CN108623825B - Marine pollution micro-plastic dyeing method - Google Patents

Marine pollution micro-plastic dyeing method Download PDF

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Publication number
CN108623825B
CN108623825B CN201810483394.9A CN201810483394A CN108623825B CN 108623825 B CN108623825 B CN 108623825B CN 201810483394 A CN201810483394 A CN 201810483394A CN 108623825 B CN108623825 B CN 108623825B
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dyeing
micro
plastic
marine
mixture
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CN108623825A (en
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徐秋阳
齐丹
郑伟
艾小琪
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Hainan Tropical Ocean University
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Hainan Tropical Ocean University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/205Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase
    • C08J3/2053Compounding polymers with additives, e.g. colouring in the presence of a continuous liquid phase the additives only being premixed with a liquid phase
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2300/00Characterised by the use of unspecified polymers
    • C08J2300/30Polymeric waste or recycled polymer

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
  • Coloring (AREA)

Abstract

The invention relates to a method for dyeing marine pollution micro-plastics, which comprises the following steps: mixing Coomassie brilliant blue and methylene blue in an organic solvent to form a coloring agent solution; selecting a mixture comprising a micro-plastic from the marine contaminants; the mixture was stained with a stain solution and shaken to maintain the stain for a predetermined time. According to the marine pollution micro-plastic dyeing method, the Coomassie brilliant blue and the methylene blue are mixed in the organic solvent to prepare the dyeing agent solution, and the marine pollution is dyed by the dyeing agent solution, so that the dyeing time is short, the effect is fast, the dyeing is convenient and fast, and the operation is simple and convenient. Compared with the traditional expensive nile red, the cost of the Coomassie brilliant blue and the methylene blue is lower, and the method is suitable for the extensive research on the marine pollution micro-plastic.

Description

Marine pollution micro-plastic dyeing method
Technical Field
The invention relates to the technical field of marine pollutant research, in particular to a marine pollution micro-plastic dyeing method.
Background
The micro-plastics are the key research objects of the current marine pollutants, and research on the content of the micro-plastics in the sea is being intensified in various places. However, since the micro-plastic is very stable, it is very difficult to react with various reagents, and most micro-plastics are transparent and difficult to observe. Thus, the current approach is to find a suitable coloring agent, which is colored to aid experimental studies. At present, only the literature reports that nile red can dye micro plastics, but nile red is expensive and is not suitable for extensive research. Therefore, there is a need to develop a new method for dyeing micro-plastics with low cost.
Disclosure of Invention
In view of the above, a method for dyeing marine pollution micro-plastics with low cost, high dyeing speed, high efficiency, convenience and rapidness is provided.
A marine pollution micro-plastic dyeing method comprises the following steps:
preparing a coloring agent: mixing Coomassie brilliant blue and methylene blue in an organic solvent to form a coloring agent solution;
treating marine pollutants: selecting a mixture comprising a micro-plastic from the marine contaminants;
dyeing treatment: dyeing the mixture by using a dyeing agent solution, and oscillating and keeping the dyeing for a preset time;
in a preferred embodiment, the ratio of coomassie brilliant blue to methylene blue is from 1: 1, and mixing at equal concentration. Further, the concentration of the Coomassie brilliant blue is not lower than 0.1g/L, the dyeing preset time is 5-15 seconds, and the organic solvent is an alcohol solution. Wherein in the step of treating the marine pollutants, the micro-plastics float out according to a flotation method and then are dyed by using a dyeing agent; sea sand is contained in the mixture containing the micro-plastics, and the sea sand and the micro-plastics are dyed together during dyeing, and then the micro-plastics are floated out through a flotation method. Further, before shaking, it is confirmed whether the mixture containing the micro plastic contains water, if the mixture itself contains water, shaking is performed directly, and if the mixture does not contain water, shaking is performed by adding an appropriate amount of water. Prior to the dyeing treatment, the mixture containing the micro-plastics is soaked with dilute nitric acid to remove the micro-biomass.
In the method for dyeing the marine pollution micro-plastic, the Coomassie brilliant blue and the methylene blue are mixed in the organic solvent to prepare the dyeing agent solution, and the marine pollution is dyed by the dyeing agent solution, so that the dyeing time is only about 10 seconds, the time is short, the effect is fast, and the dyeing is convenient and fast. Compared with the traditional expensive nile red, the cost of the Coomassie brilliant blue and the methylene blue is lower, and the method is suitable for the extensive research on the marine pollution micro-plastic.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a method for dyeing marine pollution micro-plastics, which comprises the following steps:
s01: preparing a coloring agent: mixing Coomassie brilliant blue and methylene blue in an organic solvent to form a coloring agent solution;
s02: treating marine pollutants: selecting a mixture comprising a micro-plastic from the marine contaminants;
s03: dyeing treatment: dyeing the mixture by using a dyeing agent solution, and oscillating and keeping the dyeing for a preset time;
in the method for dyeing the marine pollution micro-plastics, the dyeing agent is prepared by mixing Coomassie brilliant blue and methylene blue in a ratio of 1: 1 equal concentration mixing is optimal. Further, the concentration of the Coomassie brilliant blue is not lower than 0.1 g/L. In the coloring agent solution, equal amount of Coomassie brilliant blue and methylene blue which are not less than 0.1g/L are mixed to dye the micro plastic. The dyeing preset time is 5-15 seconds, preferably 8-10 seconds, and the dyeing speed is high. The organic solvent is preferably an alcohol solution, such as ethanol.
In the step S02 of treating marine pollutants, the micro plastic is floated according to the flotation method, and then the dyeing agent solution is used to dye, so that the usage of the dyeing agents coomassie brilliant blue and methylene blue can be saved, and the marine pollutants can be used accurately. In addition, if sea sand exists in the mixture containing the micro-plastics, the sea sand and the micro-plastics are dyed together during dyeing, and then the micro-plastics are floated by a flotation method. Because many micro plastics are mixed in the sea sand, the sea sand and the micro plastics are dyed together, so that the research on the marine pollutants is more accurate and reliable. Further, before shaking, it is confirmed whether the mixture containing the micro plastic contains water, if the mixture itself contains water, shaking is performed directly, and if the mixture does not contain water, shaking is performed by adding an appropriate amount of water. By adding water, it is easier to separate the dyed microplastic from the organic solvent solution and other components after the microplastic is dyed. Before the dyeing treatment, the mixture containing the micro-plastics is soaked in dilute nitric acid to remove the microbial biomass, so that the consumption of the microbial biomass on the dyeing agent is eliminated, and the interference on the research of the marine pollution micro-plastics is eliminated.
Specifically, the marine pollutants are sea sand containing micro plastics, and the specific steps of the marine pollutant treatment are as follows: soaking sea sand in saturated solution of sodium iodide, sodium chloride or other sodium salt or potassium salt, aerating for half an hour or more, stopping aeration, standing for 24 hours or more, pouring out supernatant, and filtering with 0.45 μm organic filter membrane. The micro plastic is floated out by blowing air into the soaking solution, so that the separation effect is enhanced when the plastic is kept stand. The dyeing treatment comprises the following specific steps: dyeing the whole filter membrane by using a dyeing agent and water, taking out the filter membrane after dyeing, drying at 45 ℃, washing the micro-plastic on the filter membrane by using water, filtering by using a new 0.45-micron organic filter membrane, and carrying out quantitative analysis on the micro-plastic according to the dyeing condition in the filter membrane. The filter-borne microplastics can be counted using a microscope over the entire filter. After dyeing, the micro-plastics are blue under a microscope, different types of micro-plastics can be distinguished under a polarizing microscope according to the internal crystalline state of the particles, a few mixed micro-quartz can bring interference but can be distinguished obviously under polarized light, the plastic dyeing is deeper and more uniform, the quartz color is light, and the quartz crystal effect is obvious and stronger in anisotropy. In addition, the count can also be observed by fluorescence analysis, and is not limited to the above quantitative analysis of microplastics.
Therefore, according to the marine pollution micro-plastic dyeing method, the Coomassie brilliant blue and the methylene blue are mixed in the organic solvent to prepare the dyeing agent solution, the marine pollution is dyed by the dyeing agent solution, the dyeing time is only about 10 seconds, the time is short, the effect is fast, and the dyeing is convenient and fast. Compared with the traditional expensive nile red, the cost of the Coomassie brilliant blue and the methylene blue is lower, and the method is suitable for the extensive research on the marine pollution micro-plastic.
The specific implementation process of the marine pollution micro plastic dyeing method and the dyeing effect thereof will be described in detail by way of examples.
Example one
The method for dyeing the marine pollution micro-plastic of the embodiment 1 comprises the following steps:
preparing a coloring agent solution: coomassie brilliant blue was mixed with methylene blue at a ratio of 1: 1, mixing the two kinds of solution in ethanol to form a coloring agent solution, wherein the concentration of Coomassie brilliant blue is 0.1g/L, and the concentration of methylene blue is 0.1g/L, and the coloring agent solution is prepared by mixing the two kinds of solution in ethanol;
treating marine pollutants: a quantity of marine contaminants is preselected, and a mixture comprising micro-plastics, such as sea sand, is selected from the marine contaminants. Specifically, sea sand is collected, the sample sand is soaked in saturated sodium iodide solution, the aeration is stopped after half an hour, the mixture is kept stand for more than 24 hours, and then the supernatant is poured out and filtered by a 0.45-micron organic filter membrane.
Dyeing treatment: and adding a staining agent and water into the filter membrane formed in the previous step to stain the whole filter membrane, wherein the staining is finished within seconds. The filter was then dried at 45 ℃ and the microfilm was washed off with pure water and filtered through a new 0.45 micron filter of organic system. And (3) adding a dyeing agent solution while shaking for dyeing, dyeing for about 10 seconds, and keeping the dyeing while shaking.
And finally, analyzing and detecting the dyed micro plastic, and testing the components and the content of the micro plastic so as to research the marine pollutants. This example was counted microscopically on whole filters.
Example two
The embodiment of the invention provides a method for dyeing marine pollution micro-plastics, which comprises the following steps:
preparing a coloring agent solution: coomassie brilliant blue was mixed with methylene blue at a ratio of 1.5: 1 in the ethanol solution to form a coloring agent solution, wherein the concentration of Coomassie brilliant blue is 0.15g/L, and the concentration of methylene blue is 0.1g/L, and the coloring agent solution is prepared by mixing the Coomassie brilliant blue and the methylene blue in the ethanol solution;
treating marine pollutants: a quantity of marine contaminants is preselected, and a mixture comprising micro-plastics, such as sea sand, is selected from the marine contaminants. Specifically, sea sand is collected, soaked in dilute nitric acid to remove microbial biomass, washed, soaked in saturated sodium chloride solution to obtain sample sand, inflated for half an hour, then stopped inflating, and stood for 24 hours, and then supernatant is poured out and filtered with 0.45 micron organic filter membrane.
Dyeing treatment: and adding a staining agent and water into the filter membrane formed in the previous step to stain the whole filter membrane, wherein the staining is finished within seconds. The filter was then dried at 45 ℃ and the microfilm was washed off with pure water and filtered through a new 0.45 micron filter of organic system. And (3) adding a dyeing agent solution while shaking during dyeing, dyeing for about 8 seconds, and keeping the dyeing while shaking.
And finally, analyzing and detecting the dyed micro plastic, and testing the components and the content of the micro plastic so as to research the marine pollutants. The different types of microplastics are distinguished according to the crystalline state in the particles by observing through a polarizing microscope, and the microplastics are counted.
EXAMPLE III
The embodiment of the invention provides a method for dyeing marine pollution micro-plastics, which comprises the following steps:
preparing a coloring agent solution: mixing the mixture with methylene blue in a ratio of 1: 1.5, mixing the mixture in an ethanol solution to form a coloring agent solution, wherein the concentration of Coomassie brilliant blue is 0.1g/L, and the concentration of methylene blue is 0.15g/L, and the coloring agent solution is the ethanol solution;
treating marine pollutants: a quantity of marine contaminants is preselected, and a mixture comprising the microplastic is selected from the marine contaminants. Specifically, sea sand and other marine pollutants are collected together, soaked in dilute nitric acid to remove microbial biomass, then washed, soaked in a sodium iodide saturated solution, aerated for more than half an hour, then stopped aerated, kept stand for more than 24 hours, then the supernatant is poured out, and filtered by a 0.45-micron organic system filter membrane.
Dyeing treatment: adding a proper amount of water into the filter membrane, adding a staining agent solution while shaking, staining for about 10 seconds, taking out the filter membrane, drying at 45 ℃, washing the micro-plastic on the filter membrane by using pure water, and filtering by using a new 0.45-micrometer organic system filter membrane. And floating the micro plastic by using a flotation method, and removing the sea sand to obtain the dyed micro plastic.
And finally, analyzing and detecting the dyed micro plastic, and testing the components and the content of the micro plastic so as to research the marine pollutants. The different types of microplastics are distinguished according to the crystalline state in the particles by observing through a polarizing microscope, and the microplastics are counted.
Example four
The embodiment of the invention provides a method for dyeing marine pollution micro-plastics, which comprises the following steps:
preparing a coloring agent solution: mixing the mixture with methylene blue in a ratio of 1: 1 in the ethanol solution to form a coloring agent solution, wherein the concentration of Coomassie brilliant blue is 0.15g/L, and the concentration of methylene blue is 0.15g/L, and the coloring agent solution is prepared by mixing the Coomassie brilliant blue and the methylene blue in the ethanol solution;
treating marine pollutants: firstly, sea sand and other marine pollutants are collected together, soaked in dilute nitric acid to remove microbial biomass, then cleaned, soaked in a potassium iodide saturated solution, aerated for more than half an hour, then stopped aerated, kept stand for more than 24 hours, then poured out supernatant, and filtered by a 0.45 micron organic system filter membrane.
Dyeing treatment: adding a proper amount of water into the filter membrane, adding a staining agent solution while shaking, staining for about 12 seconds, taking out the filter membrane, drying at 45 ℃, washing the micro-plastic on the filter membrane by using pure water, and filtering by using a new 0.45-micrometer organic system filter membrane. And floating the micro plastic by using a flotation method, and removing the sea sand to obtain the dyed micro plastic.
And finally, observing the dyed micro-plastics through a polarization microscope, distinguishing different types of micro-plastics according to the internal crystalline state of the particles, and counting the micro-plastics. The dyeing effect of this example is stronger. The observation shows that the staining agent can stain the micro plastic with different concentration gradients, and the staining effect is gradually enhanced along with the increase of the concentration gradients.
It should be noted that the present invention is not limited to the above-mentioned embodiments, and other changes and modifications can be made by those skilled in the art according to the spirit of the present invention, and these changes and modifications made according to the spirit of the present invention should be included in the scope of the present invention as claimed.

Claims (6)

1. The method for dyeing the marine pollution micro-plastic is characterized by comprising the following steps:
preparing a coloring agent: mixing Coomassie brilliant blue and methylene blue in an alcohol solution to form a coloring agent solution, wherein the concentration of the Coomassie brilliant blue is not lower than 0.1 g/L;
treating marine pollutants: selecting a mixture comprising micro-plastics from a marine contaminant, the marine contaminant being sea sand comprising micro-plastics;
dyeing treatment: and dyeing the mixture by using a dyeing agent solution, oscillating and keeping the dyeing for a preset time, wherein the preset time of dyeing is 5-15 seconds, dyeing the sea sand and the micro plastic together during dyeing, and then floating the micro plastic by using a flotation method.
2. The method for staining a marine-fouling micro-plastic according to claim 1, wherein the ratio of coomassie brilliant blue to methylene blue is 1: 1, and mixing at equal concentration.
3. The method for dyeing micro plastic materials with marine pollution according to claim 1, wherein before shaking, it is determined whether the mixture containing micro plastic materials contains water, if the mixture itself contains water, the mixture is directly shaken, and if the mixture does not contain water, the mixture is added with water and shaken.
4. The method of dyeing marine pollution micro plastic according to claim 1, characterized in that the mixture containing micro plastic is soaked with dilute nitric acid to remove the micro biomass before dyeing treatment.
5. The method for dyeing the marine pollution micro plastic as claimed in claim 1, wherein the specific steps of the marine pollution treatment are as follows: soaking sea sand in saturated sodium salt or potassium salt solution, aerating for half an hour or more, stopping aerating, standing for 24 hours or more, pouring out supernatant, and filtering with 0.45 μm organic filter membrane.
6. The method for dyeing the marine pollution micro plastic according to claim 5, wherein the dyeing treatment comprises the following specific steps: dyeing the whole filter membrane by using a dyeing agent and water, taking out the filter membrane after dyeing, drying, washing the micro-plastic on the filter membrane by using water, filtering by using a new 0.45-micron organic filter membrane, and carrying out quantitative analysis on the micro-plastic according to the dyeing condition in the filter membrane.
CN201810483394.9A 2018-05-18 2018-05-18 Marine pollution micro-plastic dyeing method Expired - Fee Related CN108623825B (en)

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CN109253907B (en) * 2018-10-17 2020-11-13 大连理工大学 Method for rapidly and auxiliarily detecting micro-plastic in water environment sample by using Nile red dyeing
ES2973958T3 (en) * 2019-02-18 2024-06-25 Kemira Oyj Evaluation method and optionally selection of suitable chemical characteristics for the elimination of microplastics in a liquid matrix
CN110108892A (en) * 2019-05-17 2019-08-09 舟山巨洋技术开发有限公司 A kind of micro- plastics automatic analyzer
CN112730368A (en) * 2020-12-30 2021-04-30 北京师范大学 Thermal cycle method for preparing fluorescent dyed micro plastic and concentration analysis method
WO2022239852A1 (en) * 2021-05-13 2022-11-17 国立大学法人東京海洋大学 Staining solution, plastic detecting method, processing device, and program

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