CN103969235A - Quick pre-warning method for organic pollution of surface water - Google Patents

Quick pre-warning method for organic pollution of surface water Download PDF

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CN103969235A
CN103969235A CN201410180587.9A CN201410180587A CN103969235A CN 103969235 A CN103969235 A CN 103969235A CN 201410180587 A CN201410180587 A CN 201410180587A CN 103969235 A CN103969235 A CN 103969235A
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water
standard
water sample
sample
concentrated
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CN103969235B (en
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李军
陈飞
肖倩倩
周昀
刘流
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Zhejiang University of Technology ZJUT
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Zhejiang University of Technology ZJUT
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Abstract

The invention relates to a quick pre-warning method for organic pollution of surface water. The pre-warning method comprises the following steps: (1) collecting surface water as raw water; (2) filtering the raw water through a micro-pore filter film; (3) taking 1-1.5 L of the filtered water sample for concentration through a reverse osmosis device to obtain the concentrated water sample; (4) taking the concentrated water sample obtained in step (3) into a fluorescent cuvette, and placing into a sample cell in a fluorescence spectrophotometer for three-dimensional fluorescence spectrum scan to obtain the three-dimensional fluorescence spectra of the concentrated water sample; (5) preparing the standard water sample according to the toplimit of the Standard of Drinking Water, and obtaining a standard spectra after concentration through the reverse osmosis device and scan through three-dimensional fluorescence; (6) comparing the standard spectra with the three-dimensional fluorescence spectra of the water sample. If the fluorescence intensity of the three-dimensional fluorescence spectra of the water sample is less than or equal to that of the standard spectra, the organic pollution of the surface water is confirmed to be under the standard; whereas, the organic pollution of the surface water is confirmed to exceed the standard. The pre-warning method is quick, convenient, easy to operate and high in efficiency.

Description

A kind of quick method for early warning of surface water organic contamination
Technical field
The invention belongs to water quality monitoring field, especially a kind of detection method of surface water organic contamination.
Technical background
Along with human society is industrialized, develop rapidly, a large amount of pollutants are discharged in water environment.Organic contaminant is large with its toxicity, and conventional method is difficult to the features such as removal, has caused great potential safety hazard to the mankind's drinking-water.In order to ensure the people's safe drinking water, the Ministry of Public Health and national standardization management committee combine and have issued new mandatory national < < drinking water sanitary standard > > (GB5749-2006), in indices, 53 organic compounds in toxicity index, have been contained.If each organic contaminant is tested, although the existing conventional physics and chemistry means in laboratory can record various organic concentration quantitatively, however practical operation inefficiency, and consuming time longer, be difficult to play the effect to organic contaminant early warning.
Summary of the invention
In order to overcome the troublesome poeration of the detection mode of existing surface water organic contamination, long, deficiency that work efficiency is low consuming time, the invention provides the quick method for early warning of a kind of easy to operate, rapid and convenient, high efficiency surface water organic contamination.
The technical solution used in the present invention is:
A quick method for early warning for surface water organic contamination, said method comprising the steps of:
(1) gather surface water as former water;
(2) by miillpore filter, filter and gather the former water of coming, hold back gravel, mud and clay particle in former water;
(3) get the water sample 1-1.5L after filtration, concentrated through reverse osmosis unit, the water sample after being concentrated;
(4) get the water sample of step (3) after concentrated in fluorescence cuvette, the sample cell that is placed in fluorospectrophotometer carries out three-dimensional fluorescence spectrum scanning, obtains the three-dimensional fluorescence collection of illustrative plates of water sample;
(5) according to the upper limit of < < drinking water standard > >, prepare standard water sample, concentrated through reverse osmosis unit, same through three-dimensional fluorescence scanning, obtain standard diagram;
(6) the three-dimensional fluorescence collection of illustrative plates of the water sample of described standard diagram and step (4) is compared, if the fluorescence intensity of the three-dimensional fluorescence collection of illustrative plates of water sample is less than or equal to the fluorescence intensity of described standard diagram, judge that surface water organic contamination does not exceed standard; Otherwise, judge that surface water organic contamination exceeds standard.
Further, the cycles of concentration of the water sample of the concentrated multiple of described step (5) Plays water sample after filtering with step (3) is identical.
Technical conceive of the present invention is: at normal temperatures, most molecule is in ground state, when the care of the molecule in ground state through shorter wavelength, energy storage is got up, and then slowly emits the light of longer wavelength, and the light of emitting is exactly fluorescence.Energy-wavelength relationship the figure of fluorescence is done out, and the graph of a relation of gained is exactly fluorescence spectrum.High intensity laser beam can make a considerable amount of molecules in absorbing material rise to excitation quantum state, the sensitivity that has therefore greatly improved fluorescence spectrum.53 organism in < < drinking water standard > > (GB5749-2006) index have quite a few to have fluorescence, be partly dissolved in organism in water when being subject to the irradiation of specific wavelength, organism is subject to exciting light that can specific wavelength.Experiment shows, glimmering light intensity and organic concentration that organism sends exist good correlativity, utilize this characteristic, can fast and effeciently set up the early warning mechanism to water head site earth's surface organic pollutants.
With it, quick, sensitive and good selective is widely used in detecting and identifies the many kinds of substances such as organism, medicine, inorganics three-dimensional fluorescence atlas analysis, in a plurality of fields, has a wide range of applications.The present invention is in conjunction with micro-filtration, and the means such as counter-infiltration and three-dimensional fluorescence atlas analysis, have increased the sensitivity of fluorescence pattern, and water head site surface water is monitored, and fast and effeciently the some organic pollutants in water are played to forewarning function.
Beneficial effect of the present invention is mainly reflected in:
(1) ultimate principle of utilizing fluorescence to produce, carries out three-dimensional fluorescence to water head site surface water and scans and in early warning water, have the generation of fluorescent characteristic organic contaminant and exceed standard.
(2) adopt micro-filtration, counter-infiltration to concentrate water sample, greatly improve the effect sensitivity of detection of contamination, whole operating process can complete within 15 minutes, had fast, advantage easily.
(3) can realize the on-line monitoring to surface water, further improve early warning efficiency.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of embodiment 1.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further.
With reference to Fig. 1, a kind of quick method for early warning of surface water organic contamination, said method comprising the steps of:
(1) gather surface water as former water;
(2) by miillpore filter, filter and gather the former water of coming, hold back gravel, mud and clay particle in former water;
(3) get the water sample 1-1.5L after filtration, concentrated through reverse osmosis unit, the water sample after being concentrated;
(4) get the water sample of step (3) after concentrated in fluorescence cuvette, the sample cell that is placed in fluorospectrophotometer carries out three-dimensional fluorescence spectrum scanning, obtains the three-dimensional fluorescence collection of illustrative plates of water sample;
(5) according to the upper limit of < < drinking water standard > >, prepare standard water sample, concentrated through reverse osmosis unit, same through three-dimensional fluorescence scanning, obtain standard diagram;
(6) the three-dimensional fluorescence collection of illustrative plates of the water sample of described standard diagram and step (4) is compared, if the fluorescence intensity of the three-dimensional fluorescence collection of illustrative plates of water sample is less than or equal to the fluorescence intensity of described standard diagram, judge that surface water organic contamination does not exceed standard; Otherwise, judge that surface water organic contamination exceeds standard.
Further, the cycles of concentration of the water sample of the concentrated multiple of described step (5) Plays water sample after filtering with step (3) is identical.
This example be take phenol and is described as example, and experiment equipment used is by vacuum filtration device, and reverse osmosis unit and fluorospectrophotometer three parts form, and the schematic flow sheet of experiment is referring to Fig. 1.
(1) Shang Tang river, the Hangzhou river that takes a morsel.
(2), by vacuum extractor, use the filtering with microporous membrane river of 0.45 μ m.
(3) get the water sample after 1L filters, with reverse osmosis unit, concentrate this water sample, and obtain the water sample of original solution concentration.
(4) get that (3) say water sample in 1cm fluorescence cuvette, the sample cell that is placed in fluorospectrophotometer carries out three-dimensional fluorescence spectrum scanning, Main is set as follows: excitation wavelength Ex:200-600nm, is spaced apart 10nm; Emission wavelength Em:200-600nm; Sweep velocity is 6000nm/min, and sweep spacing is 1nm.Obtain the three-dimensional fluorescence collection of illustrative plates of concentrated rear water sample.
(5) phenol solution of the 0.002mg/L preparing with pure water, concentrates this solution by reverse osmosis unit, obtain the phenol concentrated solution with identical multiple in (4).This solution is carried out to three-dimensional fluorescence scanning, the three-dimensional fluorescence spectrum of the phenol solution after being concentrated, and with (4) in the three-dimensional fluorescence spectrum that obtains compare.
The fluorescence intensity of the phenol in river, the upper pool river after concentrated can not show a candle to the fluorescence intensity in the standard phenol solution after concentrating, and illustrates that the phenol in the river of river, the pool surpasses drinking water sanitary standard.
The present invention carries out three-dimensional fluorescence scanning to water head site surface water, improves the detection limit of pollutant by enrichment facility, improves the sensitivity of experimental apparatus.By long-term monitoring, obtain the normal three-dimensional fluorescence spectrum of a certain water head site surface water, if the fluorescence spectrum of water sample being detected occurs abnormal, can cause the concrete material that fluorescence spectrum is abnormal by further detection means (as GC-MS) analysis, and can send timely and accurately drinking water safety early warning notice.

Claims (2)

1. a quick method for early warning for surface water organic contamination, is characterized in that: said method comprising the steps of:
(1) gather surface water as former water;
(2) by miillpore filter, filter and gather the former water of coming, hold back gravel, mud and clay particle in former water;
(3) get the water sample 1-1.5L after filtration, concentrated through reverse osmosis unit, the water sample after being concentrated;
(4) get the water sample of step (3) after concentrated in fluorescence cuvette, the sample cell that is placed in fluorospectrophotometer carries out three-dimensional fluorescence spectrum scanning, obtains the three-dimensional fluorescence collection of illustrative plates of water sample;
(5) according to the upper limit of < < drinking water standard > >, prepare standard water sample, concentrated through reverse osmosis unit, same through three-dimensional fluorescence scanning, obtain standard diagram;
(6) the three-dimensional fluorescence collection of illustrative plates of the water sample of described standard diagram and step (4) is compared, if the fluorescence intensity of the three-dimensional fluorescence collection of illustrative plates of water sample is less than or equal to the fluorescence intensity of described standard diagram, judge that surface water organic contamination does not exceed standard; Otherwise, judge that surface water organic contamination exceeds standard.
2. the quick method for early warning of a kind of surface water organic contamination as claimed in claim 1, is characterized in that: the cycles of concentration of the water sample after the concentrated multiple of described step (5) Plays water sample filters with step (3) is identical.
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CN105334198A (en) * 2015-11-14 2016-02-17 常州大学 Method for analyzing DOMs (dissolved organic matters) in water on basis of three-dimensional fluorescence spectra
CN105466893A (en) * 2015-11-14 2016-04-06 常州大学 Three-dimensional fluorescence spectrum based method for rapid alert of organic pollution of surface water
CN105784617A (en) * 2016-04-25 2016-07-20 河海大学 Water quality testing method based on spectral analysis
CN107561180A (en) * 2017-08-24 2018-01-09 山东省城市供排水水质监测中心 A kind of method that volatile organic matter in water is detected based on counter-infiltration
CN107561181A (en) * 2017-08-24 2018-01-09 山东省城市供排水水质监测中心 A kind of detection method of underwater trace persistence organic pollutant
CN107782705A (en) * 2016-08-31 2018-03-09 中国石油天然气股份有限公司 Rock determination method for oil content and device
CN108181286A (en) * 2018-02-02 2018-06-19 浙江工业大学 Water tank with real-time pesticide monitoring function by adopting three-dimensional fluorescence technology
CN113567401A (en) * 2020-04-28 2021-10-29 中国环境科学研究院 Rapid detection method and application of landfill leachate polluted underground water condition

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105334198A (en) * 2015-11-14 2016-02-17 常州大学 Method for analyzing DOMs (dissolved organic matters) in water on basis of three-dimensional fluorescence spectra
CN105466893A (en) * 2015-11-14 2016-04-06 常州大学 Three-dimensional fluorescence spectrum based method for rapid alert of organic pollution of surface water
CN105784617A (en) * 2016-04-25 2016-07-20 河海大学 Water quality testing method based on spectral analysis
CN107782705A (en) * 2016-08-31 2018-03-09 中国石油天然气股份有限公司 Rock determination method for oil content and device
US10598595B2 (en) 2016-08-31 2020-03-24 Petrochina Company Limited Method for determining oil contents in rock formations
CN107782705B (en) * 2016-08-31 2020-11-06 中国石油天然气股份有限公司 Method and device for measuring oil content of rock
CN107561180A (en) * 2017-08-24 2018-01-09 山东省城市供排水水质监测中心 A kind of method that volatile organic matter in water is detected based on counter-infiltration
CN107561181A (en) * 2017-08-24 2018-01-09 山东省城市供排水水质监测中心 A kind of detection method of underwater trace persistence organic pollutant
CN108181286A (en) * 2018-02-02 2018-06-19 浙江工业大学 Water tank with real-time pesticide monitoring function by adopting three-dimensional fluorescence technology
CN113567401A (en) * 2020-04-28 2021-10-29 中国环境科学研究院 Rapid detection method and application of landfill leachate polluted underground water condition
CN113567401B (en) * 2020-04-28 2022-09-30 中国环境科学研究院 Rapid detection method and application of landfill leachate polluted underground water condition

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