CN111257464A - Method for quantitatively determining micro-plastic in water environment - Google Patents
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Abstract
A method for quantitatively determining micro-plastic in water environment comprises filtering a water sample in constant volume environment by an enrichment membrane, so that micro-plastic particles are trapped and enriched on the membrane, and nano-plastic enters filtrate; freezing and grinding the enrichment membrane enriched with the micro-plastic, adding distilled water for constant volume mixing, drying and testing to finish the method for quantitatively determining the micro-plastic in the water environment. The invention firstly proposes to separately determine the micro-plastic and the nano-plastic, realizes the micro-plastic (1 mu m) separation and quantitative determination of mu g/L level, and is successfully applied to the actual water sample; the method has the advantages of high sensitivity, high enrichment multiple, green and environment-friendly pretreatment process and simple and convenient operation.
Description
Technical Field
The invention relates to the field of environmental analytical chemistry, in particular to a method for quantitatively determining micro-plastics in a water environment.
Background
Plastics have been widely used in industrial production as well as daily life due to their excellent physicochemical properties. During production, use and recycling, large quantities of plastic can enter the environment. The plastic garbage entering the environment can form plastic particles (micro plastic) with the diameter of 1 mu m-5mm under the actions of solar radiation, mechanical abrasion, biodegradation and the like. In addition, some products such as detergents, skin care products and industrial materials also contain large amounts of artificially added micro-plastics, which may also be released into the environment during preparation, transport and use.
In recent years, micro plastic is a novel pollutant, and the environmental risk and the toxic effect of the micro plastic are concerned by scholars at home and abroad. Toxicological experiments show that the micro-plastic can be taken into the body by invertebrates to influence the growth and the reproduction of the invertebrates, and more seriously, the micro-plastic is easy to be enriched in organisms and then enters a food chain to cause the transfer in the food chain. In addition, the micro plastic is easy to adsorb organic chlorine compounds, polycyclic aromatic hydrocarbons, metal ions and the like, thereby causing compound toxicity. Moreover, the toxic effects of microplastics are strongly related to their concentration level and particle size. Therefore, qualitative and quantitative analysis of microplastics is a prerequisite for the study of their contamination levels and toxic effects.
The qualitative and quantitative methods of the micro-plastic mainly comprise visual inspection, Raman spectroscopy, Fourier transform infrared spectroscopy, thermal cracking-gas chromatography mass spectrometry (Py-GC/MS) and the like. The visual inspection method can only separate micro plastic particles with the particle size of 2-5mm, and the reproducibility and the accuracy of the result are to be improved; raman spectroscopy and Fourier transform infrared spectroscopy can only qualitatively determine the micro-plastics. Py-GC/MS has high sensitivity and low detection limit, and can qualitatively and quantitatively determine the micro plastic. However, the concentration of the micro-plastic in the environment is lower than the detection limit of the instrument, and the toxic effect of the micro-plastic is related to the particle size, so that the separation and enrichment work of the micro-plastic is very important.
At present, the separation and enrichment methods of the micro plastic mainly comprise flotation, filtration, electrostatic separation and magnetic solid-phase separation. The flotation method is to separate by using the density difference of flotation solution and micro plastic, but is easily interfered by similar density substances in water environment, and the method needs further purification and separation; the filtration method is to separate by using the particle size of the micro plastic, but when the aperture of the filtration membrane is smaller, the pores are easy to block, and the micro plastic can be tightly attached to the filtration membrane and is difficult to recover; the electrostatic separation is carried out by utilizing the electrostatic property of the micro-plastic, however, the method can only separate the micro-plastic with the diameter more than or equal to 63 mu m, and can not avoid the interference of other insulating substances; the magnetic solid phase separation is to separate the micro plastic by utilizing silanized iron nano particles through the hydrophobic effect with the micro plastic, and the method is only suitable for cleaning samples and is only effective for the micro plastic with the particle size of more than or equal to 15 mu m. The method can only separate and enrich the micro-plastics with larger size, and the current micro-plastic separation and enrichment method with the diameter less than or equal to 15 mu m is rarely reported.
Disclosure of Invention
In view of the above, one of the main objectives of the present invention is to provide a method for quantitative determination of micro-plastics in an aqueous environment, so as to at least partially solve at least one of the above technical problems.
In order to achieve the above object, the present invention provides a method for quantitatively determining a micro plastic in an aqueous environment, comprising:
filtering the water sample in the constant volume environment by using an enrichment membrane, so that micro plastic particles are intercepted and enriched on the membrane, and nano plastic enters the filtrate;
freezing and grinding the enrichment membrane enriched with the micro-plastic, adding distilled water for constant volume mixing, drying and testing to finish the method for quantitatively determining the micro-plastic in the water environment.
Based on the technical scheme, compared with the prior art, the method for quantitatively determining the micro-plastic in the water environment has at least one of the following advantages:
1. the invention firstly proposes to separately determine the micro-plastic and the nano-plastic, realizes the micro-plastic (1 mu m) separation and quantitative determination of mu g/L level, and is successfully applied to the actual water sample;
2. the sensitivity is high, and the detection limit of the method is 0.10 mug/L (PS) and 0.11 mug/L (PMMA);
3. high enrichment times, green and environment-friendly pretreatment process and simple and convenient operation.
Drawings
FIG. 1 is a schematic diagram of the technical route for quantitatively determining the micro-plastics in the water environment according to the invention;
FIG. 2 is a scanning electron microscope image of a 1 μm pore size glass fiber membrane entrapping enriched PS microplastic particles according to the present invention;
FIG. 3 is a graph showing the effect of a 1 μm glass fiber membrane on the separation of plastic particles of different particle sizes;
FIG. 4 is a Py-GC/MS measurement total ion flow diagram of an inorganic membrane such as a glass fiber membrane according to the present invention;
FIG. 5 is a graph of the effect of filtered water sample volume (50-1000mL) on micro-plastic recovery in the present invention;
FIG. 6 is a graph showing the effect of the concentration of the filtered water sample (10-1000. mu.g/L) on the recovery of the micro-plastic in the present invention;
FIG. 7 is a graph showing the data of the recovery rate of the labeled micro-plastic under the conditions of labeling 10.4. mu.g/L PS micro-plastic and labeling 10.5. mu.g/L PMMA micro-plastic when the present invention is applied to an actual water sample.
Detailed Description
In order that the objects, technical solutions and advantages of the present invention will become more apparent, the present invention will be further described in detail with reference to the accompanying drawings in conjunction with the following specific embodiments.
The invention discloses a method for quantitatively determining micro-plastics in a water environment, which comprises the following steps:
filtering the water sample in the constant volume environment by using an enrichment membrane, so that micro plastic particles are intercepted and enriched on the membrane, and nano plastic enters the filtrate;
freezing and grinding the enrichment membrane enriched with the micro-plastic, adding distilled water for constant volume mixing, drying and testing to finish the method for quantitatively determining the micro-plastic in the water environment.
In some embodiments of the invention, the enrichment membrane comprises any one of a glass fiber membrane, an aluminum oxide membrane, a quartz membrane.
In some embodiments of the invention, when the enrichment membrane is a glass fiber membrane, the glass fiber membrane has a pore size of 0.8 to 1.2 microns, for example, 0.8 microns, 0.9 microns, 1 micron, 1.1 microns, 1.2 microns.
In some embodiments of the invention, the freezing method comprises liquid nitrogen freezing.
In some embodiments of the invention, the freezing time is 4 to 6 minutes, for example, may be 5 minutes.
In some embodiments of the invention, the testing step is performed using thermal cracking-gas chromatography mass spectrometry.
In some embodiments of the invention, the drying step is carried out in a sample cup of the testing instrument.
In some embodiments of the invention, the drying temperature in the drying step is 70 to 90 ℃, for example, may be 80 ℃.
In some embodiments of the present invention, the drying time in the drying step is 40 to 80 minutes, for example, 60 minutes.
In one exemplary embodiment, the method of the present invention for quantitatively determining a micro-plastic in an aqueous environment comprises the steps of:
separating micro-nano plastics: passing 100mL of an environmental water sample through a glass fiber membrane with the aperture of 0.8-1.2 mu m, intercepting the micro plastic (the diameter is 1 mu m-5mm) on the membrane, and allowing the nano plastic (the diameter is 1-999nm) to enter the filtrate;
determination of the microplastics: freezing the glass fiber membrane enriched with the micro-plastic by liquid nitrogen, grinding, fixing the volume in a 1.5mL centrifuge tube, adding deionized water to make the volume of the mixed solution be 1mL, transferring 50 mu L of the mixed solution (comprising the glass fiber membrane and the micro-plastic) into a sample cup, drying, and determining by thermal cracking-gas chromatography-mass spectrometry (Py-GC/MS);
wherein, the micro-plastic can be selectively intercepted and enriched by using inorganic membranes such as glass fiber membranes with the aperture of 0.8-1.2 mu m and the like, and the nano-plastic is not enriched.
The method comprises the following steps of freezing a glass fiber membrane and micro-plastic together by liquid nitrogen, grinding, uniformly mixing and drying at constant volume, and directly carrying out Py-GC/MS (pycnometer-gas chromatography/mass spectrometry), wherein a filter membrane does not interfere with the measurement.
In another exemplary embodiment, the method for quantitatively determining the micro-plastic in the aqueous environment of the present invention uses Polystyrene (PS) and polymethyl methacrylate (PMMA) micro-plastic as a model, and selects a glass fiber membrane with a pore size of 1 μm to selectively enrich the micro-plastic in the environmental water sample, but not enrich the nano-plastic. Then the quantitative determination of Py-GC/MS was carried out on the microplastics. The method comprises the following steps:
step (1): passing 100mL of an environmental water sample through a glass fiber membrane with the aperture of 1 mu m, intercepting the micro-plastic on the membrane, and allowing the nano-plastic to enter the filtrate;
step (2): freezing the glass fiber membrane enriched with the micro-plastic by liquid nitrogen, then quickly grinding, transferring to a 1.5mL centrifuge tube, adding deionized water to enable the volume of the mixed solution to be 1mL, after fully mixing, transferring 50 mu L of the mixed solution comprising the glass fiber membrane and the micro-plastic into a sample cup, and after drying (80 ℃, 1h), determining Py-GC/MS;
and (3): finally, data analysis was performed, and styrene (m/Z104) and methyl methacrylate (m/Z100) were analyzed under selective ion current conditions (SIC).
Toxicological studies of micro-plastics and nano-plastics (1-999nm) show that the micro-plastics and the nano-plastics have different particle sizes and different harms to environmental organisms. Therefore, the separation and measurement of the micro-plastic and the nano-plastic become a great challenge for exploring the environmental effect of the micro-nano plastic. In the experimental process, the glass fiber membrane (with the aperture of 0.8-1.2 μm) can successfully separate the micro-plastic from the nano-plastic, the micro-plastic is trapped in the glass fiber membrane, then the membrane and the micro-plastic are frozen by liquid nitrogen, the membrane and the micro-plastic are quickly ground and transferred to a 1.5mL centrifuge tube, deionized water is added to make the volume of the mixed solution be 1mL, after the mixed solution is fully mixed, 50 μ L of the mixed solution (comprising the glass fiber membrane and the micro-plastic) is transferred to a sample cup, and after the mixed solution is dried, the Py-GC/MS measurement is carried out.
The technical solution of the present invention is further illustrated by the following specific embodiments in conjunction with the accompanying drawings. It should be noted that the following specific examples are given by way of illustration only and the scope of the present invention is not limited thereto.
The chemicals and raw materials used in the following examples were either commercially available or self-prepared by a known preparation method.
Example 1
The method for quantitatively determining the micro-plastic in the water environment, as shown in fig. 1, comprises the following steps:
(1) filtering 100mL of water sample to be detected by using a glass fiber membrane with the aperture of 1 mu m, intercepting and enriching micro plastic particles on the glass fiber membrane, and allowing nano plastic to enter filtrate;
(2) freezing the glass fiber membrane enriched with the micro-plastic by liquid nitrogen, quickly grinding, transferring to a 1.5mL centrifuge tube, adding deionized water to enable the volume of the mixed solution to be 1mL, fully mixing, transferring 50 mu L of the mixed solution (comprising the glass fiber membrane and the micro-plastic) to a sample cup, drying, and determining the thermal cracking-gas chromatography-mass spectrometry (Py-GC/MS);
(3) finally, data analysis was performed, and styrene (m/Z104) and methyl methacrylate (m/Z100) were analyzed under selective ion current conditions (SIC).
In the step (1), a glass fiber membrane with a pore diameter of 1 μm is selected, the glass fiber membrane is made of carbon-free glass fibers, a dense net structure is favorable for retaining enriched micro plastic particles, and as shown in fig. 2, the plastic particles are retained in the net structure of the glass fiber membrane. Moreover, the adsorption effect of the glass fiber membrane on the nano-plastic is low, as shown in fig. 3, the retention rate of the glass fiber membrane with the aperture of 1 μm on the micro-plastic is 90.7% (PS) and 95.8% (PMMA), and the retention rate on the nano-plastic is less than or equal to 15.9(PS is less than or equal to 500nm) and less than or equal to 11.3% (PMMA is less than or equal to 500nm), so that the adsorption rate of the glass fiber membrane with the aperture of 1 μm on the nano-plastic can be ignored, and the micro-plastic and the nano-plastic can be separated.
In the step (2), as shown in fig. 4, since the glass fiber membrane is formed by pressing glass fiber, the measurement of the micro-plastic is not interfered, so that the centrifuge tube containing the membrane and the micro-plastic is put into liquid nitrogen for freezing, the centrifuge tube is clamped out by forceps after about 5min, the centrifuge tube is quickly put into a mortar for grinding together, the mixed solution is carefully transferred back to the centrifuge tube until no obvious particles exist, pure water is added to the centrifuge tube to a constant volume of 1mL, after full mixing, 50 muL of the mixed solution is taken out and transferred into a sample cup, the sample cup is dried at 80 ℃ for 1h, and then Py-GC/MS measurement is directly carried out. Figure 5 investigates the effect of water sample filtration volume on the recovery of this method. Add 10. mu.g of PS and PMMA to 50-1000mL of water, respectively, with a normalized recovery of 72-96% (PS) and 76-95% (PMMA). As can be seen from FIG. 5, under the condition that the addition amount is 10. mu.g, the recovery rate is slightly decreased as the sample volume is increased. However, at a filtration volume of 1L, the recovery was still greater than 71.9%.
Therefore, when the filtering volume is 1L, the volume of the final enrichment solution is 1mL, and the enrichment multiple can reach 1000. After comprehensive consideration, a sample volume of 100mL is selected for the investigation of the water sample concentration on the recovery rate of the micro plastic. As shown in FIG. 6, 100mL of each of the sample solutions having a concentration of 10 to 1000. mu.g/L was passed through a glass fiber membrane, and according to the operation of step (2), a recovery rate of 82 to 117% was obtained. In three replicates with a spiked 100. mu.g/L, the relative standard deviation for PS microplastic (1 μm) was 1.3% and for PMMA microplastic (1 μm) was 1.9%. As can be seen from fig. 6, the recovery rate slightly decreased and then tended to stabilize as the sample concentration increased.
As shown in FIG. 7, when the method is applied to an actual water sample, the recovery rate of the micro-plastic is 81.1-111% under the conditions of adding standard 10.4 mug/L PS and 10.5 mug/L PMMA, and the method is effective and reliable.
Example 2
And (4) quantitatively measuring the micro-plastics in different matrix water bodies.
Firstly, 100mL of different matrix water samples pass through a glass fiber membrane with the aperture of 1 mu m, micro plastic particles are trapped and enriched on the glass fiber membrane, the glass fiber membrane is transferred into a 1.5mL centrifuge tube, liquid nitrogen is frozen for 5min, then the glass fiber membrane is taken out, the glass fiber membrane is quickly ground until no obvious particles exist, the glass fiber membrane is transferred back into the centrifuge tube, and deionized water is added to ensure that the volume of the mixed solution is 1 mL. After vortexing and mixing well, 50. mu.L of the mixed solution was taken in a thermal cracking sample cup, dried and measured. Wherein PS micro-plastics are detected in 6 environmental water samples, the concentration is 1.2-9.2 mug/L, and PMMA micro-plastics are not detected. As shown in Table 1, it is demonstrated that the method can be used for the determination of micro-plastics at the level of μ g/L concentration in an environmental water body.
TABLE 1 determination of micro-plastics in water in actual environmental conditions
ND is lower than detection limit
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A method for quantitatively determining a micro-plastic in an aqueous environment, comprising:
filtering the water sample in the constant volume environment by using an enrichment membrane, so that micro plastic particles are intercepted and enriched on the membrane, and nano plastic enters the filtrate;
freezing and grinding the enrichment membrane enriched with the micro-plastic, adding distilled water for constant volume mixing, drying and testing to finish the method for quantitatively determining the micro-plastic in the water environment.
2. The method of claim 1,
the enrichment membrane comprises any one of a glass fiber membrane, an aluminum oxide membrane and a quartz membrane.
3. The method of claim 2,
when the enrichment membrane is a glass fiber membrane, the pore size of the glass fiber membrane is 0.8 to 1.2 microns.
4. The method of claim 1,
the freezing method comprises liquid nitrogen freezing.
5. The method of claim 1,
the freezing time is 4 to 6 minutes.
6. The method of claim 1,
the testing step adopts thermal cracking-gas chromatography mass spectrometry for determination.
7. The method of claim 1,
the drying step is carried out in a sample cup of the testing instrument.
8. The method of claim 1,
the drying temperature in the drying step is 70 to 90 ℃.
9. The method of claim 1,
the drying time in the drying step is 40 to 80 minutes.
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| CN113109464A (en) * | 2021-03-18 | 2021-07-13 | 广州大学 | Method for quantitatively analyzing nano-plastic in environmental water body |
| CN113109464B (en) * | 2021-03-18 | 2022-11-11 | 广州大学 | Method for quantitatively analyzing nano-plastic in environmental water body |
| CN113189253A (en) * | 2021-04-28 | 2021-07-30 | 沈阳大学 | Method for detecting nanoscale plastic particles in soil environment |
| CN113466095A (en) * | 2021-06-02 | 2021-10-01 | 国科大杭州高等研究院 | Method for determining content of granular black carbon in water environment |
| CN113959971A (en) * | 2021-09-30 | 2022-01-21 | 自然资源部第三海洋研究所 | Method for rapidly and fully detecting small-particle-size plastics based on focal plane array infrared technology |
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