CN101196471A - Soil heavy metal pollution quantification detecting system and detecting method - Google Patents
Soil heavy metal pollution quantification detecting system and detecting method Download PDFInfo
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- CN101196471A CN101196471A CNA2007101726909A CN200710172690A CN101196471A CN 101196471 A CN101196471 A CN 101196471A CN A2007101726909 A CNA2007101726909 A CN A2007101726909A CN 200710172690 A CN200710172690 A CN 200710172690A CN 101196471 A CN101196471 A CN 101196471A
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Abstract
The invention discloses a soil heavy metal pollution quantification testing system and the testing method, which is used to conduct quantification monitoring to medium and light heavy metal polluted soil. The quantification testing system of the invention comprises a laser, a beam splitter, a collecting optics lens, an optical fiber detector, optical fiber, a spectrograph, a laser dynamometer instrument and a computer. The quantification testing system of the invention normalizes the laser induction and plasma spectrum strength value of the trace element in soil standard sample into the strength value of injecting laser, and then utilized the linear relation between the normalized value and the element content to build calibrating plot, and finally utilizes the calibrating plot and the same normalization method to conduct quantitative detecting to the heavy metal element in the unknown soil sample.
Description
Technical field
The present invention relates to the plasma spectrometry quantitative analysis tech of material, specifically be meant a kind of soil heavy metal pollution quantification detecting system and detection method, it is used for the quantification monitoring of centering, slight heavy-metal contaminated soil.
Background technology
Heavy metal is " pollutant " in the environment, follows socioeconomic fast development, and its pollution level and contaminated area all are increases trend year by year.In a single day soil suffer heavy metal pollution, and will and amplify through the food chain enrichment finally influence human health, so problems such as the domestic and international monitoring of all paying special attention to heavy metal pollution of soil and improvement.
Heavy metal-polluted soil element kind is various, they in environment background value and in " Chinese soil environmental quality standards " critical value of defined all be not quite similar, adopt classic method that heavy metal-polluted soil is analyzed very difficulty simultaneously, usually arrive first and pollute place collection pedotheque, return the laboratory applications atomic absorption spectrum then, atomic fluorescence spectrophotometry, plasma---atomic emission spectrum or mass spectrum etc. carries out chemical analysis, and different heavy metal analytical approachs there are differences, the operational sequence complexity, time-consuming, not only expend a large amount of manpower and materials, experimenter's health is also had certain influence.The laser induced plasma spectral technique is a fast-developing in recent years analysis of chemical elements technology, has the advantage that real-time, quick, on-the-spot detection and multielement are surveyed simultaneously, is fit to very much heavy metal pollution of soil and monitors.
The working mechanism of laser induced plasma spectral technique is: the high energy pulse laser beam converges at sample surfaces, obtain the photon energy density (unit square centimetre) of MW class at the convergent point place, material absorbing highdensity photon " multi-photon absorption ionization " takes place, the free electron that ionization goes out under the accelerating effect of laser electric field with atom generation sharp impacts and make its ionization and produce the more freedom electronics, these free electrons continue to participate in the impact ionization process, thereby " the cascade ionization " of similar " chain reaction " takes place, when electron density is increased to a certain degree, disassociation takes place and the plasma of formation high temperature high-energy state, simultaneously with clear and melodious shock wave sound and strong flash of light.Usually below 10ns, after laser pulse disappeared, plasma cooled down laser pulse duration gradually, gives off various atoms of elements spectrum simultaneously.These atomic spectral lines are contained elements of material " fingerprint ", the kind of its wavelength location corresponding element, the content of its signal intensity corresponding element, the basis that Here it is photoinduction plasma light spectral technology is qualitative, the quantitative test material element is formed.
At present, the qualitative analysis ability of laser induced plasma spectral technique has obtained universally acknowledged, but aspect quantitative test owing to be subjected to the influence of " nonlinear effect ", be difficult to find a kind of quantitative method of versatility always.The atomic spectral line signal intensity that so-called " nonlinear effect " refers to the element-specific that laser induced plasma gives off not only depends on the content of this kind element in plasma, also be subjected to the influence of other several factors simultaneously, thereby cause presenting nonlinear relationship between this element atom line strength and the corresponding content.In causing the effect of nonlinear factor, most importantly " self-absorption " effect of atomic spectral line, be that the atomic radiation of specific wavelength " self-absorption " takes place when passing through highdensity plasma and decays, this " self-absorption " effect be difficult to quantize, thereby causes the nonlinear relationship between element atom line strength and the corresponding content also to be difficult to quantize.
A large amount of experimental studies show: for containing the trace element of quantity not sufficient 300ppm in the sample, during the atomic spectrum radiation influence of " self-absorption " effect very little, can keep the better linearity relation between element atom line strength and the corresponding content.In " the soil environment quality standard " of Chinese Government's promulgation, heavy metal pollution of soil divides does three grades, and one-level is polluted the lightest; Three grades of pollutions are the heaviest; Secondary pollution divides again makes three grades of A, B, C, and wherein the C level is polluted the heaviest.The quality standard value of contrast different stage, Quantitative Monitoring is made in heavy metal pollution below the 300ppm, can be good at estimating one-level, the secondary pollution degree of most heavy metal elements, that is to say can precise quantification 300ppm following in, the degree of slight pollution.
In addition, when utilizing the laser induced plasma spectral technique to carry out quantitative test, because sampled point small-sized (usually less than 1mm), thereby the unevenness of tested sample matrix is easy to cause measurement result to present bigger discreteness, for precision and the accuracy that improves quantitative test, usually need duplicate measurements, on basis, provide comparatively ideal result to the mass data statistical study, but in each measuring process because the instability of pulsed laser energy is often introduced bigger measured deviation, need take measures necessary to eliminate this influence, common way is that the intensity level to element-specific specific wavelength atomic spectral line carries out normalization, the selection of normalization standard has directly determined the precision and the accuracy of quantification, it normally is the normalization Standard Selection signal intensity of certain bar atomic spectral line of main element in the sample (element that content is higher), the starting point of this selection is to think that the relativeness between the atomic spectral line intensity of the atomic spectral line intensity of trace element and main element can keep consistance preferably in different measuring processes, and in fact, because the unevenness of sample matrix, the content of main element also changes in each measuring process, and this variation can't quantize at all, thereby causes main element atomic spectral line intensity also to change and can't quantize; Therefore when a variation and amount that can't quantize were carried out normalization as standard value, the normalization result also must have randomness to a certain degree, will bring inevitable negative influence to final statistics.
Summary of the invention
The objective of the invention is to set up a kind of soil heavy metal pollution quantification detecting system and detection method thereof, eliminate the influence of the shake of pulsed laser energy in each laser excitation process to measuring accuracy, realize in below the 300ppm, the soil of slight heavy metal pollution makes accurate quantification and detects.
As shown in Figure 1, soil heavy metal pollution quantification detecting system of the present invention comprises: laser instrument 1, beam splitter 2, converging optical lens 3, sample 4, fibre-optical probe 5, optical fiber 6, spectrometer 7, laser powermeter 8, computing machine 9.The system works principle is: the laser beam that laser instrument 1 is launched is at first by beam splitter 2, wherein 10% pulsed laser energy is reflexed on the probe of laser powermeter 8 by beam splitter 2, other 90% pulsed laser energy sees through beam splitter 2, be focused at sample 4 surfaces via convergent mirror 3 again and bring out the generation plasma, laser powermeter 8 is measured 10% pulsed laser energy and energy value is passed to computing machine 9 as the normalization standard value by interface circuit, the atomic spectrum that laser induced plasma gives off is collected by fibre-optical probe 5, be coupled to by optical fiber 6 in the entrance slit of spectrometer 7, spectral analysis data is passed to computing machine 9 by interface circuit, spectroscopic data and laser power data acquisition process software are housed in the computing machine 9, data acquisition and processing (DAP) software is realized the collection and the processing of spectroscopic data and pulsed laser energy data, the quantification calibration curve of element-specific contrast in result and the computing machine, thus the quantification that realizes element-specific in the tested sample detects.
The quantification detection method of soil heavy metal pollution quantification detecting system of the present invention comprises the following steps:
1) sets up the quantification calibration curve
The laser beam that laser instrument 1 is launched is at first by beam splitter 2, wherein 10% pulsed laser energy is reflexed on the probe of laser powermeter 8 by beam splitter 2, other 90% pulsed laser energy sees through beam splitter, is focused at specific model master sample 4 surfaces via convergent mirror 3 again and brings out the generation plasma; Laser powermeter 8 is measured 10% pulsed laser energy and energy value is passed to computing machine 9 by interface circuit store as the normalization standard value; The atomic spectrum that laser induced plasma gives off is collected by fibre-optical probe 5, is coupled to by optical fiber 6 in the entrance slit of spectrometer 7, and spectral analysis data is passed to computing machine 9 storages by interface circuit; Select the specific wavelength atomic spectral line of element to be measured, the laser energy value that records with laser powermeter 8 is as the normalization standard value, with the normalization of line strength value.Different specific model master samples are repeated above-mentioned steps to be measured, the content value of survey data and this element is formed (an x, y) coordinate (y represents the atomic spectral line intensity level after the normalization, x representative element content value), and simulate a calibration curve at element to be measured.
2) the normalization atomic spectrum intensity level of element to be measured in the measurement unknown sample
The laser beam that laser instrument 1 is launched is at first by beam splitter 2, wherein 10% pulsed laser energy is reflexed on the probe of laser powermeter 8 by beam splitter 2, other 90% pulsed laser energy sees through beam splitter 2, is focused at unknown sample 4 surfaces via convergent mirror 3 again and brings out the generation plasma; Laser powermeter 8 is measured 10% pulsed laser energy and energy value is passed to computing machine 9 by interface circuit store as the normalization standard value; The atomic spectrum that laser induced plasma gives off is collected by fibre-optical probe 5, is coupled to by optical fiber 6 in the entrance slit of spectrometer 7, and spectral analysis data is passed to computing machine 9 storages by interface circuit; The wavelength of selected element to be measured when setting up calibration curve according to step 1) the atomic spectral line intensity level normalization of the identical wavelength of element to be measured in the unknown sample, obtains normalized atomic spectral line intensity level measured value y
0
3) obtain element quantitative data to be measured
According to step 2) the normalized atomic spectral line intensity level of element to be measured (y=y in the unknown sample that obtains
0), the quantification calibration curve that utilizes step 1) to obtain just can obtain the content value x (x=x of this element
0), thereby the quantification that realizes element-specific detects.
Advantage of the present invention is:
(1) the quantification detection method of measuring system only is directed to the following trace element of 300ppm, can effectively avoid because line strength value that " self-absorption " effect of atomic spectral line causes and the nonlinear relationship between the constituent content.
(2) measuring system all normalizes to the intensity level of incident laser to various element plasma line strength values, has eliminated the influence of the shake of pulsed laser energy in each laser excitation process to measuring accuracy fully, has improved the quantification measuring accuracy.
Description of drawings
Fig. 1 is a detection system structural representation of the present invention; Wherein:
1---laser instrument;
2---beam splitter;
3---converging optical lens;
4---tested sample;
5---fibre-optical probe;
6---optical fiber;
7---spectrometer;
8---laser powermeter;
9---computing machine.
Embodiment
Provide better embodiment of the present invention according to Fig. 1 below.
The system that is used for the quantification detection comprises following several sections:
1) laser instrument 1
The light beam that laser instrument 1 is launched is used to excite sample to produce plasma spectrometry, produces the required normalization standard value of quantification process simultaneously.Select the Nd:YAG Q-switched pulse laser for use, operation wavelength 1064nm, pulsewidth 3-5ns, maximum impulse energy 200mJ, pulse energy degree of stability ± 2%, maximum impulse repetition frequency 20Hz, the laser-beam divergence angle is less than 1mrad.
2) beam splitter 2
Beam splitter 2 is used for the laser beam that laser instrument is launched is carried out beam splitting.245 ° of placements of beam splitter, beam splitter 2 is coated with reflectance coating in the one side of light beam incident, makes incident beam have 10% pulse energy to reflex on the probe of laser powermeter, and other 90% pulse energy transmissive excites sample to form plasma.
3) converging optical lens 3
Converging optical lens 3 is used for the convergent laser bundle, makes the laser energy density of sample surface reach breakdown threshold, thereby brings out the generation plasma.Aperture of lens 20mm, focal length 200mm.
4) fibre-optical probe 5
Fibre-optical probe 5 is used for collecting the atomic spectrum energy that plasma resonance goes out and is coupled in the optical fiber 6.Fibre-optical probe bore 30mm, focal length 52mm, transmission peak wavelength scope 200-1100nm.
5) spectrometer 7
Spectrometer 7 is used for the laser induced plasma spectrum that fibre-optical probe 5 is collected is done spectral analysis.Spectrometer 7 adopts echelle grating, spectrometer 7 response wave length 200-850nm, and the entrance slit of spectrometer 7 replaces spectral resolution 0.04-0.2nm with the ultraviolet transmission optical fiber of core diameter 50 μ m.The spectrometer detector adopts enhancement mode CCD device, and spectral signal is connected with computing machine by pci interface card after its A/D conversion.
6) laser powermeter 8
7) computing machine 9
Spectroscopic data and laser power data acquisition process software are housed in the computing machine 9.Spectrometer links to each other with computing machine by pci interface card, laser powermeter links to each other with computing machine by the RS232 interface, data acquisition and processing (DAP) software is realized the collection of spectroscopic data and pulsed laser energy data, and the realization of quantification process, can obtain the quantification calibration curve of element to be measured in the master sample, can realize that the quantification of element to be measured in the unknown sample detects.
Claims (2)
1. soil heavy metal pollution quantification detecting system, it comprises laser instrument, converging optical lens, fibre-optical probe, optical fiber, spectrometer and computing machine, it is characterized in that: it also has beam splitter (2) and laser powermeter (8), the laser beam that laser instrument (1) is launched is at first by beam splitter (2), wherein 10% pulsed laser energy is reflexed on the probe of laser powermeter (8) by beam splitter (2), other 90% pulsed laser energy sees through beam splitter (2), be focused at tested sample (4) surface via convergent mirror (3) again and bring out the generation plasma, laser powermeter (8) is measured 10% pulsed laser energy and energy value is passed to computing machine (9) as the normalization standard value by interface circuit, the atomic spectrum that laser induced plasma gives off is collected by fibre-optical probe (5), be coupled in the entrance slit of spectrometer (7) by optical fiber (6), spectral analysis data is passed to computing machine (9) by interface circuit, spectroscopic data and laser power data acquisition process software are housed in the computing machine (9), data acquisition and processing (DAP) software is realized the collection and the processing of spectroscopic data and pulsed laser energy data, the spectral intensity values that records is normalized to the intensity level of incident laser.
2. soil heavy metal pollution quantification detection method, it is characterized in that: it comprises the steps:
A. set up the quantification calibration curve, a series of specific model master samples are measured, the content value of survey data and this element is formed (an x, y) coordinate, y represents the atomic spectral line intensity level after the normalization, x representative element content value, and simulate a calibration curve at element to be measured;
B. measure the normalization atomic spectrum intensity level of element to be measured in the tested sample (4);
C. the normalized atomic spectral line intensity level of element to be measured in the tested sample that records according to step B (4) from the quantification calibration curve, obtains the corresponding content value of this element, realizes the quantification of element-specific is detected.
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| CN102253020A (en) * | 2011-05-03 | 2011-11-23 | 杭州电子科技大学 | Cavity enhanced detection apparatus for heavy metal content in air |
| CN102680436A (en) * | 2012-06-16 | 2012-09-19 | 山西大学 | Method and device for measuring content of carbon in coal ash |
| CN102680413A (en) * | 2012-05-25 | 2012-09-19 | 浙江大学 | Device and method for hyperspectral rapid detection on content of field soil organic matters by using panoramic annular belt |
| CN102830071A (en) * | 2012-08-13 | 2012-12-19 | 浙江大学 | Detection apparatus and method for total phosphorus content in soil |
| CN102901717A (en) * | 2012-06-12 | 2013-01-30 | 中国科学院安徽光学精密机械研究所 | Laser-induced breakdown spectroscopy-based portable handheld soil heavy mental detection device |
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| CN102253020B (en) * | 2011-05-03 | 2012-12-05 | 杭州电子科技大学 | Cavity enhanced detection apparatus for heavy metal content in air |
| CN102253020A (en) * | 2011-05-03 | 2011-11-23 | 杭州电子科技大学 | Cavity enhanced detection apparatus for heavy metal content in air |
| CN102680413A (en) * | 2012-05-25 | 2012-09-19 | 浙江大学 | Device and method for hyperspectral rapid detection on content of field soil organic matters by using panoramic annular belt |
| CN102901717B (en) * | 2012-06-12 | 2014-10-29 | 中国科学院安徽光学精密机械研究所 | Laser-induced breakdown spectroscopy-based portable handheld soil heavy mental detection device |
| CN102901717A (en) * | 2012-06-12 | 2013-01-30 | 中国科学院安徽光学精密机械研究所 | Laser-induced breakdown spectroscopy-based portable handheld soil heavy mental detection device |
| CN102680436A (en) * | 2012-06-16 | 2012-09-19 | 山西大学 | Method and device for measuring content of carbon in coal ash |
| CN102830071A (en) * | 2012-08-13 | 2012-12-19 | 浙江大学 | Detection apparatus and method for total phosphorus content in soil |
| CN102830071B (en) * | 2012-08-13 | 2015-01-21 | 浙江大学 | Detection apparatus and method for total phosphorus content in soil |
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| CN103424389A (en) * | 2013-07-25 | 2013-12-04 | 华南师范大学 | Test system for measuring PL spectrum and PLE spectrum of fluorescent powder |
| CN103604782A (en) * | 2013-11-22 | 2014-02-26 | 天津陆海石油设备系统工程有限责任公司 | Solid sample element analyzer based on laser technology |
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| CN111551510A (en) * | 2020-05-22 | 2020-08-18 | 浙江科达检测有限公司 | Soil heavy metal ion detection system and detection method |
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