CN114166820A - Method for detecting micro/nano plastic and organic pollutant adsorbed on surface of micro/nano plastic - Google Patents

Method for detecting micro/nano plastic and organic pollutant adsorbed on surface of micro/nano plastic Download PDF

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CN114166820A
CN114166820A CN202111447271.8A CN202111447271A CN114166820A CN 114166820 A CN114166820 A CN 114166820A CN 202111447271 A CN202111447271 A CN 202111447271A CN 114166820 A CN114166820 A CN 114166820A
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micro
nano
nano plastic
organic pollutants
plastic
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鲁逸林
王春波
刘超
徐青雲
徐升敏
刘中刚
刘国华
武赟
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Anhui University
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    • G—PHYSICS
    • G01—MEASURING; TESTING
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    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/65—Raman scattering
    • G01N21/658—Raman scattering enhancement Raman, e.g. surface plasmons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract

The invention relates to the technical field of trace pollutant detection, in particular to a method for detecting micro/nano plastic and organic pollutants adsorbed on the surface of the micro/nano plastic, which comprises the steps of firstly synthesizing an SERS signal reinforcing agent, separating the micro/nano plastic and the organic pollutants adsorbed on the surface of the micro/nano plastic by using a TLC (thin layer chromatography) technology, dropwise adding the SERS signal reinforcing agent added with a coagulant to organic pollutant sites on a TLC plate except the micro/nano plastic, and finally performing spectrum acquisition on the TLC plate by using a Raman spectrometer. By adding the SERS signal reinforcing agent, the detection sensitivity of the organic pollutants is improved, the defects that only TLC is used for non-specificity and inaccurate quantification of target analytes are overcome, and the problem that pollutants with similar contrast shift values cannot be separated is solved.

Description

Method for detecting micro/nano plastic and organic pollutant adsorbed on surface of micro/nano plastic
Technical Field
The invention relates to the technical field of trace pollutant detection, in particular to a method for detecting micro/nano plastic and organic pollutants adsorbed on the surface of the micro/nano plastic.
Background
The process of plastic degradation can generate micro/nano plastic, and the micro/nano plastic has high specific surface area, so that the micro/nano plastic can adsorb pollutants such as organic pollutants, toxic heavy metals and the like more easily. The micro/nano plastic forms composite toxicity after adsorbing organic pollutants, and generates various hazards: biological accumulation and transfer, toxicity of the micro/nano-plastics themselves, toxicity of leaching compounds and adsorbing contaminants. Therefore, it is urgent to research how to rapidly detect micro/nano plastics and adsorb organic pollutants on the surface of the micro/nano plastics. However, the distribution of micro/nano plastics in the environment and the adsorption of micro/nano plastics to pollutants in the environment and their associated toxicity are very limited, partly because of the lack of special techniques for separating and identifying micro/nano plastics from the complex environmental background, and the signal of micro/nano plastics itself increases the difficulty of detecting organic pollutants adsorbed on its surface, so that there is an urgent need for techniques capable of detecting micro/nano plastics and organic pollutants adsorbed on its surface.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the technical problems, the invention provides a method for detecting micro/nano plastic and organic pollutants adsorbed on the surface of the micro/nano plastic.
The adopted technical scheme is as follows:
a method for detecting micro/nano plastic and organic pollutants adsorbed on the surface of the micro/nano plastic comprises the following steps:
s1: synthesizing a SERS signal enhancer;
s2: separating the micro/nano plastic and the organic pollutants adsorbed on the surface of the micro/nano plastic by using a TLC (thin layer chromatography) technology;
s3: dropping the SERS signal reinforcing agent added with the coagulant on organic pollutant sites except micro/nano plastics on a TLC plate;
s4: the TLC plate was spectrally collected using a raman spectrometer.
Further, the organic pollutant is an aromatic amine compound, and the aromatic amine compound in the invention is an amine with an aromatic substituent, namely-NH2The aromatic hydrocarbon is usually one or more benzene rings, i.e. the nitrogen atom is directly bonded to the carbon atom of the benzene ring, and can be aniline, benzidine, m-phenylenediamine, p-phenylenediamine, etc., which are only examples and not intended to be limiting.
Further, the SERS signal enhancer is silver sol or gold sol.
Further, the SERS signal enhancer is any one of nano silver sol reduced by beta-cyclodextrin, nano silver sol reduced by sodium citrate or nano gold sol reduced by sodium citrate.
Further, the SERS signal enhancer is nano silver sol reduced by beta-cyclodextrin.
Further, the preparation method of the beta-cyclodextrin reduced nano silver sol comprises the following steps:
dissolving beta-cyclodextrin with water, adding NaOH solution, heating to 70-80 deg.C, stirring for 10-20min, adding silver nitrate solution, stirring for 10-40min, turning off heat source, stirring until the reaction solution is cooled to room temperature to obtain yellow solution, washing with water, and centrifuging.
Further, the coagulant is NaOH or NaNO3、CaCl2KBr, KCl, NaCl or NaOH solution, NaNO3Solution, CaCl2Any one of a solution, a KBr solution, a KCl solution and a NaCl solution.
Further, the coagulant is a NaCl solution.
Further, the molar concentration of the NaCl solution is 1.5-50 mmol/L.
Further, the developing solvent used for separating the micro/nano plastic and the organic pollutants adsorbed on the surface thereof by using the TLC technology is any one or combination of ethyl acetate, n-hexane, methanol, ethanol, dichloromethane and petroleum ether, and preferably ethyl acetate.
The invention has the beneficial effects that:
the invention combines thin-layer chromatography and surface enhanced Raman spectroscopy (TLC-SERS), realizes the co-detection of micro/nano plastic and organic pollutants, improves the detection sensitivity of the organic pollutants by adding an SERS signal intensifier, and has the following excellent detection effects compared with the single TLC technology and SERS technology: the difficulty of the SERS detection technology in detecting and analyzing mixed pollutants is solved, and in the mixture SERS detection, because each component of the mixture contributes to an SERS spectrum, the quantitative relation between a spectrum peak and the content of a single substance is difficult to establish. By means of a TLC separation method, the mixture is separated in a physical space, and a corresponding relation between a spectrum and the type and content of a substance component is established conveniently; the TLC-SERS not only can solve the difficulty of spectral analysis, but also can solve the problem that only the SERS technology is used to generate high-concentration components to cover the low-concentration component signals, thereby improving the detection limit of the system; the introduction of SERS technology solves the defects of no specificity and inaccurate quantification of target analytes only by TLC, and also solves the problem that pollutants with similar contrast shift values cannot be separated.
Drawings
FIG. 1 is a schematic diagram of the technical route of the method for detecting micro/nano plastic and organic pollutants adsorbed on the surface thereof in example 1 of the present invention;
fig. 2-a is a UV-Vis absorption spectrum of the SERS signal enhancer in examples 1-3 of the present invention, wherein a is a nano silver sol reduced by sodium citrate, b is a nano gold sol reduced by sodium citrate, and c is a nano silver sol reduced by β -cyclodextrin;
FIG. 2-B is a graph showing the effect of SERS signal enhancers on the detection of m-phenylenediamine in examples 1-3, wherein a is a nanosilver sol reduced by sodium citrate, B is a nanogold sol reduced by sodium citrate, and c is a nanosilver sol reduced by beta-cyclodextrin;
as can be seen from fig. 2-B, the nano silver sol reduced by beta-cyclodextrin has the most excellent enhancement effect;
FIG. 2-C is an SEM photograph of the nano-silver sol reduced by beta-cyclodextrin in example 1;
FIG. 2-D is the particle size statistics of the nano-silver sol reduced by beta-cyclodextrin in example 1;
as shown in fig. 2-D, the particle size of the nano-silver particles in the nano-silver sol reduced by β -cyclodextrin is about 45nm, and the particle size distribution is uniform;
FIG. 2-E is an SEM photograph of the sodium citrate-reduced nanosilver sol of example 2;
FIG. 2-F is an SEM photograph of the nano gold sol reduced by sodium citrate in example 3;
FIG. 3-A is a graph showing the effect of different flocculants on SERS signals in examples 1, 3-7, wherein a is NaOH solution and b is NaNO3Solution c is CaCl2The solution d is KBr solution, e is KCl solution, and f is NaCl solution;
as can be seen from FIG. 3-A, the NaCl solution had the most excellent strengthening effect as a coagulant;
FIG. 3-B is the effect of different concentrations of NaCl solutions on SERS signals in examples 1, 8-12, wherein a is 1.5mmol/L, B is 3mmol/L, c is 6mmol/L, d is 12mmol/L, e is 25mmol/L, and f is 50 mmol/L;
as can be seen from FIG. 3-B, the most excellent enhancement effect was obtained when the NaCl solution concentration was 50 mmol/L;
FIG. 4 is a typical Raman spectrum corresponding to different contaminants before mixing of the simulated contaminants in example 1; wherein a is polystyrene (PS, d is 100nm), b is benzidine, c is m-phenylenediamine, and d is p-phenylenediamine.
FIG. 5 shows Raman spectra of different contaminants after TLC separation of the simulated contaminants in example 13, where a is polystyrene (PS, d 200nm), b is benzidine, c is m-phenylenediamine, and d is p-phenylenediamine.
FIG. 6 shows the Raman spectra of the different contaminants after TLC separation of the simulated contaminants in example 14, wherein a is poly (methyl methacrylate) (PMMA, d 200nm), b is benzidine, and c is m-phenylenediamine.
FIG. 7-A is the corresponding Raman spectra of different contaminants after TLC separation of the simulated contaminants in example 1;
FIG. 7-B is the corresponding Raman spectra of different contaminants after TLC separation of the simulated contaminants in example 15.
As can be seen from the comparison of FIGS. 7-A and 7-B, the method of the present invention has a better detection effect for both the simulated pollutants in ultrapure water configuration and the simulated pollutants in lake water configuration, which indicates that the method of the present invention has practical application significance.
Detailed Description
The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1:
a method for detecting micro/nano plastic and organic pollutants adsorbed on the surface of the micro/nano plastic comprises the following steps:
s1: dissolving 400mg of beta-cyclodextrin in 50mL of ultrapure water, adding 250 mu L of NaOH solution with the concentration of 1M, heating the mixed solution to 80 ℃, stirring for 10min, adding 2mL of silver nitrate solution with the concentration of 20mmol/L, stirring for reaction for 10min, closing a heat source, continuously stirring until the reaction solution is cooled to room temperature to obtain a yellow solution, washing the yellow solution with water, and centrifuging to obtain an SERS signal enhancer (nano silver sol reduced by beta-cyclodextrin);
s2: adding polystyrene with the diameter of 100nm into ultrapure water to prepare suspension with the concentration of 1g/L, then mixing the suspension with benzidine, m-phenylenediamine and p-phenylenediamine with the concentration of 50ppm in an equal volume manner to serve as a simulated pollutant for standby, marking a dotted line on a thin-layer chromatography plate by using a pencil at 1.5cm and 6cm respectively, taking the simulated pollutant, carrying out point sample application at a position 1.5cm away from the bottom edge, wherein the diameter of an original point is not more than 5mm, drying the solution by using a blower after point sample application, then carrying out point sample application for 5 times, separating the point-applied thin-layer chromatography plate in a developing cylinder by using an ethyl acetate developing agent, and positioning the position of an organic pollutant site by using a handheld ultraviolet lamp with the wavelength of 254/365 nm;
s3: adding SERS signal reinforcing agent (except the position of micro/nano plastic) added with 50mmol/LNaCl solution dropwise on each organic pollutant site on the thin-layer chromatographic plate, and collecting the SERS spectrum of each organic pollutant site and the common Raman spectrum of the micro/nano plastic by using a Raman spectrometer based on a silicon wafer at 520.7cm-1The main vibration peak of (1), calibration number Raman spectrometer (HORIBA, HR Evolution), placing thin-layer chromatography plate on microscope stage of Raman spectrometer, focusing laser spot on sample, selecting Olympus 50X long-focus lens to make Raman spectrum collection, collecting laser light source (lambda is 532nm), laser intensity is 1%, single exposure time is 10s, signal accumulation is 3 times, collecting range is 50-2500cm-1Repeat 5 times.
The micro/nano plastic Raman imaging test conditions are as follows: a 785nm laser is used for excitation, the step length is 90 mu m, the integration time is 10s, and a 50-time long-focus objective lens is adopted;
the test conditions of the organic pollutants are that the step length is 90 mu m, the integration time is 1s, and a 10-time long-focus objective lens is adopted.
Example 2:
substantially the same as example 1, except that the SERS signal enhancer was replaced with a sodium citrate-reduced nanosilver sol, which was prepared as follows:
19mg of AgNO3Adding into 100mL deionized water, heating to boil rapidly, adding 2mL 1.00 wt.% sodium citrate solution and 0.02 wt.% polyvinylpyrrolidone solution, keeping for 30min while boiling, cooling to room temperature, and centrifuging at 8000 rpm.
Example 3:
substantially the same as example 1, except that the SERS signal enhancer was replaced with a sodium citrate-reduced nanogold sol, which was prepared as follows:
100mL of 0.25mmol/L aqueous chloroauric acid solution was added to a 250mL Erlenmeyer flask, the pH of the aqueous chloroauric acid solution was adjusted to 7.0 with 1M HCl and 1M NaOH, stirred and heated to boiling, then 490. mu.L of 5.00 wt.% aqueous sodium citrate solution was added, stirring was continued until the solution turned wine red, and a condenser tube was used to prevent evaporation of the solvent during the reaction.
Experimental example 3:
essentially the same as in example 1, except that the coagulant was replaced with the same concentration of NaOH solution.
Experimental example 4:
substantially the same as in example 1 except that the coagulant was replaced with NaNO at the same concentration3And (3) solution.
Experimental example 5:
essentially the same as in example 1, except that the coagulant was replaced with the same concentration of CaCl2And (3) solution.
Experimental example 6:
essentially the same as in example 1, except that the coagulant was replaced with a KBr solution of the same concentration.
Experimental example 7:
essentially the same as in example 1, except that the coagulant was replaced with a KCl solution of the same concentration.
Experimental example 8:
substantially the same as in example 1 except that the concentration of the coagulant in NaCl solution was adjusted to 1.5 mmol/L.
Experimental example 9:
substantially the same as in example 1 except that the concentration of the coagulant in NaCl solution was adjusted to 3 mmol/L.
Experimental example 10:
substantially the same as in example 1 except that the concentration of the coagulant in NaCl solution was adjusted to 6 mmol/L.
Experimental example 11:
substantially the same as in example 1 except that the concentration of the coagulant in NaCl solution was adjusted to 12 mmol/L.
Experimental example 12:
substantially the same as in example 1 except that the concentration of the coagulant in NaCl solution was adjusted to 25 mmol/L.
Experimental example 13:
substantially the same as in example 1 except that polystyrene having a diameter of 100nm was replaced with polystyrene having a diameter of 200 nm.
Experimental example 14:
substantially the same as in example 1 except that the polystyrene having a diameter of 100nm was replaced with polymethyl methacrylate having a diameter of 200nm, and p-phenylenediamine was not added.
Experimental example 15:
basically the same as example 1 except that the ultrapure water used for preparing the suspension was replaced with ordinary lake water.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. A method for detecting micro/nano plastic and organic pollutants adsorbed on the surface of the micro/nano plastic is characterized by comprising the following steps:
s1: synthesizing a SERS signal enhancer;
s2: separating the micro/nano plastic and the organic pollutants adsorbed on the surface of the micro/nano plastic by using a TLC (thin layer chromatography) technology;
s3: dropping the SERS signal reinforcing agent added with the coagulant on organic pollutant sites except micro/nano plastics on a TLC plate;
s4: the TLC plate was spectrally collected using a raman spectrometer.
2. The method for detecting the micro/nano plastic and the adsorbed organic pollutants on the surface thereof according to claim 1, wherein the organic pollutants are aromatic amine compounds.
3. The method for detecting micro/nano plastic and organic pollutants adsorbed on the surface of micro/nano plastic as claimed in claim 1, wherein the SERS signal enhancer is silver sol or gold sol.
4. The method for detecting micro/nano plastic and organic pollutants adsorbed on the surface of micro/nano plastic as claimed in claim 3, wherein the SERS signal enhancer is a nano silver sol reduced by beta-cyclodextrin, a nano silver sol reduced by sodium citrate or a nano gold sol reduced by sodium citrate.
5. The method for detecting micro/nano plastic and organic pollutants adsorbed on the surface of micro/nano plastic as claimed in claim 4, wherein the SERS signal enhancer is nano silver sol reduced by beta-cyclodextrin.
6. The method for detecting micro/nano plastic and organic pollutants adsorbed on the surface of the micro/nano plastic as claimed in claim 5, wherein the preparation method of the nano silver sol reduced by beta-cyclodextrin is as follows:
dissolving beta-cyclodextrin with water, adding NaOH solution, heating to 70-80 deg.C, stirring for 10-20min, adding silver nitrate solution, stirring for 10-40min, turning off heat source, stirring until the reaction solution is cooled to room temperature to obtain yellow solution, washing with water, and centrifuging.
7. The method for detecting the organic pollutants adsorbed on the surfaces of micro/NaNO plastics and micro/NaNO plastics according to claim 1, wherein the coagulant is NaOH or NaNO3、CaCl2KBr, KCl, NaCl or NaOH solution, NaNO3Solution, CaCl2Any one of a solution, a KBr solution, a KCl solution and a NaCl solution.
8. The method for detecting the organic pollutants adsorbed on the surfaces of the micro/nano plastic and the micro/nano plastic as claimed in claim 7, wherein the coagulant is NaCl solution.
9. The method for detecting the micro/nano plastic and the adsorbed organic pollutants on the surface thereof according to claim 8, wherein the molar concentration of the NaCl solution is 1.5-50 mmol/L.
10. The method for detecting micro/nano plastic and organic pollutants adsorbed on the surface thereof according to claim 2, wherein the developing solvent used for separating the micro/nano plastic and the organic pollutants adsorbed on the surface thereof by using the TLC technology is any one or more of ethyl acetate, n-hexane, methanol, ethanol, dichloromethane and petroleum ether, and preferably ethyl acetate.
CN202111447271.8A 2021-11-30 2021-11-30 Method for detecting micro/nano plastic and organic pollutant adsorbed on surface of micro/nano plastic Pending CN114166820A (en)

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