CN110261346A - A method of quickly detecting PVC content in soil based near infrared spectrum - Google Patents
A method of quickly detecting PVC content in soil based near infrared spectrum Download PDFInfo
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- 239000002689 soil Substances 0.000 title claims abstract description 50
- 238000002329 infrared spectrum Methods 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 30
- 229920003023 plastic Polymers 0.000 claims abstract description 29
- 239000004033 plastic Substances 0.000 claims abstract description 29
- 238000001514 detection method Methods 0.000 claims abstract description 20
- 239000002344 surface layer Substances 0.000 claims abstract description 5
- 239000000356 contaminant Substances 0.000 claims abstract description 4
- 239000003814 drug Substances 0.000 claims abstract description 3
- 229940079593 drug Drugs 0.000 claims abstract description 3
- 239000004800 polyvinyl chloride Substances 0.000 claims description 35
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 33
- 230000003595 spectral effect Effects 0.000 claims description 13
- 238000001228 spectrum Methods 0.000 claims description 12
- 238000005259 measurement Methods 0.000 claims description 6
- 238000007605 air drying Methods 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 2
- 230000001419 dependent effect Effects 0.000 claims description 2
- 238000011156 evaluation Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 3
- 238000004611 spectroscopical analysis Methods 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000004458 analytical method Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000001066 destructive effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000004227 thermal cracking Methods 0.000 description 2
- 238000012935 Averaging Methods 0.000 description 1
- 229920000426 Microplastic Polymers 0.000 description 1
- 238000001237 Raman spectrum Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 238000009614 chemical analysis method Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 230000005283 ground state Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000002381 microspectrum Methods 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000009659 non-destructive testing Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000045 pyrolysis gas chromatography Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 238000012706 support-vector machine Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
- G01N2021/3572—Preparation of samples, e.g. salt matrices
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Abstract
The invention discloses a kind of methods that PVC content in soil is quickly detected based near infrared spectrum, belong to spectroscopy, environmental pollution detection field, the following steps are included: (1) takes the soil of the surface layer depths 0~30cm, grinds, sieve with 100 mesh sieve after being air-dried under room temperature ventilated environment；(2) at least 15 sample tablettings, each 0.3g are taken；(3) atlas of near infrared spectra of sample tabletting prepared by acquisition step (2)；(4) it is 110 that the regularization parameter gam of setting LS-SVM algorithm, which is the kernel parameter sig2 of 256, LS-SVM algorithm,.In the LS-SVM detection model that the near infrared spectrum data input of the drug tabletting of step (3) acquisition is established, the contaminant capacity of PVC plastic in soil is obtained.The micro- plastic content detection method of PVC type based on near-infrared spectrum technique is not necessarily to extract doubtful micro- plastic flakes in pedotheque by Density Separation, can save time and cost.Furthermore the prediction model of PVC content in soil is established by LS-SVM method, prediction accuracy is high.
Description
Technical field
The present invention relates to spectroscopy, environmental pollution detection field, specifically, being related to a kind of quick based near infrared spectrum
The method for detecting PVC content in soil.
Background technique
Micro- plastics refer to plastic pollution object of the partial size less than 5mm in environment comprising fragment, fiber, particle, film etc. are no
Same morphotype, chemical composition and density are variant and source is various.Micro- plastic pollution has become global environment problem,
Source, abundance and its ecological effect of micro- plastics are by common concern especially in ocean and tidal flat environment.Research shows that annual
The micro- plastic content for entering Europe and North America agricultural land soil by sources such as sludge is respectively 63000-430000 and 44000-
300000 tons, far more than the general input of micro- plastics in the global ocean surface water estimated at present, 93000-236000 tons, therefore
Micro- plastic pollution should also cause enough attention in the especially soil of land.
The method of micro- plastic content mainly has three classes in detection environmental sample at present, first is that destructive chemical analysis method
Such as thermal cracking gas chromatography Mass Spectrometry (Py-GC/MS), after doubtful micro- plastic pellet thermal cracking in detection environmental sample
Product analyze its polymer type and content；Second is that mainly having scanning electricity in conjunction with the method for visual discrimination and non-destructive testing
Sub- microscope (SEM) method and the microspectrum technology for identifying individual particle polymer type according to chemical feature, such as micro- Fu
In infrared technique and micro Raman spectra technology in leaf.Since soil is organic matter, clay, minerals, the mixture of liquid etc.,
It is also the habitat of geobiont, complicated ingredient will lead to the difficulty of analysis detection in soil, therefore first two method is being examined
It needs to carry out complicated micro- plastics extraction separation process before survey.Third is that based near infrared spectrum or high light spectrum image-forming technology to soil-like
Micro- plastics in product carry out the qualitative and quantitative detection of quick nondestructive, and this analysis method is not necessarily to carry out complicated sample treatment,
But existing research accuracy is not high enough.
Polyvinyl chloride (PVC) is the plastics that yield is most in the world, therefore PVC is to may cause the most micro- plastics of pollution
Type.Near infrared spectrum is mainly since the anharmonicity of molecular vibration makes molecular vibration from ground state to generation when high energy order transition
, near infrared spectrum record be in molecule the frequency multiplication of the fundamental vibration of single chemical bond and with sum of fundamental frequencies information, near infrared light
In spectral limit, the frequency multiplication and sum of fundamental frequencies of mainly hydric group X-H (X=C, N, O) vibration of measurement absorb.Sample does not need pre- place
It manages, light penetration depth is big near infrared region, near-infrared spectrum technique is directly measured with diffusing reflection technology to sample, together
When also there is analysis to have non-destructive, analysis speed fast, telemetering and analysis in real time, measurement favorable reproducibility, applicable
The advantages that sample scope is wide, analysis cost is lower, the requirement to operator is lower.
Summary of the invention
It is an object of the present invention to provide a kind of methods that PVC content in soil is quickly detected based near infrared spectrum, intend knot
The method for closing Chemical Measurement, the model of PVC content in prediction soil is established by the near infrared spectrum data of acquisition, and is passed through
PVC content in the model monitoring soil, entire method is convenient and simple, easily operated.
To achieve the goals above, the side provided by the invention that PVC content in soil is quickly detected based near infrared spectrum
Method the following steps are included:
(1) soil for taking the surface layer depths 0~30cm is ground after air-drying under room temperature ventilated environment, broken to sieve with 100 mesh sieve；
(2) at least 15 sample tablettings, each 0.3g are taken；
(3) near infrared spectrum data of sample tabletting prepared by acquisition step (2)；
(4) it by the near infrared spectrum data input detection model of the drug tabletting of step (3) acquisition, obtains in soil
The contaminant capacity of PVC plastic.
The method for building up of detection model are as follows:
(4-1) soil is ground after air-drying, broken to sieve with 100 mesh sieve；
Polyvinyl chloride standard items are added in soil and are uniformly mixed by the concentration gradient set by (4-2)；
(4-3) carries out tabletting to the sample that step (4-2) is mixed into, and sample, and the near infrared spectrum of collecting sample is made
Data；
(4-4), using spectral information as dependent variable, is supported using polyvinyl chloride concentration in soil as independent variable using least square
Vector machine (LS-SVM) algorithm establishes the quantitative detection model of the micro- plastic content of polyvinyl chloride type in spectral signal and soil.If
It is 110 that the regularization parameter gam for setting LS-SVM algorithm, which is the kernel parameter sig2 of 256, LS-SVM algorithm,.
The model-evaluation index that the quantitative detection model of the micro- plastic content of polyvinyl chloride type uses in soil has determining system
Number, modeling root-mean-square error, predicted root mean square error and remaining predicted deviation.
Acquiring the spectral conditions of spectrometer used in atlas of near infrared spectra are as follows: spectral wavelength ranges are 900~1700nm, point
Resolution is 10nm.Spectrometer preheats 15min and carries out blackboard and blank correct operation before carrying out spectral measurement.Setting 400
The spectra collection parameter of a point, by asking the average value scanned three times to obtain spectrum, spectra re-recorded information in this reflection mode.
Compared with prior art, the invention has the benefit that
The present invention is compared with existing micro- plastic content detection method, the micro- modeling of PVC type based on near-infrared spectrum technique
Expect that detection method of content is not necessarily to extract doubtful micro- plastic flakes in pedotheque by Density Separation, time and cost can be saved.
Furthermore the prediction model of PVC content in soil is established by LS-SVM method, prediction accuracy is high.
Detailed description of the invention
Fig. 1 is the quantitative inspection for quickly detecting the method for PVC content in soil in the embodiment of the present invention based near infrared spectrum
Survey model foundation flow chart；
Fig. 2 is near infrared spectrometer acquisition system figure in the embodiment of the present invention；
Fig. 3 is the original atlas of near infrared spectra obtained in the embodiment of the present invention；
Fig. 4 is the forecast set true value and predicted value fitted figure of the micro- plastic content of P in soil VC in the embodiment of the present invention.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, with reference to embodiments and its attached drawing is to this hair
It is bright to be described further.
Embodiment
Referring to Fig. 1 to Fig. 4, the method that PVC content in soil is quickly detected based near infrared spectrum of the present embodiment includes
Following steps:
(1) preparation of soil and micro- plastic sample
The dark brown earth collected from the Greater Hinggan Mountains in Heilongjiang is selected, for soil in acidity, there are more rich organic matter, humic in surface layer
The accumulation of matter is more.It mills and sieves with 100 mesh sieve after soil is air-dried under room temperature ventilated environment, obtain soil of the partial size less than 150 μm
Earth.Since polyvinyl chloride (PVC) is the maximum general-purpose plastics of yield in the world, PVC standard items, PVC standard items powder are selected
The average grain diameter at end is 107 μm.
(2) preparation of sample
PVC standard items powder is added by a certain concentration gradient (0.1%, 0.2%, 0.5%, 1%, 2%, 5%, 10%)
It in soil and is uniformly mixed, each gradient has 15 identical samples.Above-mentioned configured sample is pressed into round sample,
Diameter is 10mm, with a thickness of 1mm.In addition, 10 blank soil samples of setting and 10 PVC standard items samples compare, it is above-mentioned
Altogether 125 sample tablettings and the micro- plastic pollution for preventing other sources is placed in aluminium box.
(3) acquisition of near infrared spectrum
Using the portable near infrared spectrometer in Fig. 2, sample is placed on its scanning window.900-1700nm's
Spectral information, resolution ratio 10nm are acquired in acquisition range.Before carrying out spectral measurement, instrument should preheat 15min and carry out
Blackboard and blank correct operation.Spectra collection parameter provided with 400 points, by asking the average value scanned three times to obtain light
Spectrum, the spectrum of sample prepared by recording step (2) in this reflection mode, each soil tabletting obverse and reverse respectively in triplicate
Scanning collection operation, original spectrum are as shown in Figure 3.
(4) processing of near infrared spectrum data
Each sample obtains 6 near infrared spectrums in step 3, is averaging spectrum to it, by being averaged for 125 samples
Spectroscopic data is spliced into the matrix of a 125x400.Using least square method supporting vector machine (least squares support
Vector machine, LS-SVM) regression algorithm is used for quickly detecting the micro- plastic content of PVC type in soil, and is arranged
The regularization parameter gam of LS-SVM algorithm is that the kernel parameter sig2 of 256, LS-SVM algorithm is 110.Wherein LS-SVM algorithm is built
Mould the result shows that, forecast set RP2 be 0.9873, RPD 8.5611, show that model prediction result is fine, forecast set true value with
The fitted figure of predicted value is as shown in Figure 4.
(5) near infrared spectrum data of object detection area is acquired
Acquisition needs the soil of detection zone, takes the soil of surface layer 0-30cm depth, grinds after air-drying under room temperature ventilated environment
It is broken to sieve with 100 mesh sieve；15 sample tablettings are taken, take 0.3g every time；After the near infrared spectrum data for acquiring sample, input is had built up
Model, PVC plastic contaminant capacity in the soil predicted.
Claims (6)
1. a kind of method for quickly detecting PVC content in soil based near infrared spectrum, which comprises the following steps:
(1) soil for taking the surface layer depths 0~30cm is ground after air-drying under room temperature ventilated environment, broken to sieve with 100 mesh sieve；
(2) at least 15 sample tablettings, each 0.3g are taken；
(3) near infrared spectrum data of sample tabletting prepared by acquisition step (2)；
(4) by the near infrared spectrum data input detection model of the drug tabletting of step (3) acquisition, PVC plastic in soil is obtained
The contaminant capacity of material.
2. the method according to claim 1 for quickly being detected PVC content in soil based near infrared spectrum, feature are existed
In the method for building up of detection model described in step (4) are as follows:
(4-1) soil is ground after air-drying, broken to sieve with 100 mesh sieve；
Polyvinyl chloride standard items are added in soil and are uniformly mixed by the concentration gradient set by (4-2)；
(4-3) carries out tabletting to the sample that step (4-2) is mixed into, and sample, and the near infrared spectrum data of collecting sample is made；
(4-4), using spectral information as dependent variable, utilizes least square supporting vector using polyvinyl chloride concentration in soil as independent variable
Machine algorithm establishes the quantitative detection model of the micro- plastic content of polyvinyl chloride type in spectral signal and soil, least square support to
The regularization parameter gam of amount machine algorithm is 256, and kernel parameter sig2 is 110.
3. the method according to claim 2 for quickly being detected PVC content in soil based near infrared spectrum, feature are existed
In the model evaluation that the quantitative detection model of the micro- plastic content of polyvinyl chloride type uses in soil described in step (4-4)
Index has a determining coefficient, modeling root-mean-square error, predicted root mean square error and remaining predicted deviation, setting least square support to
The regularization parameter gam of amount machine algorithm is 256, and kernel parameter sig2 is 110.
4. the method according to claim 2 for quickly being detected PVC content in soil based near infrared spectrum, feature are existed
In the spectral conditions of spectrometer used in acquisition atlas of near infrared spectra in step (3) and step (4-3) are as follows: spectral wavelength ranges
For 900~1700nm, resolution ratio 10nm.
5. the method according to claim 4 for quickly being detected PVC content in soil based near infrared spectrum, feature are existed
In the spectrometer preheats 15min and carry out blackboard and blank correct operation before carrying out spectral measurement.
6. the method according to claim 5 for quickly being detected PVC content in soil based near infrared spectrum, feature are existed
In, the spectra collection parameter of 400 points is set, by asking the average value scanned three times to obtain spectrum, recording light in this reflection mode
Spectrum information.
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Cited By (3)
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| CN113155753A (en) * | 2021-05-17 | 2021-07-23 | 华南农业大学 | Farmland surface soil micro-plastic detection method and system |
| CN116952923A (en) * | 2023-07-27 | 2023-10-27 | 南京大学 | Machine learning-based micro-plastic on-site high-precision monitoring method and system |
| CN118443538A (en) * | 2024-05-06 | 2024-08-06 | 中国环境监测总站 | Soil microplastic detection method and system |
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