CN110186863A - The detection method of the micro- plastic degradation situation in mulch source in a kind of pair of soil - Google Patents
The detection method of the micro- plastic degradation situation in mulch source in a kind of pair of soil Download PDFInfo
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- 239000004033 plastic Substances 0.000 title claims abstract description 67
- 229920003023 plastic Polymers 0.000 title claims abstract description 67
- 239000002689 soil Substances 0.000 title claims abstract description 46
- 238000006731 degradation reaction Methods 0.000 title claims abstract description 35
- 230000015556 catabolic process Effects 0.000 title claims abstract description 33
- 239000002362 mulch Substances 0.000 title claims abstract description 30
- 238000001514 detection method Methods 0.000 title claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 8
- 238000004458 analytical method Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 239000000725 suspension Substances 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000011780 sodium chloride Substances 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 238000013517 stratification Methods 0.000 claims abstract description 3
- 238000000926 separation method Methods 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 229960004756 ethanol Drugs 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000000605 extraction Methods 0.000 claims description 3
- 206010068150 Acoustic shock Diseases 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- 238000009963 fulling Methods 0.000 abstract description 3
- 230000008859 change Effects 0.000 abstract description 2
- 238000010276 construction Methods 0.000 abstract description 2
- 229920001577 copolymer Polymers 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000002329 infrared spectrum Methods 0.000 description 2
- 238000000899 pressurised-fluid extraction Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 241001276618 Mayaca fluviatilis Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000009313 farming Methods 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000010871 livestock manure Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000003895 organic fertilizer Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000007539 photo-oxidation reaction Methods 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229920001896 polybutyrate Polymers 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Classifications
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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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
- G01N23/2251—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion using incident electron beams, e.g. scanning electron microscopy [SEM]
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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
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/071—Investigating materials by wave or particle radiation secondary emission combination of measurements, at least 1 secondary emission
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The detection method of the micro- plastic degradation situation in mulch source in a kind of pair of soil, described method includes following steps: taking soil to be measured, the biggish micro- plastics of partial size are screened out after drying, are then added in saturation NaCl solution, fulling shake is suspended in micro- plastics in solution, standing makes suspension and soil solids stratification, then suspension is poured out, is filtered, the micro- plastics washes of absolute alcohol that will be filtered out, it is placed in drying in vacuum oven again, obtains sample to be tested；Gained sample to be tested is taken, using the variation of Fourier infrared spectrograph, the carbon-based index of the micro- plastics of scanning electron microscope analysis, crystallinity and sample surface morphology, degradation situation is evaluated with this；The method of the present invention is easy, quickly, can with direct viewing into soil the micro- plastic degradation situation of change in mulch source and without destroying micro- plastic construction, can further evaluate ecological risk of the soil after the micro- plastic degradation in mulch source with the method for the present invention.
Description
(1) technical field
The present invention relates to a kind of methods of the micro- plastic degradation situation in mulch source in identification soil environment.
(2) background technique
Micro- plastic pollution has been the hot issue by global concern.The current research in relation to micro- plastic pollution, mostly with
Most of plastic garbage based on marine environment, but in ocean all originates from the human activity of land.However, it is in land ring
Pollution situation in border, especially soil not yet causes enough concerns.Micro- plastics can degrade in soil, and release and all kinds of have
Malicious nocuousness additive can also adsorb the pollutants such as hydrophobic organic compound and the heavy metal in environment in degradation process, to soil
The ecosystem constitutes harm.There are sewage, organic fertilizer, atmospheric sedimentation and agricultural mulching residual in micro- plastic pollution source in soil
Deng.Wherein, plastic film residual has become the main source of micro- plastic pollution in agricultural land soil.China is that mulch covers in the world
The maximum country of lid cultivated area, its area coverage has had reached 1.84 × 10 in recent years7Hectare.It can significantly be mentioned using mulch
High crop yield, but its residue may bring many harm, and such as contaminated soil interferes farming, destroys topsoil knot
Structure hinders liquid manure transporting, influences soil permeability and crop growth, constitutes significant threat to agricultural environment.
Due to being influenced by the soil texture, organic matter and aggregate structure, thus micro- modeling is separated and identified from soil
Expect more difficult than in water and deposit.Currently, the separation of micro- plastics mainly uses for reference in deposit and separates micro- modeling in soil
The correlation technique of material, for example use the methods of Density Separation, air bearing.But these methods can not remove the soil of its surface adhesion
Grain, causes surface topography to have certain deviation.Also researcher proposes to carry out in soil using the method for pressurized fluid extraction (PFE)
The separation of micro- plastics.This method although can in the complex matrices such as quantitative analysis soil micro- plastics content, it can not be obtained
The physical messages such as the partial size of micro- plastics, shape, surface appearance feature in sample, therefore micro- frosting degradation can not be can be visually seen
Situation.Therefore, in view of the complexity of the diversity of soil property and micro- plastics physics, chemical property, it is necessary to develop a kind of needle
Methodological study to the micro- plastic degradation situation in mulch source in soil.
(3) summary of the invention
With the micro- plastics in biodegradable mulch source (tetramethylene adipate copolymer) for object, analyze in simulated environment
The influence degraded to it.Micro- plastics after being degraded using the method that Density Separation is combined with low temperature drying.By infrared
The instruments such as spectrometer, scanning electron microscope analyze the features such as the carbon-based index of micro- plastics and sample surface morphology in degradation process
Variation, to observe the variation of micro- frosting structure.
Technical scheme is as follows:
The detection method of the micro- plastic degradation situation in mulch source in a kind of pair of soil, described method includes following steps:
(1) separation and Extraction of the micro- plastics in mulch source
Soil to be measured is taken, micro- plastics of partial size larger (0.2mm or more) are screened out after dry, are then added to saturation NaCl solution
In, fulling shake is suspended in micro- plastics in solution, and standing makes suspension and soil solids stratification, then suspension is poured out,
It filters (0.45 μm of filter sizes), the micro- plastics washes of absolute alcohol that will be filtered out, then is placed in drying (drying in vacuum oven
20~30 DEG C of temperature, 8~12h of time), obtain sample to be tested；
The method of the micro- plastics washes of absolute alcohol filtered out are as follows: the micro- plastics filtered out are placed in dehydrated alcohol,
Ultrasonic vibration 10min stands 5min, pours out ethyl alcohol later, which is repeated 3 times；
(2) analysis of the micro- plastics in mulch source
Sample to be tested obtained by step (1) is taken, Fourier infrared spectrograph, the micro- plastics carbon of scanning electron microscope analysis are used
The variation of base index, crystallinity and sample surface morphology evaluates degradation situation with this.
The present invention has the advantages that
1, present approach provides the effective ways of the micro- plastic degradation situation identification in mulch source in soil.
2, the method for the present invention is easy to operate, reasonable, is one and meets easy, quick analysis method.
3, the method for the present invention can with direct viewing into soil the micro- plastic degradation situation of change in mulch source and without destroy it is micro-
Plastic construction.
4, ecological risk of the soil after the micro- plastic degradation in mulch source can further be evaluated with the method for the present invention.
(4) Detailed description of the invention
Fig. 1: the microscopic appearance of the micro- plastics in degradation front and back tetramethylene adipate copolymer mulch source；A: before degradation；B: drop
After Xie Liuzhou；
Fig. 2: the infrared spectrum of the micro- plastics in degradation front and back tetramethylene adipate copolymer mulch source；A: before degradation；B: drop
Solution two weeks；C: degradation surrounding；D: degradation six weeks.
(5) specific embodiment
Below by specific embodiment, the present invention is further illustrated, but protection scope of the present invention is not limited in
This.
The tetramethylene adipate copolymer used in following embodiment is purchased from the limited public affairs of plastics rich in Yunnan Province Xuanwei City
Department.
Embodiment 1
(1) degradation experiment
The concentration that the micro- plastics in tetramethylene adipate copolymer mulch source in soil are arranged is 1%, is dispersed in
In soil.24 ± 1 DEG C of environment in the incubator, under 4500lx irradiation, daily 12:12 hours illumination: dark cycle, simulated environment
In degradation behavior.Soil use OECD standard soil: be mainly characterized by 69.5% sand, 20% kaolin, 10% bog moss,
0.5%CaCO3.Its water content will be controlled in 20%-25% after the sieving of 80 mesh of standard soil.
(2) separation and Extraction of the micro- plastics in mulch source
It is sieved using sieve after antecedent soil moisture after taking 10g to degrade to remove the biggish micro- plastics of partial size, then will be after screening
Soil be transferred in saturation NaCl solution, fulling shake is suspended in micro- plastics in solution, and standing keeps suspension and soil solid
The solution for being suspended with the micro- plastics in mulch source, is then transferred in beaker by body layering, is filtered using 0.45 μm of filter.It will obtain
Micro- plastics be placed in 100ml conical flask and be added 50ml dehydrated alcohol, 5min is stood after ultrasonic vibration 10min, is slowly inclined afterwards
Ethyl alcohol out, the step is in triplicate.In order not to destroy micro- frosting structure, filtered product is in 30 DEG C of environment in vacuum
Drying 12 hours in drying box.
(3) analysis of the micro- plastics in mulch source
Use Fourier infrared spectrograph, scanning electron microscope analysis degradation micro- carbon-based finger of plastics in different time periods
The variation of the features such as number, crystallinity and sample surface morphology.
Experimental result:
The micro- frosting in mulch source after degrading six weeks compared with surface relatively smooth before degradation occurs irregular
Sheet layering, and there are many gullies there is (Fig. 1).As can be seen that prolonging with degradation time from Fourier's infrared spectrum
It is long, 3486cm-1There is wider absorption peak and has the tendency that gradually increasing (Fig. 2) in place, which is the absorption peak of hydroxyl.From
The absorption peak variation of degradation front and back is as can be seen that the micro- plastics of PBAT may produce strand under the action ofs photooxidation, hydrolysis etc.
Broken to form hydroxyl.It can be seen that the micro- plastics of tetramethylene adipate copolymer have obvious degradation in soil environment, I
Need further to evaluate the potential ecological risk of the micro- plastics of biodegradable, rationally, specification ground use agricultural film.
Claims (5)
1. the detection method of the micro- plastic degradation situation in mulch source in a kind of pair of soil, which is characterized in that the method includes as follows
Step:
(1) separation and Extraction of the micro- plastics in mulch source
Take soil to be measured, screen out the biggish micro- plastics of partial size after dry, be then added in saturation NaCl solution, fully shake make it is micro-
Plastics are suspended in solution, and standing makes suspension and soil solids stratification, then pour out suspension, are filtered, micro- by what is filtered out
Plastics washes of absolute alcohol, then it is placed in drying in vacuum oven, obtain sample to be tested；
(2) analysis of the micro- plastics in mulch source
Sample to be tested obtained by step (1) is taken, Fourier infrared spectrograph, the carbon-based finger of the micro- plastics of scanning electron microscope analysis are used
The variation of number, crystallinity and sample surface morphology evaluates degradation situation with this.
2. as described in claim 1 to the detection method of the micro- plastic degradation situation in mulch source in soil, which is characterized in that step
(1) in, micro- plastics of partial size 0.2mm or more are screened out after the antecedent soil moisture to be measured.
3. as described in claim 1 to the detection method of the micro- plastic degradation situation in mulch source in soil, which is characterized in that step
(1) in, the filter sizes of the suction filtration are 0.45 μm.
4. as described in claim 1 to the detection method of the micro- plastic degradation situation in mulch source in soil, which is characterized in that step
(1) in, the temperature of the drying is 20~30 DEG C, and the time is 8~12h.
5. as described in claim 1 to the detection method of the micro- plastic degradation situation in mulch source in soil, which is characterized in that step
(1) in, the method for the micro- plastics washes of absolute alcohol filtered out are as follows: the micro- plastics filtered out are placed in dehydrated alcohol, are surpassed
10min is swung in acoustic shock, is stood 5min, is poured out ethyl alcohol later, which is repeated 3 times.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111044472A (en) * | 2019-11-27 | 2020-04-21 | 北京农业智能装备技术研究中心 | Farmland mulching film volatile matter detection device and detection method |
| CN111257539A (en) * | 2020-02-25 | 2020-06-09 | 贵州省烟草科学研究院 | Experimental method for researching response of mulching film degradation characteristics to moisture conditions |
| CN111257464A (en) * | 2020-02-26 | 2020-06-09 | 中国科学院生态环境研究中心 | Method for quantitatively determining micro-plastic in water environment |
| CN112284867A (en) * | 2020-09-23 | 2021-01-29 | 西北农林科技大学 | Method for separating and extracting soil residual micro-plastic |
| CN112304815A (en) * | 2020-10-26 | 2021-02-02 | 中国水产科学研究院黄海水产研究所 | Evaluation method for pollution level of marine sediment micro-plastic |
| CN112525635A (en) * | 2020-11-20 | 2021-03-19 | 哈尔滨工业大学（深圳） | Method for extracting micro-plastic |
| CN112985898A (en) * | 2021-02-09 | 2021-06-18 | 深圳海关工业品检测技术中心 | Method for extracting micro-plastic from recycled plastic or waste plastic |
| CN113075160A (en) * | 2021-03-24 | 2021-07-06 | 浙江工业大学 | Method for rapidly extracting and analyzing micro-plastics in soil based on density separation method |
| CN113155558A (en) * | 2021-02-05 | 2021-07-23 | 北京市理化分析测试中心 | Method for extracting, separating and purifying micro-plastic in soil |
| CN114062071A (en) * | 2021-10-14 | 2022-02-18 | 中国农业科学院农业环境与可持续发展研究所 | Method for quickly separating and detecting plastic from soil |
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| CN112284867A (en) * | 2020-09-23 | 2021-01-29 | 西北农林科技大学 | Method for separating and extracting soil residual micro-plastic |
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| CN112525635B (en) * | 2020-11-20 | 2022-01-04 | 哈尔滨工业大学（深圳） | Method for extracting micro-plastic |
| CN113155558A (en) * | 2021-02-05 | 2021-07-23 | 北京市理化分析测试中心 | Method for extracting, separating and purifying micro-plastic in soil |
| CN113155558B (en) * | 2021-02-05 | 2023-11-24 | 北京市理化分析测试中心 | Method for extracting, separating and purifying microplastic in soil |
| CN112985898A (en) * | 2021-02-09 | 2021-06-18 | 深圳海关工业品检测技术中心 | Method for extracting micro-plastic from recycled plastic or waste plastic |
| CN113075160A (en) * | 2021-03-24 | 2021-07-06 | 浙江工业大学 | Method for rapidly extracting and analyzing micro-plastics in soil based on density separation method |
| CN114062071A (en) * | 2021-10-14 | 2022-02-18 | 中国农业科学院农业环境与可持续发展研究所 | Method for quickly separating and detecting plastic from soil |
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