CN112903349A - Method for extracting and detecting micro-plastics in urban river sediment - Google Patents

Method for extracting and detecting micro-plastics in urban river sediment Download PDF

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CN112903349A
CN112903349A CN202110067908.4A CN202110067908A CN112903349A CN 112903349 A CN112903349 A CN 112903349A CN 202110067908 A CN202110067908 A CN 202110067908A CN 112903349 A CN112903349 A CN 112903349A
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plastic
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plastics
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宋丹丹
王秀莉
尚玉俊
庞海岩
宋晓宇
庄玉伟
周连伟
张金玉
李珂庆
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High and New Technology Research Center of Henan Academy of Sciences
Henan Academy of Sciences
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Abstract

The invention discloses a method for extracting and detecting micro-plastics in urban riverway sediments, and belongs to the field of detection of environmental pollutants. The method comprises the following steps: drying the deposit, and then carrying out flotation, digestion, filtration, re-flotation and filtration to obtain a micro plastic filtration membrane sample with a purer substrate; and (2) adopting a Lovins microscopic coordinate slide to perform block segmentation on the filtering membrane sample, utilizing the microscopic coordinate slide to perform coordinate labeling on the micro-plastic, observing, identifying, photographing and counting the micro-plastic by using a combination type/biological microscope, and analyzing and identifying the suspected micro-plastic with smaller size by adopting a transmission mode or an Attenuated Total Reflection (ATR) mode of a Fourier transform microscopic infrared spectrometer (mu-FTIR), and finally obtaining the distribution result of the abundance, size, structure and morphological characteristics of the micro-plastic in the sediment. According to the characteristic that the content of organic matters in the sediments of the urban riverway is high, the secondary flotation treatment of the digestion solution is provided, the separation effect of the micro-plastics is obvious, the obtained micro-plastic filter membrane substrate is pure, and the interference in the subsequent micro-plastic measurement is greatly reduced; the coordinate numbering is carried out on the micro-plastic sample on the filter membrane by adopting the Lovins micro-coordinate slide, so that the micro-plastic can be rapidly and accurately counted and analyzed, and the repetition and the omission of the detection of the micro-plastic sample are effectively avoided.

Description

Method for extracting and detecting micro-plastics in urban river sediment
Technical Field
The invention discloses a method for extracting and analyzing micro-plastics in urban riverway sediments, and belongs to the field of detection of environmental pollutants.
Background
The plastic product has the characteristics of light weight, portability, durability, low price and the like, and is widely applied to the aspects of food packaging, industry and agriculture, medical treatment and the like. However, with the ever-increasing production of plastics, the low recovery of plastics and the improper disposal of plastics contaminants, there is an increasing accumulation of these in the environment. According to statistical data, 2016 year is over 3 hundred million tons/year of global plastic pollution. Plastic pollution is now spread over land, rivers and oceans, resulting in white pollution in the environment, and these plastic pollutants are extremely difficult to degrade and can remain in the environment for decades or even hundreds of years.
Plastics in the environment are degraded, embrittled and broken under the action of physical (such as wave action and sand friction), chemical (such as ultraviolet radiation) and biological action for a long time, and are slowly decomposed into plastic particles or fragments with the size of less than 5mm, which are defined as micro plastics. As the micro plastic is used as a kind of emerging pollutants which are continuously increased in the environment, the micro plastic has a larger specific surface area and lower surface polarity, and can enrich a large amount of environmental pollutants, including heavy metal ions, persistent organic pollutants, environmental hormones and the like. Microplastics, which act as carriers for these contaminants, are easily ingested by organisms and can accumulate in the food chain, thereby potentially posing a serious threat to ecosystem and human health. Recent studies found that micropolastics were detected in human placental tissue, which found that micropolastics could appear in various parts of the placenta (maternal, fetal and amniotic membranes), and confirmed that these micropolastics carry endocrine disrupting substances that could have a long-term effect on human health (Ragusa et al, 2021).
In recent years, a great deal of research on micro-plastics has been conducted at home and abroad, but most of them are focused on marine environments. Research shows that the micro-plastics in the marine environment mainly come from the input of the land source micro-plastics, while rivers are important ways for transmitting the micro-plastics to the sea in the land, and urban rivers which are greatly influenced by human activities often show higher micro-plastic occurrence level and pollution risk. Urban rivers are subject to greater micro-plastic pollution than fresh water systems in less populated areas. The urban river sediment is a possible storage base of the land source micro-plastic and is also a source of the marine micro-plastic, is a result of long-term action of a water area and land interface, and reflects important information of migration and tendency of pollutants.
Therefore, the deep research on the micro-plastic pollution in the urban river sediment can provide basic data and scientific basis for the ecological risk evaluation and pollution control of the micro-plastic in the urban river environment in the future of China. However, since the organic matter content of sediments in urban rivers is particularly high, the micro-plastics and the organic matters are often wrapped together, and the micro-plastic filter membrane sample base which cannot be obtained by adopting conventional density flotation is complex, the difficulty of quantitative and qualitative analysis of the micro-plastics is increased, so that researchers try to increase the previous digestion step to improve the organic matter oxidation efficiency (CN 111426545A), but the residual organic matter carbon remaining on the filter membrane after digestion and filtration still interferes with the subsequent analysis of the micro-plastics; in addition, when the microscope examined, because when microscope magnification was high, the visual field scope can reduce, can not observe the micro plastics on the whole filter membrane under a field of vision, need constantly to move the filter membrane and observe, often can cause the repetition that the micro plastics sample detected and leak to examine, had reduced the degree of accuracy that the micro plastics detected. (Ragusa A, Svelato A, Santacroce C, et al. Plastic: First evidence of plastics in human Plastic International,2021,146:106274.)
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for extracting and detecting micro-plastics in urban river sediments, which can be used for simply, quickly, efficiently and accurately extracting and detecting the micro-plastics in the urban river sediments.
In order to realize the purpose of the invention, the invention adopts the technical scheme that: performing density flotation separation, organic matter oxidation digestion, re-flotation separation, Lovins microscopic coordinate slide assisted micro plastic microscopic microscopy and Fourier transform microscopic infrared spectrometer analysis on the micro plastic in the sediment sample. The method comprises the following specific steps:
1. density flotation separation of sediment sample: drying the sediment sample to constant weight, sieving, collecting micro plastic on the sieve, observing and counting through a magnifying glass, and measuring the particle size under the sieve<1mm sediment is subjected to micro-plastic flotation and separation; placing the sediment in a container, adding a saturated NaCl solution, magnetically stirring for a certain time, continuously and slowly adding the saturated NaCl solution to the bottle mouth, standing overnight, continuously adding the saturated NaCl solution into the container until the upper suspension completely overflows, and collecting an overflow liquid; then using ZnCl2Solution (1.50 g/cm)3) Repeating the flotation steps, mixing the first and second flotation overflow liquids, sieving with 500 mesh sieve, transferring the oversize material to the containerIn the device.
2. Oxidizing and digesting organic matters: adding hydrogen peroxide (30 mass percent) or a mixed solution of hydrogen peroxide (30 mass percent) and nitric acid (65 mass percent) into the container in which the micro-plastic is collected after the density flotation for digestion; the digestion temperature is 30-60 ℃, and the digestion time is 2-12 h.
3. Re-flotation separation: pumping the organic matter oxidation digestion solution obtained in the step (2) onto a glass cellulose filter membrane, and then putting the filter membrane into ZnCl2And performing secondary flotation in the flotation solution. At this time, the organic residue carbonized by digestion is separated from the micro plastic. And finally, carrying out suction filtration on the overflowing liquid again to collect the micro-plastic on the cellulose nitrate filter membrane, placing the filter membrane in a culture dish, and airing at room temperature.
4. Microscopic examination and Fourier transform microscopic infrared spectrometer analysis: and (3) carrying out block segmentation on the filtering membrane sample obtained in the step (3) by adopting a Lovins microscopic coordinate slide, carrying out coordinate labeling, observing, identifying, photographing and counting on the micro-plastic by adopting a microscope, analyzing and identifying the suspected micro-plastic with smaller size by adopting a transmission mode or an Attenuated Total Reflection (ATR) mode of a Fourier transform microscopic infrared spectrometer (mu-FTIR), and finally obtaining the distribution result of the abundance, size, structure and morphological characteristics of the micro-plastic in the sediment.
The invention has the beneficial effects that:
(1) after the flotation solution is digested, the method for refloating the digestion solution is adopted to extract and separate the micro-plastic in the urban river sediment, so that the residual carbon substances generated after the digestion of the organic matters can be well separated from the micro-plastic, a micro-plastic filter membrane sample with a purer substrate is obtained, the separation effect on the micro-plastic is good, and the interference of the residual organic matters during microscopic examination and mu-FTIR identification is greatly reduced.
(2) The invention adopts a Lovins microscopic coordinate slide to carry out coordinate labeling on the micro plastic particles during microscopic examination of the micro plastic microscope, wherein the Lovins microscopic coordinate slide consists of 1100 micro plastic particles with the area of 1mm2The minimum scale of the grid ruler is 0.1mm, and the particle size of the micro plastic particles can be quickly estimated. By adopting Lovins microscopic coordinate glass slide to carry out block segmentation on the collected filter membrane sample of the micro-plastic and utilizing the microscopic coordinate glass slide to carry out coordinate labeling on the micro-plastic, the micro-plastic on the filter membrane can be quickly and accurately observed and counted, the repetition and omission of the detection of the micro-plastic sample caused by the fact that the micro-plastic on the whole filter membrane cannot be observed under one visual field due to the improvement of the magnification of a microscope and the reduction of the visual field range are effectively avoided, and the microscopic examination efficiency and accuracy of the micro-plastic microscope are obviously improved. In addition, for suspected micro-plastics and particles with small sizes which are difficult to distinguish through a microscope, the transmission mode or the Attenuated Total Reflection (ATR) mode of a Fourier transform microscopic infrared spectrometer (mu-FTIR) is adopted for analysis and identification, and the accuracy of micro-plastic identification is improved.
(3) Compared with the existing method, the method for extracting, analyzing and identifying the micro-plastic greatly shortens the analysis time and obviously improves the accuracy of analysis of the micro-plastic.
Drawings
FIG. 1 is a photograph of the microplastic particles obtained on the membrane before and after refloatation in example 1 of the present invention, 1-before refloatation, 2-after refloatation;
FIG. 2 is a 40 times and 100 times magnification photograph of a coordinate microscopic image of the microplastic particle of example 1 of the present invention; FIG. 3 is a micrograph and corresponding IR spectra of microplastic particles of example 1 of the present invention, wherein the microplastic particles are 1-polystyrene, 2-polypropylene, 3-polyethylene, 4-polyester resin, and 5-polyethylene-polypropylene blend.
FIG. 4 shows the distribution characteristics of the size (1), shape (2) and color (3) of the micro-plastic in the deposit according to example 2 of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, but is not limited thereto.
Example 1
The invention provides a method for extracting and analyzing micro-plastics in urban riverway sediments, which comprises the following specific steps:
(1) sampling: selecting a river channel in the urban area of Zhengzhou city, and collecting surface sediments (0-5 cm) by adopting a stainless steel mud sampler after determining a sampling station. All sediment samples are put into an aluminum foil sealing bag for sealing and then transported back to a laboratory, impurities such as gravel, shells, plant residues and the like in the samples are removed, and then the samples are stored in a refrigerator at low temperature.
(2) Flotation: drying the sediment sample to constant weight at 60 ℃ by using an oven, then lightly pressing large particles by using a mortar, sieving a certain amount of sediment sample by using standard stainless steel sieves with 18 meshes (aperture diameter of 1mm) and 4 meshes (aperture diameter of 4.8mm), removing plastic products or sand stones with overlarge sizes, and collecting micro plastic with the size of 1-5 mm for visual inspection and statistics. Undersize sediment sample (<1mm) is subjected to micro-plastic flotation extraction separation. 100g of the above-mentioned sieved sediment was weighed into a 500ml conical flask, and 300ml of a saturated sodium chloride solution was added thereto, followed by stirring with a magnetic stirrer for 20 min. The saturated NaCl solution was added slowly to the bottle mouth and left overnight. Then, continuously adding saturated NaCl solution into the conical flask until the upper suspension completely overflows, collecting overflow liquid, washing the outer wall of the conical flask by using ultrapure water, and combining the upper clear liquid in the conical flask with the overflow liquid; adding 300mL of ZnCl into the sample after flotation2Solution (1.50 g/cm)3) And repeating the extraction steps, combining the first flotation overflow liquid and the second flotation overflow liquid, sieving the mixture by a 500-mesh stainless steel sieve, and transferring substances on the sieve into a volumetric flask by ultrapure water, wherein the volume of the substances is not more than 25 ml.
(3) Organic matter oxidation digestion
Adding 30% by mass of hydrogen peroxide into the volumetric flask collected with the micro-plastic or adding hydrogen peroxide into the volumetric flask with the micro-plastic collected with the micro-plastic in a volume ratio of 1:2 (30 mass percent) and concentrated nitric acid (65 mass percent) in a constant-temperature water bath for 2-4 h at the digestion temperature of 30-60 ℃. Then, a vacuum pump glass sand core filter device is adopted to collect the micro-plastic on a glass cellulose filter membrane with the aperture of 0.45 mu m. Research shows that when hydrogen peroxide (30%) and nitric acid (65%) in a volume ratio of 1:2 are added to the sediments with more plant residues during digestion, organic matters are more completely digested, the digestion temperature is 60 ℃, and the digestion is carried out for 2 hours.
(4) Refloatation
Putting the filter membrane into ZnCl2And (3) performing secondary flotation in the flotation solution, wherein the flotation method is the same as the step 2, collecting the overflowing liquid, and collecting the micro plastic on a cellulose nitrate filter membrane with the aperture of 0.45 mu m by using a glass sand core filter filtering device of a vacuum pump again. And finally, quickly and stably placing the filter membrane in a clean and dry culture dish, airing at room temperature, and correspondingly marking each culture dish. A group of blank controls is arranged in each experiment to eliminate the pollution of micro-plastics in the experimental operation process and air. The micro plastic particles on the filter membrane obtained before and after the refloatation are shown in figure 1. It can be seen that the organic carbon residue material on the filter membrane is significantly reduced by the refloatation, which provides a favourable environment for the subsequent determination of the microplastics.
(5) Microscopic microscopy and Fourier transform microscopic infrared spectrometer analysis
Firstly, a Lovins microscopic coordinate slide is adopted to carry out block segmentation on the filtering membrane sample, the microscopic coordinate slide is utilized to carry out coordinate labeling on the micro-plastic, and a biological microscope is adopted to carry out observation, identification, photographing and statistics on the micro-plastic. For suspected micro-plastic and particles with small size which are difficult to distinguish by microscope, the transmission mode or Attenuated Total Reflection (ATR) mode of fourier transform microscopic infrared spectrometer (μ -FTIR) is adopted for analysis and identification, and the obtained micro-plastic microscope image and the identification and analysis of μ -FTIR structure are shown in fig. 2 and fig. 3. As can be seen from FIG. 2, the counting of the microplastic particles on the filter was performed rapidly and accurately by means of Lovins microscope slides. The micro plastic structure extracted from the river channel by the method of the invention is found to be various types of polystyrene, polypropylene, polyethylene, polyester resin and polyethylene-polypropylene mixture through the structural identification of 3 mu-FTIR.
Example 2
Selecting an east wind channel river channel of a central urban area of Zhengzhou city to investigate and sample, and analyzing the extraction of the micro-plastic in the sediment, wherein the method comprises the following specific steps:
(1) sampling: after the sampling station position is determined, 3 parallel sampling points are selected, 3 sediment samples are collected from each parallel sampling point, a stainless steel mud sampler is selected as a sampling tool, and surface sediments (0-5 cm) are collected. All sediment samples are put into an aluminum foil sealing bag for sealing and then transported back to a laboratory, impurities such as gravel, shells, plant residues and the like in the samples are removed, and then the samples are stored in a refrigerator at low temperature.
(2) Flotation: drying the sediment sample to constant weight at 60 ℃ by using an oven, then lightly pressing large particles by using a mortar, sieving a certain amount of sediment sample by using standard stainless steel sieves with 18 meshes (aperture diameter of 1mm) and 4 meshes (aperture diameter of 4.8mm), removing plastic products or sand stones with overlarge sizes, and collecting micro plastic with the size of 1-5 mm for visual inspection and statistics. Undersize sediment sample (<1mm) is subjected to micro-plastic flotation extraction separation. 100g of the above-mentioned sieved sediment was weighed into a 500ml conical flask, and 300ml of a saturated sodium chloride solution was added thereto, followed by stirring with a magnetic stirrer for 20 min. The saturated NaCl solution was added slowly to the bottle mouth and left overnight. Then, continuously adding saturated NaCl solution into the conical flask until the upper suspension completely overflows, collecting overflow liquid, washing the outer wall of the conical flask by using ultrapure water, and combining the upper clear liquid in the conical flask with the overflow liquid; adding 300mL of ZnCl into the sample after flotation2Solution (1.50 g/cm)3) And repeating the extraction steps, combining the first flotation overflow liquid and the second flotation overflow liquid, sieving the mixture by a 500-mesh stainless steel sieve, and transferring substances on the sieve into a volumetric flask by ultrapure water, wherein the volume of the substances is not more than 25 ml.
(3) Oxidizing and digesting organic matters: 40ml of mixed solution of hydrogen peroxide (30 percent by mass) and nitric acid (65 percent by mass) in a volume ratio of 1:2 is added into the volumetric flask with the collected micro-plastics, and digestion is carried out in a constant temperature water bath at 60 ℃ for 2 h. Then, a vacuum pump glass sand core filter device is adopted to collect the micro-plastic on a glass cellulose filter membrane with the aperture of 0.45 mu m.
(4) And (3) re-flotation: putting the filter membrane into ZnCl2And (3) performing secondary flotation in the flotation solution, wherein the flotation method is the same as the step (2), collecting the overflowing liquid, and collecting the micro plastic on a cellulose nitrate filter membrane with the aperture of 0.45 mu m by using a glass sand core filter filtering device of a vacuum pump again. Finally, the filter membrane is quickly and stably placed in a clean and dry culture dish and dried at room temperature,and are numbered correspondingly for each culture dish. A group of blank controls is arranged in each experiment to eliminate the pollution of micro-plastics in the experimental operation process and air.
(5) Microscopic examination and Fourier transform microscopic infrared spectrometer analysis: and (3) adopting a Lovins microscopic coordinate slide to perform block segmentation on the filter membrane sample, utilizing the microscopic coordinate slide to perform coordinate labeling on the micro-plastic, and adopting a body type microscope to perform observation, identification, photographing and counting statistics on the micro-plastic. And analyzing and identifying suspected micro-plastics and particles with small sizes which are difficult to distinguish by a microscope by adopting a transmission mode or an Attenuated Total Reflection (ATR) mode of a Fourier transform microscopic infrared spectrometer (mu-FTIR), so that the abundance of the micro-plastics in the east canal sediments is 611/100 g, and is obviously higher than the pollution abundance of the micro-plastics in other natural fresh water riverways. The results of the size, shape and color distribution characteristics of the micro-plastics are shown in fig. 4(1-3), and it can be seen that the particle size of the micro-plastics in the river channel is mostly 250-1000 μm, and the micro-plastics with the particle size smaller than 1000 μm account for more than 85%; the main shapes of the micro-plastics are fibers, fragments and spheres; the color of the micro-plastic is mainly transparent and white.

Claims (2)

1. A method for extracting and detecting micro-plastics in urban riverway sediments is characterized by comprising the following steps:
(1) density flotation separation of sediment sample: drying the sediment sample to constant weight, sieving, collecting micro plastic on the sieve, observing and counting through a magnifying glass, and measuring the particle size under the sieve<1mm sediment is subjected to micro-plastic flotation and separation; placing the sediment in a container, adding a saturated NaCl solution, magnetically stirring for a certain time, continuously and slowly adding the saturated NaCl solution to the bottle mouth, standing overnight, continuously adding the saturated NaCl solution into the container until the upper suspension completely overflows, and collecting an overflow liquid; then using ZnCl2The solution is subjected to the flotation step, the first flotation overflow liquid and the second flotation overflow liquid are combined and then are sieved by a 500-mesh sieve, and substances on the sieve are transferred into a container;
(2) oxidizing and digesting organic matters: adding hydrogen peroxide or a mixed solution of hydrogen peroxide and nitric acid into the container which collects the micro-plastic after the density flotation for digestion;
(3) re-flotation separation: pumping the organic matter oxidation digestion solution obtained in the step (2) onto a glass cellulose filter membrane, and then putting the filter membrane into ZnCl2Performing secondary flotation in the flotation solution; filtering the overflow liquid again to collect the micro plastic on the cellulose nitrate filter membrane, placing the filter membrane in a culture dish, and airing at room temperature;
(4) microscopic examination and Fourier transform microscopic infrared spectrometer analysis: and (3) carrying out block segmentation on the filtering membrane sample obtained in the step (3) by adopting a Lovins microscopic coordinate slide, carrying out coordinate labeling, observing, identifying, photographing and counting on the micro-plastic by adopting a microscope, carrying out analysis and identification on the suspected micro-plastic with smaller size by adopting a transmission mode or an attenuated total reflection mode of a Fourier transform microscopic infrared spectrometer, and finally obtaining the distribution result of the abundance, size, structure and morphological characteristics of the micro-plastic in the sediment.
2. The method for extracting and detecting the micro-plastics in the urban riverway sediments according to claim 1, wherein the hydrogen peroxide in the step (2) is 30% in mass percentage; the mass percentage content of the nitric acid is 65 percent; the volume ratio of the mixed solution of hydrogen peroxide and nitric acid is 1: 2.
CN202110067908.4A 2021-01-19 2021-01-19 Method for extracting and detecting micro-plastics in urban river sediment Pending CN112903349A (en)

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