The outlet of Water collecting cover tube bottom connects the 8# syringe needle, can use.
During sampling, will lift piston I II earlier and shift the end onto, and syringe needle be inserted the solution of waiting to sample pull out with carrying handle 9 and lift piston to scale mark 10 positions.Water sample is sucked film carrier sleeve II.Push and lift piston I II, water sample is pushed the interlayer of catchment sleeve I and film carrier sleeve II, absorption is 5 minutes on tunica fibrosa.Sample once more as need, repeat above action.After treating that water sampling is finished, syringe needle is inserted hplc grade methanol solution, suck methyl alcohol, shook the palycyclic aromatic that adsorbs on the desorb film 3 minutes to the sleeve II that catchments.After desorb is finished, push piston I II, the palycyclic aromatic methanol solution is gone out water cock 1 output and preservation through always.
Wherein, described tunica fibrosa is electrospinning PLA-caprolactone (P (LA/CL)) nano fibrous membrane, prepare with the high-tension electricity spin processes, concrete preparation method is: take by weighing 1.2 gram molecular weights and be PLA-caprolactone (P (LA/CL)) particle of 100,000, be dissolved in the 20 gram methylene chloride, concussion is to dissolving, this solution is inserted the high-tension electricity device for spinning, at 12 kilovolts, carry out the operation of electrospinning silk under 15 centimetres of conditions of utmost point target spacing, the gained tunica fibrosa is deposited on receiver sheet, spins after 3 hours, stop spinning, tunica fibrosa is taken off standby.In this embodiment, the synthetic ratio of PLA and polycaprolactone is 7: 3 in PLA-caprolactone material.
Embodiment 1
Use palycyclic aromatic absorption type sampling thief that simulated water sample (containing fluorenes 1 micrograms per litre, luxuriant and rich with fragrance 1 micrograms per litre, anthracene 1 micrograms per litre, fluoranthene 1 micrograms per litre, pyrene 1 micrograms per litre) is carried out sampling analysis.1000 milliliters of sampling quantities back and forth extract 8 times, and water sample was stopped 5 minutes in the sleeve that catchments, and slight concussion.After sampling finishes, with 50 ml methanol desorbs 3 minutes.Measure through high performance liquid chromatography (DIONEX U3000, the U.S.), this method to the recovery of five kinds of palycyclic aromatics is respectively: fluorenes 86.4%, phenanthrene 90.4%, anthracene 89.5%, fluoranthene 87.8%, pyrene 87.8%.
Use palycyclic aromatic absorption type sampling thief that simulated water sample (containing fluorenes 2 micrograms per litre, luxuriant and rich with fragrance 2 micrograms per litre, anthracene 2 micrograms per litre, fluoranthene 2 micrograms per litre, pyrene 2 micrograms per litre) is carried out sampling analysis.500 milliliters of sampling quantities back and forth extract 4 times, and water sample was stopped 5 minutes in the sleeve that catchments, and slight concussion.After sampling finishes, with 50 ml methanol desorbs 3 minutes.Through high-performance liquid chromatogram determination, this method to the recovery of five kinds of palycyclic aromatics is respectively: fluorenes 85.6%, phenanthrene 90%, anthracene 88.9%, fluoranthene 84.2%, pyrene 88.9%.
Embodiment 3
Use palycyclic aromatic absorption type sampling thief that simulated water sample (containing fluorenes 3 micrograms per litre, luxuriant and rich with fragrance 3 micrograms per litre, anthracene 3 micrograms per litre, fluoranthene 3 micrograms per litre, pyrene 3 micrograms per litre) is carried out sampling analysis.2000 milliliters of sampling quantities back and forth extract 15 times, and water sample was stopped 5 minutes in the sleeve that catchments, and slight concussion.After sampling finishes, with 50 ml methanol desorbs 3 minutes.Through high-performance liquid chromatogram determination, this method to the recovery of five kinds of palycyclic aromatics is respectively: fluorenes 82.1%, phenanthrene 84.8%, anthracene 83.5%, fluoranthene 88.7%, pyrene 87.5%.
Embodiment 4
Use palycyclic aromatic absorption type sampling thief that simulated water sample (containing fluorenes 4 micrograms per litre, luxuriant and rich with fragrance 4 micrograms per litre, anthracene 4 micrograms per litre, fluoranthene 4 micrograms per litre, pyrene 4 micrograms per litre) is carried out sampling analysis.1500 milliliters of sampling quantities back and forth extract 12 times, and water sample was stopped 5 minutes in the sleeve that catchments, and slight concussion.After sampling finishes, with 50 ml methanol desorbs 3 minutes.Through high-performance liquid chromatogram determination, this method to the recovery of five kinds of palycyclic aromatics is respectively: fluorenes 84.3%, phenanthrene 83.8%, anthracene 86.5%, fluoranthene 89.7%, pyrene 84.5%.
Use palycyclic aromatic absorption type sampling thief that simulated water sample (containing fluorenes 5 micrograms per litre, luxuriant and rich with fragrance 5 micrograms per litre, anthracene 5 micrograms per litre, fluoranthene 5 micrograms per litre, pyrene 5 micrograms per litre) is carried out sampling analysis.1000 milliliters of sampling quantities back and forth extract 8 times, and water sample was stopped 5 minutes in the sleeve that catchments, and slight concussion.After sampling finishes, with 50 ml methanol desorbs 3 minutes.Through high-performance liquid chromatogram determination, this method to the recovery of five kinds of palycyclic aromatics is respectively: fluorenes 80.4%, phenanthrene 86.9%, anthracene 84.1%, fluoranthene 84.4%, pyrene 83.4%.
Claims (8)
1. a micro polycyclic aromatic hydrocarbon sampling thief is characterized in that: comprise the sleeve that catchments (I), film carrier sleeve (II) and lift piston (III); Wherein, the sleeve that catchments (I) top has opening, has internal thread and film carrier sleeve (II) fixing; Sleeve (I) bottom of catchmenting is provided with a water inlet retaining valve and connects sampling syringe needle and film carrier sleeve (II), and the middle and upper part outer wall is provided with two apopores, and is connected in total water delivering orifice cock with stainless-steel tube, is used for external teflon sampling pipe; Film carrier sleeve (II) outer wall is used for fixing palycyclic aromatic in the tunica fibrosa planar water, film carrier sleeve (II) top has opening, barrel has external thread fixing with the sleeve (I) that catchments, the bottom is provided with watershed storage (8), watershed storage center upper portion opening directly penetrates the catchment retaining valve of sleeve (I) of watershed storage (8) and bottom and links to each other, watershed storage (8) top both-side opening is communicated with the watershed storage outer wall through going out water one-way valve, makes the interior water sample of film carrier sleeve (II) can unidirectionally export the sleeve that catchments (I) to; Lift piston (III) and be used to draw water sample and it is delivered to the sleeve that catchments (I) and contact with tunica fibrosa, described tunica fibrosa is electrospinning PLA-caprolactone nano fibrous membrane.
2. micro polycyclic aromatic hydrocarbon sampling thief according to claim 1, wherein, described tunica fibrosa is electrospinning PLA-caprolactone (P (LA/CL)) nano fibrous membrane, prepare with the high-tension electricity spin processes, concrete preparation method is: take by weighing 1.2 gram molecular weights and be PLA-caprolactone (P (LA/CL)) particle of 100,000, be dissolved in the 20 gram methylene chloride, concussion is to dissolving, this solution is inserted the high-tension electricity device for spinning, at 12 kilovolts, carries out the operation of electrospinning silk under 15 centimetres of conditions of utmost point target spacing, the gained tunica fibrosa is deposited on receiver sheet, after spinning about 3 hours, stop spinning, tunica fibrosa is taken off standby.
3. micro polycyclic aromatic hydrocarbon sampling thief as claimed in claim 2, wherein, the fibre diameter of described nano fibrous membrane is between 200～800 nanometers, and film thickness is 0.3 millimeter.
4. micro polycyclic aromatic hydrocarbon sampling thief described in claim 1, it is characterized in that: the sleeve that catchments has identical water sample capacity with the film carrier sleeve.
5. micro polycyclic aromatic hydrocarbon sampling thief as claimed in claim 1 is characterized in that: catchment sleeve and film carrier sleeve all adopt the infuse non-return operation of barrier film micro one-way valve.
6. micro polycyclic aromatic hydrocarbon sampling thief as claimed in claim 1 is characterized in that: the sleeve that catchments, film carrier sleeve and lift piston and be stainless steel.
7. micro polycyclic aromatic hydrocarbon sampling thief as claimed in claim 1 is characterized in that: the film carrier sleeve adopts fixedly electricity spinning fibre film of semi-circular magnet.
8. micro polycyclic aromatic hydrocarbon sampling thief as claimed in claim 1 is characterized in that: the palycyclic aromatic concentration range is in 1～5 micrograms per litre in the water sample that the sleeve that catchments (I) bottom sampling syringe needle is drawn.
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| CN103197087B (en) * | 2012-01-09 | 2014-03-19 | 北京瑞利分析仪器有限公司 | Automatic sampler sampling needle used for strong acidic solution |
| CN103759976B (en) * | 2014-01-28 | 2015-11-11 | 中国地质科学院水文地质环境地质研究所 | Mouth of pipe reducing plug-in type sampling instrument |
| CN103759972B (en) * | 2014-01-28 | 2015-11-11 | 中国地质科学院水文地质环境地质研究所 | Organic Pollution water sample pump line mouth sampling thief |
| CN103743598B (en) * | 2014-01-28 | 2015-10-28 | 中国地质科学院水文地质环境地质研究所 | Organic Pollution water sample negative pressure sampler |
| CN104458341B (en) * | 2014-12-03 | 2018-08-10 | 中国环境科学研究院 | A kind of portable case type solid-phase extraction device and method can be used for natural water sampling |
| CN106669446A (en) * | 2017-01-06 | 2017-05-17 | 宁波大学 | SVOCs solid-phase extraction membrane |
| CN107219344A (en) * | 2017-06-02 | 2017-09-29 | 南开大学 | A kind of method for predicting PAHs in soil biological effectiveness |
| CN109374343B (en) * | 2018-11-29 | 2023-09-15 | 中国科学院武汉岩土力学研究所 | In-situ water sample collecting probe and collecting method for shallow gas-containing stratum |
| CN109556924A (en) * | 2018-12-28 | 2019-04-02 | 河海大学 | A kind of acquisition method and device of multi-layer Soil water sample |
| CN112834282B (en) * | 2021-01-15 | 2023-01-06 | 山东初行环保科技有限公司 | Soil solution extractor for ecological environment detection |
| CN115508475A (en) * | 2022-11-01 | 2022-12-23 | 未名环境分子诊断(广东)有限公司 | Method for detecting content of diphenoxylate in sewage |
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| DE4316690C2 (en) * | 1993-05-14 | 1996-02-15 | Dankwart Klein Erdbohrungen Gm | Probe for the quantitative detection of pollutants in groundwater |
| JP2000249633A (en) * | 1999-02-26 | 2000-09-14 | Isuzu Motors Ltd | Analysis pretreatment method for polycyclic aromatic hydrocarbons in diesel engine particles |
| US7407568B1 (en) * | 2002-11-08 | 2008-08-05 | University Of South Florida | Method of using sol-gel coatings for on-line preconcentration of amino acids in capillary electrophoresis |
| CN100504377C (en) * | 2007-02-05 | 2009-06-24 | 同济大学 | Extraction purifying measuring method of polycyclic aromatic hydrocarbons in soil |
| CN101407803B (en) * | 2008-07-01 | 2011-04-06 | 北京师范大学 | Polylactic acid electrospinning fibre immobilized laccase and preparation thereof |
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