CN104062255A - Method and device for detecting heavy metal content in soil based on sample box method - Google Patents
Method and device for detecting heavy metal content in soil based on sample box method Download PDFInfo
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Abstract
The invention discloses a method and device for detecting heavy metal content in soil based on a sample box method, and relates to the technical field of agriculture and environment detection. The method comprises the following steps: acquiring a soil sample of which the heavy metal content does not exceed the standard, pretreating to prepare a standard soil sample, putting the standard soil sample into a sample box, acquiring a terahertz pulse time-domain waveform of the standard soil sample, establishing a fingerprint spectrum bank, and comparing a terahertz spectrum of the soil sample to be tested after the pretreatment with the fingerprint spectrum bank of the standard soil sample, thereby acquiring the heavy metal data of the soil sample to be tested. By adopting the method and the device, heavy metal pollution qualitative and quantitative detection on the soil sample acquired in fields can be efficiently, rapidly, nondestructively and safely performed, and theory and method basis are provided for application of terahertz spectrum technique to detection on important physical and chemical parameters of agricultural soil and application technique development and study.
Description
Technical field
The present invention relates to Agriculture and Environment detection technique field, be specifically related to a kind of detection method and device of the heavy metal content in soil based on sample box method.
Background technology
Soil is the important growing environments of crops, and high-quality soil is to ensure national food, the important substance basis of development " high yield, high-quality, efficient, ecological, safety " modern agriculture.In recent years, along with rapid development of economy, a large amount of industrial source, life source pollutants and agricultural chemicals etc. enter and accumulate in agricultural land soil by multi-form, affect agricultural product quality, and then affect food security and ecologic environment by food chain, threaten human health.Show according to network data, since two thousand nine, China has recurred more than 30 particularly serious heavy metal pollution event.A lot of " blood lead " events such as the Jiangsu great Feng, Longchang, Sichuan, Jiahe, Hunan, Gansu Guazhou County, Chongyang, Hubei, Huaining, Anhui in succession occurring for 2010, become the focus of social concerns.Ministry of Land and Resources is once expression also, and the annual approximately 1,200 ten thousand ton-grain foods of China suffer that heavy metal pollution, direct economic loss exceed 20,000,000,000 yuan, and these grains are enough to support every year more than 4,000 ten thousand people more.Farmland soil heavy metals pollution problem relates to the people's livelihood, causes showing great attention to of people.Studying advanced, efficient, applicable heavy metal content in soil detection method is the most important condition addressing this problem.
At present, the quantitative test of heavy metal and detection method mainly contain spectroscopic methodology, electrochemical method and novel detection technique etc.Spectroscopic methodology is more traditional method, mainly contains atomic absorption method (AAS), atomic fluorescence method (AFS), inductively coupled plasma method (ICP), X-fluorescence spectrum (XRF) etc.Electrochemical detection method is current popular detection method, and detection speed is very fast, and numerical value is accurate, has larger application potential in environmental emergency context of detection.In addition, the detection technique that some are newer, as enzyme suppresses method, immunoassay and biology sensor method etc., has also launched exploratory development.Compare by analysis, although spectroscopic methodology can effectively be analyzed the heavy metal ion in various environmental samples with higher sensitivity, but mostly need large-scale expensive instrument, analytical approach cost is high, sample need to be through clearing up, analysis time is long, and the consideration of safety factor etc., are restricting the popularization and application of the method for farmland soil heavy metals content detection; Electrochemical method has good research and application in trace element detects, but in current heavy metal detects, there is the problems such as ion interference, add in pedotheque pre-treatment, need to carry out soil sample and clear up, the use of strong acid etc. may bring the secondary pollution of soil; Novel detection technique, combines with bio-science, shows good application prospect, but the preparation of specific antibody is more difficult at present, is restricting the application of the method.Existing detection means all exists relative merits separately, awaits further research and improves, and new effective detection means requires study.
Tera-hertz spectra (Terahertz is called for short THz), as a field of not yet being carried out in a deep going way applied research in spectral band, is one of focus of current scientific and technological circle innovative technology research.Its frequency is in 0.1THz～10THz (1THz=1012Hz), and the position in electromagnetic wave band, between infrared and radiowave, is a kind of radiation source newly, that have a lot of particular advantages.In recent years, developing rapidly of ultrafast laser technique, for the generation of terahertz pulse provides stably excitation source, made the generation of Terahertz and application obtain flourish.Terahertz photon energy is low, radiationless, can carry out safely and effectively contactless lossless detection, the rotational frequency of many light molecules, the large molecule vibration mode of functional group alive and the resonance frequency of biomacromolecule etc. are all in terahertz wave band, and the tera-hertz spectra response of research material is significant for its composition of deep announcement, structure and physicochemical property.Inventor had once carried out desk study and the research of Terahertz Technology in agriculture field application year September in October, 2009 to 2010 in the vertical university of Oklahoma, United States, after returning to the homeland, carry on further investigation, confirmed that the measurement that terahertz light spectral technology carries out heavy metal content in soil has feasibility.
There is following problem in existing method of testing: (1), the detection main equipments that rely on more, and expensive, need under laboratory condition, measure; (2), traditional detection means are by Atomic absorption/emission spectrum principle, operator's safety factor needs to consider; (3), pedotheque need to be through the clearing up of strong acid, analysis time is long, may bring secondary pollution; (4), detection means that galvanochemistry, biological detection etc. are new is still immature, testing result is unreliable.
Summary of the invention
(1) technical matters that will solve
The technical problem to be solved in the present invention is: how by terahertz light spectral technology, the content of effect of fertilizer to be detected.
(2) technical scheme
In order to solve the problems of the technologies described above, the invention provides a kind of detection method of the heavy metal content in soil based on sample box method, the method comprises:
S1, preparation standard pedotheque;
S2, standard pedotheque is put into sample box, obtain the terahertz pulse time domain waveform of standard pedotheque, build fingerprint spectrum library;
S3, the fingerprint spectrum library of pedotheque to be measured and described standard pedotheque is contrasted, obtain the heavy metal data of pedotheque to be measured.
Preferably, step S1 specifically comprises:
S10, collection soil, and carry out pre-service;
S11, the content of beary metal of pretreated soil is detected;
S12, determine that contents of heavy metal elements does not exceed standard after, prepare initial soil sample;
S13, in initial soil sample by adding the heavy metal ion of variety classes and different content, preparation standard pedotheque.
Preferably, standard pedotheque described in step S13 comprises pedotheque, the pedotheque that contains variety classes heavy metal that content of beary metal does not exceed standard and the pedotheque that contains variable concentrations heavy metal.
Preferably, step S2 specifically comprises:
S20, obtain the terahertz pulse time domain waveform that standard pedotheque is housed in sample box;
The spectroscopic data of S21, terahertz pulse time domain waveform to standard pedotheque carries out pre-service;
S22, by chemometrics method, pretreated different standard pedotheque spectroscopic data is carried out to mathematical modeling, build fingerprint spectrum library, set up the relationship between kind and the concentration of spectrum and heavy metal-polluted soil.
Preferably, step S3 specifically comprises:
S30, the heavy metal contamination of pretreated pedotheque to be measured in sample box is detected, obtain the terahertz pulse time domain waveform of pedotheque to be measured;
The spectroscopic data of S31, terahertz pulse time domain waveform to pedotheque to be measured carries out pre-service;
S32, the standard pedotheque spectroscopic data of pretreated pedotheque spectroscopic data to be measured and fingerprint spectrum library is compared, by the relationship between kind and the concentration of described spectrum and heavy metal-polluted soil, obtain the heavy metal data of pedotheque to be measured.
Preferably, heavy metal data described in step S3 comprise kind and the concentration of heavy metal.
The present invention also provides a kind of pick-up unit of the heavy metal content in soil based on sample box method, and this device comprises that preparation of standard sample module, database build module and testing sample comparing module;
Described preparation of standard sample module, for the preparation of standard pedotheque;
Described database builds module, for standard pedotheque is put into sample box, obtains the terahertz pulse time domain waveform of standard pedotheque, builds fingerprint spectrum library;
Described testing sample comparing module, for the fingerprint spectrum library of pedotheque to be measured and described standard pedotheque is contrasted, obtains the heavy metal data of pedotheque to be measured.
Preferably, sample prepared by described preparation of standard sample module, comprises pedotheque, the pedotheque that contains variety classes heavy metal that content of beary metal does not exceed standard and the pedotheque that contains variable concentrations heavy metal.
Preferably, described database structure module comprises the first data acquisition unit, the first data pretreatment unit and data modeling unit;
Described the first data acquisition unit, for obtaining the terahertz pulse time domain waveform that standard pedotheque is housed at sample box;
Described the first data pretreatment unit, carries out pre-service for the spectroscopic data of the terahertz pulse time domain waveform to standard pedotheque;
Described data modeling unit, for by chemometrics method, pretreated different standard pedotheque spectroscopic data being carried out to mathematical modeling, builds fingerprint spectrum library, sets up the relationship between kind and the concentration of spectrum and heavy metal-polluted soil.
Preferably, described testing sample comparing module comprises the second data acquisition unit, the second data pretreatment unit and testing sample data capture unit;
Described the second data acquisition unit, detects for the heavy metal contamination to the pretreated pedotheque to be measured of sample box, obtains the terahertz pulse time domain waveform of pedotheque to be measured;
Described the second data pretreatment unit, carries out pre-service for the spectroscopic data of the terahertz pulse time domain waveform to pedotheque to be measured;
Described testing sample data capture unit, for the standard pedotheque spectroscopic data of pretreated pedotheque spectroscopic data to be measured and fingerprint spectrum library is compared, by the relationship between kind and the concentration of described spectrum and heavy metal-polluted soil, obtain the heavy metal data of pedotheque to be measured.
(3) beneficial effect
Technique scheme tool of the present invention has the following advantages: the invention provides a kind of detection method and device of the heavy metal content in soil based on sample box method, have the following advantages:
(1) tera-hertz spectra detects, can realize contactless, harmless safety detection;
(2) load pedotheque by sample box, load fast, convenient test, does not need the micro-wave digestion of pedotheque, avoids bringing secondary pollution;
(3) tera-hertz spectra checkout equipment is moving towards miniaturization, easy to carry, for field measurement provides possibility;
(4) tera-hertz spectra checkout equipment, has good detection sensitivity, can realize the detection of content of beary metal.
Brief description of the drawings
The detection method block diagram of a kind of heavy metal content in soil based on sample box method that Fig. 1 provides for the embodiment of the present invention;
The pedotheque preparation flow figure that Fig. 2 provides for the embodiment of the present invention;
The sample box schematic diagram that Fig. 3 provides for the embodiment of the present invention;
The frequency domain transmission spectrum curve map under the environment that is full of nitrogen with to empty sample box test that Fig. 4 provides for the embodiment of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the embodiment of invention is further described.Following examples are only for technical scheme of the present invention is more clearly described, and can not limit the scope of the invention with this.
As shown in Figure 1, the invention provides a kind of detection method of the heavy metal content in soil based on sample box method, the method comprises:
S1, preparation standard pedotheque, pedotheque, the pedotheque that contains variety classes heavy metal that described standard pedotheque content of beary metal does not exceed standard and the pedotheque that contains variable concentrations heavy metal.
Step S1 specifically comprises the steps:
S10, collection soil, and carry out pre-service, realization is air-dry to prevent soil deterioration to soil;
S11, the content of beary metal of pretreated soil is detected, go the chemical examination of authoritative inspection center, learn that the heavy metal containing is very low, compared with the detectability of national regulation, negligible; If authoritative test result has exceeded the detectability of national regulation, illustrate that soil itself is just contaminated, that just can not be used, and need to change the soil that contents of heavy metal elements does not exceed standard;
S12, determine that contents of heavy metal elements does not exceed standard after, prepare initial soil sample;
S13, in initial soil sample by adding the heavy metal ion of variety classes and different content, approximate simulation heavy metal ion enters the natural process of soil, preparation standard pedotheque.Standard pedotheque preparation flow as shown in Figure 2, prepare pure (contents of heavy metal elements does not exceed standard) pedotheque and variety classes, variable concentrations (ppb～ppm rank, specifically specifying to formulate according to GB) pedotheque of heavy metal is as standard model, ensure that soil particle grinds evenly, diameter is below 0.1mm, Criterion pedotheque preparation method, described different types of heavy metal element mainly comprises mercury (Hg), cadmium (Cd), plumbous (Pb), the significant elements of bio-toxicity such as chromium (Cr) and metallic arsenic (As), and there is the zinc (Zn) of certain toxicity, copper (Cu), the elements such as nickel (Ni).
S2, standard pedotheque is put into sample box, obtain the terahertz pulse time domain waveform of standard pedotheque, build fingerprint spectrum library, set up the relationship between kind and the concentration of spectrum and heavy metal-polluted soil;
Sample box schematic diagram as shown in Figure 3, described sample box is generally transparent, and the material that THz wave is not absorbed or absorbed is less made.Pedotheque is carried on and in the sample box of even thickness, is convenient to Terahertz and measures, in the present invention, the length size of sample box design is respectively 35 × 3.5 × 35mm and two kinds of specifications of 35 × 5 × 35mm, wherein intermediate gaps thickness is respectively 1.5mm and 3mm, can select according to the amount of pedotheque the specification of sample box.
Wherein, step S2 specifically comprises:
S20, obtain the terahertz pulse time domain waveform that standard pedotheque and empty sample box are housed in sample box;
As shown in Figure 4, for fear of sample box, test result is caused to error, the present invention also uses terahertz time-domain spectroscopy equipment, the environment and the empty sample box that are full of nitrogen are tested, the frequency domain transmission spectrum curve obtaining, curve one represents to be full of the frequency domain transmission spectrum curve of nitrogen environment, curve two represents the frequency domain transmission spectrum curve of empty sample box, as seen from the figure, sample box itself is less to the absorption of tera-hertz spectra, can be for the test of sample.
The spectroscopic data of S21, terahertz pulse time domain waveform to standard pedotheque carries out pre-service; The spectrum that terahertz time-domain spectroscopy equipment gathers, except the self information of pedotheque, has also comprised sample box itself and other irrelevant information and noise, as electrical noise, sample background noise etc.By obtaining the spectroscopic data of standard pedotheque itself, adopt the process of data preprocessings such as level and smooth, polynary scatter correction and standard normalization to carry out pre-service to spectroscopic data, reduce the impact that other factor produces spectrum, stable for setting up, reliable peg model is laid a good foundation;
S22, by chemometrics method, pretreated different standard pedotheque spectroscopic data is carried out to modeling, build fingerprint spectrum library, on the basis of data acquisition, use for reference near-infrared spectrum analysis knowledge, introduce chemometrics method, to variety classes, the tera-hertz spectra data of the pedotheque of variable concentrations heavy metal have been carried out respectively pre-service and the partial least square method modeling based on spectral information, the mathematical modeling of the partial least square method based on interval method selection characteristic wave bands and the partial least square method mathematical modeling based on genetic algorithm selection characteristic wave bands, choose optimum modeling result, build fingerprint spectrum library, set up the relationship between kind and the concentration of spectrum and heavy metal-polluted soil.。
S3, the fingerprint spectrum library of pedotheque to be measured and described standard pedotheque is contrasted, obtain the heavy metal data of pedotheque to be measured;
Wherein, step S3 specifically comprises:
S30, the heavy metal contamination of pretreated pedotheque to be measured in sample box is detected, obtain the terahertz pulse time domain waveform of pedotheque to be measured, described pre-service mainly comprises air-dry, the processing procedure such as sieve to soil, to prevent soil deterioration;
The spectroscopic data of S31, terahertz pulse time domain waveform to pedotheque to be measured carries out pre-service;
S32, the standard pedotheque spectroscopic data of pretreated pedotheque spectroscopic data to be measured and fingerprint spectrum library is compared, by the relationship between kind and the concentration of described spectrum and heavy metal-polluted soil, by mode identification method, find optimum matching, obtain the heavy metal data of pedotheque to be measured.
The present invention also provides a kind of pick-up unit of the heavy metal content in soil based on sample box method, and this device comprises that preparation of standard sample module, database build module and testing sample comparing module;
Described preparation of standard sample module, for the preparation of standard pedotheque;
Described database builds module, for standard pedotheque is put into sample box, obtains the terahertz pulse time domain waveform of standard pedotheque, builds fingerprint spectrum library;
Described testing sample comparing module, for the fingerprint spectrum library of pedotheque to be measured and described standard pedotheque is contrasted, obtains the heavy metal data of pedotheque to be measured.
Wherein, sample prepared by described preparation of standard sample module, comprises pedotheque, the pedotheque that contains variety classes heavy metal that content of beary metal does not exceed standard and the pedotheque that contains variable concentrations heavy metal.
Wherein, described database structure module comprises the first data acquisition unit, the first data pretreatment unit and data modeling unit;
Described the first data acquisition unit, for obtaining the terahertz pulse time domain waveform that standard pedotheque is housed at sample box;
Described the first data pretreatment unit, carries out pre-service for the spectroscopic data of the terahertz pulse time domain waveform to standard pedotheque;
Described data modeling unit, for by chemometrics method, pretreated different standard pedotheque spectroscopic data being carried out to mathematical modeling, builds fingerprint spectrum library, sets up the relationship between kind and the concentration of spectrum and heavy metal-polluted soil.
Wherein, described testing sample comparing module comprises the second data acquisition unit, the second data pretreatment unit and testing sample data capture unit;
Described the second data acquisition unit, detects for the heavy metal contamination to the pretreated pedotheque to be measured of sample box, obtains the terahertz pulse time domain waveform of pedotheque to be measured;
Described the second data pretreatment unit, carries out pre-service for the spectroscopic data of the terahertz pulse time domain waveform to pedotheque to be measured;
Described testing sample data capture unit, for the standard pedotheque spectroscopic data of pretreated pedotheque spectroscopic data to be measured and fingerprint spectrum library is compared, by the relationship between kind and the concentration of described spectrum and heavy metal-polluted soil, obtain the heavy metal data of pedotheque to be measured.
The preparation of standard sample module, the database that the present invention is based on foundation build module and testing sample comparing module, by the fingerprint spectrum library of setting up, the pedotheque that can gather field carry out efficiently, fast, can't harm, safe heavy metal pollution qualitative and quantitative detection.Along with the development of Terahertz Technology, as miniaturization, low cost, high flux etc., the detection and the application technology development research that are applied to the important physical and chemical parameter of agricultural land soil for terahertz light spectral technology provide theoretical and method foundation.
The above is only the preferred embodiment for the present invention; it should be pointed out that for those skilled in the art, do not departing under the prerequisite of the technology of the present invention principle; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (10)
1. a detection method for the heavy metal content in soil based on sample box method, is characterized in that, the method comprises:
S1, preparation standard pedotheque;
S2, standard pedotheque is put into sample box, obtain the terahertz pulse time domain waveform of standard pedotheque, build fingerprint spectrum library;
S3, the fingerprint spectrum library of pedotheque to be measured and described standard pedotheque is contrasted, obtain the heavy metal data of pedotheque to be measured.
2. the method for claim 1, is characterized in that, step S1 specifically comprises:
S10, collection soil, and carry out pre-service;
S11, the content of beary metal of pretreated soil is detected;
S12, determine that contents of heavy metal elements does not exceed standard after, prepare initial soil sample;
S13, in initial soil sample by adding the heavy metal ion of variety classes and different content, preparation standard pedotheque.
3. method as claimed in claim 2, is characterized in that, the pedotheque of standard described in step S13 comprises pedotheque, the pedotheque that contains variety classes heavy metal that content of beary metal does not exceed standard and the pedotheque that contains variable concentrations heavy metal.
4. the method for claim 1, is characterized in that, step S2 specifically comprises:
S20, obtain the terahertz pulse time domain waveform that standard pedotheque is housed in sample box;
The spectroscopic data of S21, terahertz pulse time domain waveform to standard pedotheque carries out pre-service;
S22, by chemometrics method, pretreated different standard pedotheque spectroscopic data is carried out to mathematical modeling, build fingerprint spectrum library, set up the relationship between kind and the concentration of spectrum and heavy metal-polluted soil.
5. the method as described in claim 1 or 4, is characterized in that, step S3 specifically comprises:
S30, the heavy metal contamination of pretreated pedotheque to be measured in sample box is detected, obtain the terahertz pulse time domain waveform of pedotheque to be measured;
The spectroscopic data of S31, terahertz pulse time domain waveform to pedotheque to be measured carries out pre-service;
S32, the standard pedotheque spectroscopic data of pretreated pedotheque spectroscopic data to be measured and fingerprint spectrum library is compared, by the relationship between kind and the concentration of described spectrum and heavy metal-polluted soil, obtain the heavy metal data of pedotheque to be measured.
6. the method for claim 1, is characterized in that, the data of heavy metal described in step S3 comprise kind and the concentration of heavy metal.
7. a pick-up unit for the heavy metal content in soil based on sample box method, is characterized in that, this device comprises that preparation of standard sample module, database build module and testing sample comparing module;
Described preparation of standard sample module, for the preparation of standard pedotheque;
Described database builds module, for standard pedotheque is put into sample box, obtains the terahertz pulse time domain waveform of standard pedotheque, builds fingerprint spectrum library;
Described testing sample comparing module, for the fingerprint spectrum library of pedotheque to be measured and described standard pedotheque is contrasted, obtains the heavy metal data of pedotheque to be measured.
8. device as claimed in claim 7, is characterized in that, sample prepared by described preparation of standard sample module comprises pedotheque, the pedotheque that contains variety classes heavy metal that content of beary metal does not exceed standard and the pedotheque that contains variable concentrations heavy metal.
9. device as claimed in claim 7, is characterized in that, described database builds module and comprises the first data acquisition unit, the first data pretreatment unit and data modeling unit;
Described the first data acquisition unit, for obtaining the terahertz pulse time domain waveform that standard pedotheque is housed at sample box;
Described the first data pretreatment unit, carries out pre-service for the spectroscopic data of the terahertz pulse time domain waveform to standard pedotheque;
Described data modeling unit, for by chemometrics method, pretreated different standard pedotheque spectroscopic data being carried out to mathematical modeling, builds fingerprint spectrum library, sets up the relationship between kind and the concentration of spectrum and heavy metal-polluted soil.
10. device as claimed in claim 7, is characterized in that, described testing sample comparing module comprises the second data acquisition unit, the second data pretreatment unit and testing sample data capture unit;
Described the second data acquisition unit, detects for the heavy metal contamination to the pretreated pedotheque to be measured of sample box, obtains the terahertz pulse time domain waveform of pedotheque to be measured;
Described the second data pretreatment unit, carries out pre-service for the spectroscopic data of the terahertz pulse time domain waveform to pedotheque to be measured;
Described testing sample data capture unit, for the standard pedotheque spectroscopic data of pretreated pedotheque spectroscopic data to be measured and fingerprint spectrum library is compared, by the relationship between kind and the concentration of described spectrum and heavy metal-polluted soil, obtain the heavy metal data of pedotheque to be measured.
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| CN109580443A (en) * | 2019-01-15 | 2019-04-05 | 上海理工大学 | Using the method for metallic particles content in Terahertz Technology detection substance |
| CN110987853A (en) * | 2019-11-08 | 2020-04-10 | 北京农业信息技术研究中心 | Method and device for predicting soil lead pollution degree based on terahertz spectrum |
| CN110987853B (en) * | 2019-11-08 | 2022-02-11 | 北京农业信息技术研究中心 | Method and device for predicting soil lead pollution degree based on terahertz spectrum |
| CN113791040A (en) * | 2021-07-20 | 2021-12-14 | 广州华清环境监测有限公司 | Soil heavy metal detection method and system |
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