CN100363735C - Field optical investigating device and detecting method for multiple organic pollutant in sea water - Google Patents
Field optical investigating device and detecting method for multiple organic pollutant in sea water Download PDFInfo
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- CN100363735C CN100363735C CNB200410035526XA CN200410035526A CN100363735C CN 100363735 C CN100363735 C CN 100363735C CN B200410035526X A CNB200410035526X A CN B200410035526XA CN 200410035526 A CN200410035526 A CN 200410035526A CN 100363735 C CN100363735 C CN 100363735C
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Abstract
The present invention provides an in situ optical measuring device for multiple organic pollutants in sea water and a detecting method thereof. The in situ optical measuring device is mainly composed of a pulse xenon lamp, a diffracting raster, a sample pool, an absorption light detector, a fluorescence detector, a light filter, a sampling pump, a control system, etc. Categories of substances are determined by spectrum information obtained and recorded by excitation light with specific wavelength and by fluorescence condition generated by the excitation of the excitation light. Moreover, the content of substances is measured by an absorption spectrum with specific wavelength. The in situ optical measuring device can carry out in situ real-time continuous measurement for organic pollutants in water such as chlorophyll-a, phenol, yellow substances and petroleum by one instrument. The in situ optical measuring device can shorten analysis programs for detecting, and has the advantages of convenient and feasible operation and control, and no pollution to environment.
Description
Technical field
The invention belongs to the detecting instrument and the detection method of marine environmental monitoring aspect, is multiple organic contaminant live optical measurement mechanism and detection method in a kind of seawater specifically.
Background technology
For a long time, people adopted the organic contaminant in the several different methods measurement seawater once, usually adopt spectrophotometric method as chlorophyll, the laboratory fluorescence method, phenol adopts bromination titration method and ultraviolet spectrophotometry usually, oil adopts the fluorescence spectrophotometer method usually in the laboratory, ultraviolet spectrophotometry, infrared spectrophotometer and gravimetric method are measured, yellow substance (contains humic acid, the product that the soluble colored organic of black albumin and other complex compound-organism decomposes is commonly called " yellow substance ") employing laboratory chemistry concentrates absorption method and fluorescence method is measured, above-mentioned measuring method all is under lab to carry out, there is the sampling difficulty in these methods, positioning error is big, many shortcomings such as test period is long need expend great amount of manpower, material resources.In view of above reason, demand urgently studying a kind of can be at the scene to above-mentioned pollutant carry out the scene, in real time, the instrument of continuous coverage.
Summary of the invention
The objective of the invention is deficiency at the prior art existence, multiple organic contaminant live optical measurement mechanism and detection method in a kind of seawater are provided, the principle of employing optics only can be finished with an instrument the on-the-spot real-time continuous of organic contaminant chlorophyll-a, phenol, yellow substance, oil in the water is measured, and can shorten the check and analysis program; In addition, the operation, control convenient and easy, environment is not produced pollution.
The objective of the invention is to be achieved through the following technical solutions: multiple organic contaminant live optical measurement mechanism in a kind of seawater, comprise the excitation light generation device, sample cell, fluorescence detector and absorbing light detecting device and have the control system of central processing unit, the light source that it is characterized in that described excitation light generation device is a pulse xenon lamp, pulse xenon lamp, first light filter, pulsed light dispatch tube and diffraction grating shell are arranged in order and are connected as a single entity, pulsed light passes first light filter, shine on the diffraction grating behind the pulsed light dispatch tube, the diffraction grating shell is also received sample cell by the diffraction light dispatch tube, the sample cell side is provided with connected absorbing light detecting device, fluorescence detector is received second light filter by photomultiplier, and second light filter links to each other with sample cell.
Described sample cell disposes the sampling pump of a continuous water supply.
When long-term work, the sample pool wall may adhere to some pollutants, described sample cell configuration ozone generator, with generation ozone deliver to sample cell, can reach the purpose of cleaning.
Second light filter of first light filter before the described pulse xenon lamp and close sample cell is by drive of motor.
On the described diffraction grating shell motor is set, the motor-driven diffraction grating rotates, and changes the angle of diffraction grating and pulsed light, to produce the exciting light that requires.
The method of utilizing measurement mechanism of the present invention to detect is: send light by pulse xenon lamp, behind first light filter, shine on the diffraction grating, diffraction grating is separated into monochromatic light with light, with the sample in the monochromatic light irradiation sample cell of regulation, inspire fluorescence, fluorescence is received by fluorescence detector after second light filter filters, and delivers to the central processing unit of control system and handle after opto-electronic conversion, determines the kind of pollutant with this; In addition, in when work, after the light of the isolated all wavelengths of diffraction grating institute passed through sample, all the absorbed light detector recording was got off, and delivers to the central processing unit of control system, calculates the concentration of pollutant with this.
The present invention compared with prior art has many advantages and good effect:
1, measurement mechanism of the present invention is suitable for boat-carrying, also can be installed on the buoy of fixing a point to lay, only can finish four kinds of organic contaminant chlorophyll-as, phenol, oil, yellow substance are carried out scene, continuous, measurement in real time with an instrument, marine environment is carried out unmanned monitoring on the spot, the operation, control convenient and easy, environment is not produced pollution.
2, the intelligent degree of measurement mechanism of the present invention has had large increase, a large amount of human resources have been saved, improved detection efficiency and accuracy of measurement, made Monitoring Data have actual effect, the control of instructing organic contaminant in the marine environment that can be accurate and effective and improvement work.
3, measurement mechanism of the present invention also can be used for the pollution monitoring of discharge of industrial wastes mouth and the automatic monitoring system of environmental monitoring station.In addition, in the project of South-to-North water diversion of China, also have broad prospects, will bring very big economic benefit and social benefit.
Description of drawings
Fig. 1 is the one-piece construction part sectioned view of measurement mechanism of the present invention;
Fig. 2 is the principle of work synoptic diagram of measurement mechanism of the present invention;
Fig. 3 is the workflow block diagram of measurement mechanism of the present invention.
Embodiment
The measuring principle of multiple organic contaminant live optical measurement mechanism in the seawater of the present invention:
Discover, chlorophyll-a excites down at the visible light shortwave, send fluorescence in red color area, the fluorescence that planktonic organism main in absorption spectrum and the ocean is sent compares (diatomeae, green single celled monocrystalline, redness, blue-green phytoplankton) and infers: when wavelength coverage was 400～700nm, the relativity by fluorescence signal and absorption can detect above planktonic organism; Yellow substance sends fluorescence in the bluish-green zone of spectrum; In polluted water region, detect material-polyaromatic hydrocarbon that the suitable method of petroleum products is a utilization reflection petroleum products optical characteristics " trace (vestige) ", the oil Research of Spectrum Characteristics is drawn: the maximum magnitude of spectral absorption is at 255～275 wave bands, NAY maximum fluorescence intensity occurs at 400nm, this moment, to excite light wavelength be 345nm, and this exciting light is perfect condition; The fluorescence of phenol has maximal value when 280～300nm.Therefore can detect their situation that exists according to above four kinds of pollutants produce fluorescence under the particular range excitation situation.Studies confirm that, contain the planktonic organism of color can be in specific spectral range absorbing light, comprising: the blue portion in the chlorophyll-a absorption spectrum (420～460nm) and shortwave in red light part (660～665nm); Contain product (being commonly called " yellow substance ") that soluble colored organic-organism of humic acid, black albumin and other complex compound decomposes can absorb in a large number in the visible light the shortwave part and apart from the nearer part of ultraviolet light; Research of Spectrum Characteristics to petroleum products draws: the maximum magnitude of spectral absorption is at 255～275 wave bands; The absorption spectrum of phenol is the strongest in wavelength 270nm left and right sides absorption, is in the decline state at 237～245nm, is in high absorbing state in the spectrum short wavelength regions.
In sum, principle of work of the present invention is to write down the classification that the spectral information that obtains is determined material according to the fluorescence situation in specific wavelength exciting light and the generation of this excitation, and comes the content of measurement of species according to the absorption spectrum of specific wavelength.Details is as shown in table 1.
Table 1 utilizes the method for different pollutant kinds and content in the optical method for measuring seawater
Annotate: C--pollutant levels D--optical density a～h--measurement coefficient
As can be seen from the table, be 260nm at exciting light, produce fluorescence signal in 280～300nm scope, and when exciting light is 345nm, be the 400nm place at wavelength, do not exist the characteristic of fluorescence signal to determine whether phenol exists, and concern D according to spectrum
268/ D
242Determine the content of phenol; Concern D according to spectrum
268/ D
242Can record the content of water PetroChina Company Limited. product, and be 345nm at exciting light, emission light can obtain the fluorescence spectrum that proves that oil exists when being 350～400nm; When measuring chlorophyllous content, concern D according to spectrum
443/ D
547Ratio determine, when exciting light is 435nm, be 680nm place at emission light, can record the fluorescence spectrum of proof chlorophyll existence; The content of yellow substance is according to D
337/ D
660Ratio determine, be 345nm at exciting light, the fluorescence spectrum that emission light obtains during for 460nm detects.
Specific embodiments of the present invention is as follows:
According to the principle of work of system, the function of measurement mechanism of the present invention is as follows:
1, recording wavelength be 242,268,377,443,547, light absorbing minimum value during 660nm;
2, recording wavelength is the exciting light of 260nm, 345nm and 435nm; The fluorescence of record 280～300nm, 350～400nm, 460nm and 680nm.
Referring to Fig. 1-Fig. 3, be the embodiment of multiple organic contaminant live optical measurement mechanism in the seawater of the present invention, its critical piece has: pulse xenon lamp 1, diffraction grating 4, sample cell 8, absorbing light detecting device (photodiode) 7, fluorescence detector 11, photoelectricity increase pipe 10, first light filter 2, second light filter 9, sampling pump fully, have the compositions such as control system of central processing unit.The shell of pulse xenon lamp 1, first light filter 2, pulsed light dispatch tube and diffraction grating 4 is arranged in order and is connected as a single entity.Pulsed light shines on the diffraction grating 4 after passing first light filter 2, pulsed light dispatch tube.Diffraction grating 4 shells are also received sample cell 8 by the diffraction light dispatch tube, the sampling pump and an ozone generator of sample cell 8 configurations one seawater without interruption, and sample cell 8 also is connected with an absorbing light detecting device 7.Fluorescence detector 11 is received second light filter, 9, the second light filters 9 by photomultiplier 10 and is linked to each other with sample cell 8.
The workflow of the embodiment of the invention (as shown in Figure 3):
Measurement mechanism is when work, send light by pulse xenon lamp 1, behind first light filter 2, shine on the diffraction grating 4, diffraction grating 4 is separated into monochromatic light with light, sample with in the monochromatic light irradiation sample cell 8 of regulation inspires fluorescence, and fluorescence is received by fluorescence detector through second light filter 9, photomultiplier 10, after opto-electronic conversion, deliver to the control system central processing unit and handle, determine the kind of pollutant with this; In addition, when work, the light of 4 isolated all wavelengths of diffraction grating is by behind the sample, and all absorbed light detecting device 7 is noted, and delivers to the control system central processing unit, calculates the concentration of pollutant with this.Sample cell 8 is measured to guarantee on-the-spot real-time continuous by sampling pump seawater without interruption.When long-term work, may adhere to some pollutants on the wall of sample cell 8, ozone generator produces ozone, delivers to sample cell 8, can reach the purpose of cleaning.
The measurement of the embodiment of the invention is carried out according to the following steps:
1, spectrophotometry: record is from the absorption spectrum of 230～670nm.
2, fluorescence spectrometry: record exciting light λ
ExFluorescence λ when being 230～670nm
EmFrom 280～300,350～400,460, the fluorescence spectrum of 680nm is determined the pollutant classification.
3, seek: seek the abnormal signal value of four kinds of pollutant absorption spectrums and determine λ
1And λ
2
4, measure: determine 1gD λ according to two wavelength
1/ D λ
2Value, and calculate material concentration.
5, turbidimetry:, measure the scattering situation of fluorescence in the time of 90 jiaos at four wave bands 280～300,350～400,460,680nm.
6, chemiluminescence is measured: the chemiluminescence of sending during record ozone in water oxidation dissolution organism, cleaning sample cell surface.
Certainly, above-mentioned explanation is not to be limitation of the present invention, and the present invention also is not limited to above-mentioned giving an example; those skilled in the art; in essential scope of the present invention, the variation of making, remodeling, interpolation or replacement all should belong to protection scope of the present invention.
Claims (6)
1. multiple organic contaminant live optical measurement mechanism in the seawater, comprise the excitation light generation device, sample cell, fluorescence detector and absorbing light detecting device and have the control system of central processing unit, the light source that it is characterized in that described excitation light generation device is a pulse xenon lamp, pulse xenon lamp, first light filter, pulsed light dispatch tube and diffraction grating shell are arranged in order and are connected as a single entity, pulsed light passes first light filter, shine on the diffraction grating behind the pulsed light dispatch tube, the diffraction grating shell is also received sample cell by the diffraction light dispatch tube, the sample cell side is provided with connected absorbing light detecting device, fluorescence detector is received second light filter by photomultiplier, and second light filter links to each other with sample cell.
2. according to multiple organic contaminant live optical measurement mechanism in the described seawater of claim 1, it is characterized in that described sample cell disposes the sampling pump of a continuous water supply.
3. according to multiple organic contaminant live optical measurement mechanism in claim 1 or the 2 described seawater, it is characterized in that described sample cell configuration ozone generator.
4. according to multiple organic contaminant live optical measurement mechanism in claim 1 or the 2 described seawater, it is characterized in that first light filter before the described pulse xenon lamp reaches second light filter of close sample cell by drive of motor.
5. according to multiple organic contaminant live optical measurement mechanism in claim 1 or the 2 described seawater, it is characterized in that on the described diffraction grating shell motor being set, the motor-driven diffraction grating rotates, and changes the angle of diffraction grating and pulsed light, to produce the exciting light that requires.
6. one kind is utilized the method that multiple organic contaminant live optical measurement mechanism detects in the described seawater of claim 1, it is characterized in that: send light by pulse xenon lamp, behind first light filter, shine on the diffraction grating, diffraction grating is separated into monochromatic light with light, with the sample in the monochromatic light irradiation sample cell of regulation, inspire fluorescence, fluorescence is received by fluorescence detector after second light filter filters, after opto-electronic conversion, deliver to the central processing unit of control system and handle, determine the kind of pollutant with this; In addition, in when work, after the light of the isolated all wavelengths of diffraction grating institute passed through sample, all the absorbed light detector recording was got off, and delivers to the central processing unit of control system, calculates the concentration of pollutant with this.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102128779A (en) * | 2010-12-20 | 2011-07-20 | 无锡荣兴科技有限公司 | Method for analyzing algae and chormophoric dissolved organic matters on line by non-external sheath fluid flow cytometry |
| CN102128776A (en) * | 2010-12-20 | 2011-07-20 | 无锡荣兴科技有限公司 | Method for detecting alga and coloured dissolved organic matters by adopting flow cytometry |
| CN105203481A (en) * | 2015-09-21 | 2015-12-30 | 上海光谱仪器有限公司 | Spectrophotometer data collecting system and method based on pulse xenon lamp |
Families Citing this family (6)
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|---|---|---|---|---|
| CN101839858B (en) * | 2010-05-13 | 2012-11-07 | 大连海事大学 | Nonlinear laser fluorescence spectrum real-time identification method |
| CN101839854B (en) * | 2010-05-31 | 2012-05-23 | 中国科学院南海海洋研究所 | Long optical path sea water absorption coefficient measuring device and working method thereof |
| CN102128799A (en) * | 2010-12-21 | 2011-07-20 | 无锡荣兴科技有限公司 | Water quality detection sensor |
| CN102095712A (en) * | 2010-12-21 | 2011-06-15 | 无锡荣兴科技有限公司 | Photoelectric sensor for detecting blue-green algae |
| CN102866136A (en) * | 2012-08-09 | 2013-01-09 | 中国科学院烟台海岸带研究所 | Probe type on-line monitoring system and probe type on-line monitoring method for water petroleum pollutants |
| CN106053421B (en) * | 2016-08-18 | 2019-09-27 | 南昌大学 | Content of organic matter on-line checking and filter core/film breakdown early warning method and apparatus in water |
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| US3891859A (en) * | 1974-06-21 | 1975-06-24 | Us Navy | Pulsed, variable beam pattern optical measuring device |
| CN2608975Y (en) * | 2003-04-19 | 2004-03-31 | 国家海洋局第一海洋研究所 | Underwater fluorometer probe |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102128779A (en) * | 2010-12-20 | 2011-07-20 | 无锡荣兴科技有限公司 | Method for analyzing algae and chormophoric dissolved organic matters on line by non-external sheath fluid flow cytometry |
| CN102128776A (en) * | 2010-12-20 | 2011-07-20 | 无锡荣兴科技有限公司 | Method for detecting alga and coloured dissolved organic matters by adopting flow cytometry |
| CN105203481A (en) * | 2015-09-21 | 2015-12-30 | 上海光谱仪器有限公司 | Spectrophotometer data collecting system and method based on pulse xenon lamp |
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