Method for identifying nano plastic particles in aqueous solution based on scanning electron microscope-Raman technology

A nano-plastic and technical identification technology, applied in the field of nano-plastic identification, can solve the problems of easily damaged sample organic components, high electron beam energy and Raman light intensity, and achieve the effects of short time consumption, reduced background and improved quality.

Inactive Publication Date: 2020-05-08
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the scanning electron microscope-Raman measurement process, the electron beam energy and Raman light intensity are high, which is easy to damage the organic components of the sample. Up to now, there is no suitable parameter setting, so it is rarely used in the identification of nanoplastics.

Method used

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  • Method for identifying nano plastic particles in aqueous solution based on scanning electron microscope-Raman technology
  • Method for identifying nano plastic particles in aqueous solution based on scanning electron microscope-Raman technology
  • Method for identifying nano plastic particles in aqueous solution based on scanning electron microscope-Raman technology

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Embodiment 1

[0018] In-situ identification of standard nanoplastic particles in deionized aqueous solution of embodiment 1

[0019] First conduct a blank experiment, stick a clean silicon wafer to the metal substrate of the scanning electron microscope, then put it into the electron microscope for direct observation, and move it to the Raman spectrum, choose a point to measure according to the set experimental parameters, and get The Raman signal of the silicon wafer is used as a reference for subsequent tests.

[0020] A colloid solution containing standard polyvinyl chloride nanoplastic particles was dropped on a silicon wafer, and allowed to stand for 24 hours at room temperature to air-dry naturally. Before the measurement, stick the silicon chip with polyvinyl chloride nano-plastic particles on the metal substrate of the scanning electron microscope, and put it into the electron microscope for direct observation; after confirming the nano-plastic particles that need to be analyzed b...

Embodiment 2

[0022] The identification of nanoparticles in embodiment 2 mineral water solution

[0023] Carry out a blank experiment first, stick a clean silicon wafer to the metal substrate of the scanning electron microscope, then put it into the electron microscope for direct observation, and move it to the Raman spectrum, choose a point to measure according to the set test parameters, and get The Raman signal of the silicon wafer is used as a reference for subsequent tests. The Raman spectrum of the silicon substrate is shown in figure 2 B, given the silicon substrate 960cm -1 The intensity of the Raman peak is too large, which will affect the display of other peaks, so the 960cm -1 Raman Peak is hidden.

[0024] Use 10 μm and 1 μm polyethersulfone filter membranes to sequentially filter the mineral water solution that may contain nanoparticles, and finally obtain an aqueous solution containing nanoparticles (<1 μm), drop the aqueous solution containing nanoparticles on a silicon...

Embodiment 3

[0026] The identification of nanoparticles in the seawater solution of embodiment 3

[0027] First conduct a blank experiment, stick a clean silicon wafer to the metal substrate of the scanning electron microscope, then put it into the electron microscope for direct observation, and move it to the Raman spectrum, choose a point to measure according to the set test parameters, and get The Raman signal of the silicon wafer is used as a reference for subsequent tests. Use 10 μm and 1 μm polyethersulfone filter membranes to sequentially filter the aqueous solution that may contain nanoparticles, and finally obtain a seawater solution containing nanoparticles (<1 μm), drop the seawater solution containing nanoparticles on a silicon chip, and statically Let it dry naturally at room temperature for 24 hours.

[0028] Before the measurement, stick the silicon wafer containing the sample on the metal substrate of the scanning electron microscope, and then put it into the electron mi...

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Abstract

The invention belongs to the field of nano plastic identification. The invention discloses a method for identifying nano plastic particles in an aqueous solution based on a scanning electron microscope-Raman technology. Targeted recognition and in-situ identification of nano plastic particles are realized by setting and optimizing parameters of a scanning electron microscope and a white-light-containing confocal microscopic Raman spectrum combination instrument; the method comprises the following steps: uniformly dripping a to-be-detected aqueous solution on a clean silicon wafer at room temperature after carrying out graded filtration on the to-be-detected aqueous solution through 10 [mu]m and 1 [mu]m polyethersulfone filter membranes in sequence; naturally air-drying a sample, placing the sample on a sample table in a vacuum cavity of a scanning electron microscope, setting corresponding test parameters to obtain a scanning electron microscope image, automatically transmitting the detection sample to a Raman spectrum, keeping the detection sample at the same position, setting proper test parameters to obtain a Raman image, and carrying out image analysis and judgment. Compared with a traditional detection method, the method has the advantages that the morphology of the nanoparticles in the solution can be obtained while ensuring that a nano plastic sample is not damaged, andmeanwhile, whether the nanoparticles contain plastic components or not is identified.

Description

technical field [0001] The invention belongs to the technical field of nano-plastic identification, and in particular relates to a method for identifying nano-plastic particles in an aqueous solution based on a scanning electron microscope-Raman technology, which is realized through parameter setting and testing. Background technique [0002] At present, the identification techniques of nanoplastics in liquid solutions mainly include dynamic light scattering and scanning electron microscopy. Dynamic light scattering technology can measure particles from 1nm to 3mm in size through the intensity fluctuation of the suspended laser beam, which is widely used in particle size characterization, especially the characterization of primary nanoplastics in toxicology experiments, but the theory used by dynamic light scattering technology The model is sphere-based and applies to monodisperse suspensions. In practical applications, it is easy to be polluted by matrix, aggregates or dus...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N23/2251G01N23/2202G01N21/65
CPCG01N21/65G01N23/2202G01N23/2251
Inventor 邱宇平董志强张文祝凌韩文慧
Owner TONGJI UNIV
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