KR102419226B1 - A method for analyzing and reducing microplastic elution from fibers - Google Patents

A method for analyzing and reducing microplastic elution from fibers Download PDF

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KR102419226B1
KR102419226B1 KR1020200165267A KR20200165267A KR102419226B1 KR 102419226 B1 KR102419226 B1 KR 102419226B1 KR 1020200165267 A KR1020200165267 A KR 1020200165267A KR 20200165267 A KR20200165267 A KR 20200165267A KR 102419226 B1 KR102419226 B1 KR 102419226B1
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김운중
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한남대학교 산학협력단
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    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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    • G01MEASURING; TESTING
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    • G01MEASURING; TESTING
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Abstract

본 발명은 섬유로부터 미세플라스틱을 용출하여 분석하는 방법 및 미세플라스틱의 저감방법에 관한 것으로서, 보다 상세하게는 a) 섬유, 물 및 세제를 교반하여 혼합물을 제조하는 단계; b) 상기 혼합물을 필터로 여과하는 단계; c) 상기 필터에 남겨진 잔류물 및 물을 교반하여 혼합액을 제조하는 단계; d) 상기 혼합액의 일부를 샘플링하여 필터로 여과하는 단계; e) 상기 필터에 남겨진 잔류물을 건조하는 단계; 및 f) 상기 건조된 잔류물을 FT-IR microscope을 사용하여 정량분석하는 단계를 포함하는 섬유의 미세플라스틱 분석방법에 관한 것이다.The present invention relates to a method for eluting and analyzing microplastics from fibers and to a method for reducing microplastics, and more particularly, to a method comprising: a) preparing a mixture by stirring fibers, water and detergent; b) filtering the mixture with a filter; c) preparing a mixed solution by stirring the residue and water remaining in the filter; d) sampling a portion of the mixed solution and filtering it with a filter; e) drying the residue left on the filter; and f) quantitatively analyzing the dried residue using an FT-IR microscope.

Description

섬유의 미세플라스틱 분석방법 및 저감방법 {A method for analyzing and reducing microplastic elution from fibers}{A method for analyzing and reducing microplastic elution from fibers}

본 발명은 섬유로부터 미세플라스틱을 용출하여 분석하는 방법 및 미세플라스틱의 저감방법에 관한 것으로서, 보다 상세하게는 a) 섬유, 물 및 세제를 교반하여 혼합물을 제조하는 단계; b) 상기 혼합물을 필터로 여과하는 단계; c) 상기 필터에 남겨진 잔류물 및 물을 교반하여 혼합액을 제조하는 단계; d) 상기 혼합액의 일부를 샘플링하여 필터로 여과하는 단계; e) 상기 필터에 남겨진 잔류물을 건조하는 단계; 및 f) 상기 건조된 잔류물을 FT-IR microscope을 사용하여 정량분석하는 단계를 포함하는 섬유의 미세플라스틱 분석방법에 관한 것이다.The present invention relates to a method for eluting and analyzing microplastics from fibers and to a method for reducing microplastics, and more particularly, to a method comprising: a) preparing a mixture by stirring fibers, water and detergent; b) filtering the mixture with a filter; c) preparing a mixed solution by stirring the residue and water remaining in the filter; d) sampling a portion of the mixed solution and filtering it with a filter; e) drying the residue left on the filter; and f) quantitatively analyzing the dried residue using an FT-IR microscope.

최근 일상생활 속에서 배출되는 미세플라스틱으로 인해 환경적인 문제가 부가되면서 사회적인 문제가 되고 있다. Recently, microplastics emitted from daily life have added environmental problems and become a social problem.

미세플라스틱은 5mm 이하의 작은 플라스틱 입자를 말하며, 해양에서 발견되는 미세플라스틱의 35%를 차지하는 것이 미세섬유이다. Microplastics are small plastic particles less than 5mm in diameter, and microfibers account for 35% of microplastics found in the ocean.

미세섬유는 합성섬유 재질의 옷에서 나오는 미세플라스틱 섬유로 바다, 하천 등으로 흘러간 미세섬유는 물속 독성물질을 빨아들인 후 바다 생물에 흡수된다. Microfibers are microplastic fibers that come from clothes made of synthetic fibers. The microfibers that flow into the sea or rivers absorb toxic substances in the water and are then absorbed by sea creatures.

상기 미세섬유는 플랑크톤에서 작은 물고기, 큰 물고기 및 사람으로 이어지는 먹이사슬에 따라 사람에게 되돌아와 환경뿐만 아니라 인체에도 악영향을 미치고 있다. The microfibers return to humans along the food chain from plankton to small fish, large fish and humans, and adversely affect not only the environment but also the human body.

따라서 합성섬유나 천연섬유로부터 배출되는 미세섬유의 양을 정확히 분석하고, 이를 통해 배출되는 미세섬유의 양을 줄일 수 있는 기술개발이 필요하다. Therefore, it is necessary to accurately analyze the amount of microfibers discharged from synthetic or natural fibers, and to develop a technology that can reduce the amount of microfibers discharged through this.

한국등록특허 제10-2178099호Korean Patent No. 10-2178099

본 발명은 섬유로부터 미세플라스틱을 용출하여 쉽고 간단하게 분석하는 방법을 제공하는데 목적이 있다. An object of the present invention is to provide a method for eluting microplastics from fibers and analyzing them easily and simply.

또한 본 발명은 합성섬유나 천연섬유로부터 배출되는 미세섬유의 양을 정확히 분석하고, 이를 통해 배출되는 미세섬유의 양을 줄일 수 있는 방법을 제공하는 것을 목적으로 한다. Another object of the present invention is to accurately analyze the amount of microfibers discharged from synthetic fibers or natural fibers, and to provide a method capable of reducing the amount of microfibers discharged through this.

상기와 같은 목적을 달성하기 위하여 본 발명은In order to achieve the above object, the present invention

a) 섬유, 물 및 세제를 교반하여 혼합물을 제조하는 단계;a) agitating the fibers, water and detergent to prepare a mixture;

b) 상기 혼합물을 필터로 여과하는 단계;b) filtering the mixture with a filter;

c) 상기 필터에 남겨진 잔류물 및 물을 교반하여 혼합액을 제조하는 단계;c) preparing a mixed solution by stirring the residue and water remaining in the filter;

d) 상기 혼합액의 일부를 샘플링하여 필터로 여과하는 단계;d) sampling a portion of the mixed solution and filtering it with a filter;

e) 상기 필터에 남겨진 잔류물을 건조하는 단계; 및e) drying the residue left on the filter; and

f) 상기 건조된 잔류물을 FT-IR microscope을 사용하여 정량분석하는 단계를 포함하는 섬유의 미세플라스틱 분석방법을 제공한다.f) It provides a method for analyzing microplastics of fibers, comprising the step of quantitatively analyzing the dried residue using an FT-IR microscope.

본 발명의 일실시예에 있어서, 상기 세제는 액체세제, 고체세제 및 종이세제에서 하나 이상 선택되는 것을 특징으로 한다. In one embodiment of the present invention, the detergent is characterized in that at least one selected from liquid detergent, solid detergent and paper detergent.

본 발명의 일실시예에 있어서, 상기 필터는 메쉬 필터인 것을 특징으로 한다. In one embodiment of the present invention, the filter is characterized in that the mesh filter.

본 발명의 일실시예에 있어서, 상기 c) 단계 및 d) 단계를 1회 이상 반복하는 것을 특징으로 한다. In one embodiment of the present invention, it is characterized in that the steps c) and d) are repeated one or more times.

본 발명의 일실시예에 있어서, 상기 d) 단계는 혼합액 부피의 1/5~1/15를 샘플링하는 것을 특징으로 한다. In one embodiment of the present invention, step d) is characterized in that 1/5 to 1/15 of the volume of the mixed solution is sampled.

본 발명의 일실시예에 있어서, 상기 정량분석은 Chemical image을 통하여 미세플라스틱의 개수를 분석하는 것을 특징으로 한다. In one embodiment of the present invention, the quantitative analysis is characterized in that the number of microplastics is analyzed through a chemical image.

본 발명은 섬유로부터 미세플라스틱을 용출하여 쉽고 간단하게 분석하는 방법을 제공할 수 있다. The present invention can provide a method for eluting microplastics from fibers and analyzing them easily and simply.

또한 본 발명은 합성섬유나 천연섬유로부터 배출되는 미세섬유의 양을 정확히 분석하고, 이를 통해 배출되는 미세섬유의 양을 줄일 수 있는 방법을 제공할 수 있다. In addition, the present invention can accurately analyze the amount of microfibers discharged from synthetic fibers or natural fibers, and provide a method for reducing the amount of microfibers discharged through this.

도 1은 메쉬 필터에 잔류하는 미세플라스틱의 광학 현미경 사진을 나타낸다.
도 2는 본 발명의 실시예 1의 메쉬 필터에 잔류하는 미세플라스틱의 FT-IR microscope 분석 결과를 나타낸다.
도 3은 본 발명의 실시예 2의 메쉬 필터에 잔류하는 미세플라스틱의 FT-IR microscope 분석 결과를 나타낸다.
도 4는 본 발명의 실시예 3의 메쉬 필터에 잔류하는 미세플라스틱의 FT-IR microscope 분석 결과를 나타낸다.
도 5는 FT-IR microscope 분석을 통하여 측정된 미세플라스틱의 개수를 나타내고 있다.
1 shows an optical micrograph of microplastics remaining in a mesh filter.
2 shows the results of FT-IR microscope analysis of microplastics remaining in the mesh filter of Example 1 of the present invention.
3 shows the results of FT-IR microscope analysis of microplastics remaining in the mesh filter of Example 2 of the present invention.
4 shows the results of FT-IR microscope analysis of microplastics remaining in the mesh filter of Example 3 of the present invention.
5 shows the number of microplastics measured through FT-IR microscope analysis.

이하 실시예를 바탕으로 본 발명을 상세히 설명한다. 본 발명에 사용된 용어, 실시예 등은 본 발명을 보다 구체적으로 설명하고 통상의 기술자의 이해를 돕기 위하여 예시된 것에 불과할 뿐이며, 본 발명의 권리범위 등이 이에 한정되어 해석되어서는 안 된다.Hereinafter, the present invention will be described in detail based on Examples. Terms, examples, etc. used in the present invention are merely exemplified to explain the present invention in more detail and help those of ordinary skill in the art to understand, and the scope of the present invention should not be construed as being limited thereto.

본 발명에 사용되는 기술 용어 및 과학 용어는 다른 정의가 없다면 이 발명이 속하는 기술 분야에서 통상의 지식을 가진 자가 통상적으로 이해하고 있는 의미를 나타낸다. Technical terms and scientific terms used in the present invention represent meanings commonly understood by those of ordinary skill in the art to which this invention belongs, unless otherwise defined.

본 발명은 a) 섬유, 물 및 세제를 교반하여 혼합물을 제조하는 단계;The present invention comprises the steps of a) preparing a mixture by stirring fibers, water and detergent;

b) 상기 혼합물을 필터로 여과하는 단계;b) filtering the mixture with a filter;

c) 상기 필터에 남겨진 잔류물 및 물을 교반하여 혼합액을 제조하는 단계;c) preparing a mixed solution by stirring the residue and water remaining in the filter;

d) 상기 혼합액의 일부를 샘플링하여 필터로 여과하는 단계;d) sampling a portion of the mixed solution and filtering it with a filter;

e) 상기 필터에 남겨진 잔류물을 건조하는 단계; 및e) drying the residue left on the filter; and

f) 상기 건조된 잔류물을 FT-IR microscope을 사용하여 정량분석하는 단계를 포함하는 섬유의 미세플라스틱 분석방법에 관한 것이다. f) quantitatively analyzing the dried residue using an FT-IR microscope.

상기 a) 단계는 섬유, 물 및 세제를 교반하여 혼합물을 제조하는 단계로서, 섬유에 포함된 미세플라스틱을 용출할 수 있다. Step a) is a step of preparing a mixture by stirring the fibers, water, and detergent, and may elute the microplastics contained in the fibers.

상기 섬유는 천연섬유, 합성섬유(폴리에스테르 섬유, 폴리아미드 섬유, 폴리올레핀 섬유, 폴리우레탄 섬유 등) 등이 모두 사용될 수 있다. The fibers may be natural fibers or synthetic fibers (polyester fibers, polyamide fibers, polyolefin fibers, polyurethane fibers, etc.).

상기 혼합물은 섬유 100중량부에 대하여 물 500~2,000중량부 및 세제 1~10중량부를 사용하는 것이 바람직하다. 각 성분의 함량이 상기 수치범위를 만족하는 경우, 섬유에 포함된 미세플라스틱을 쉽게 용출할 수 있고, 교반에 의해 형성되는 미세플라스틱의 양을 최소화 할 수 있다. The mixture is preferably used in an amount of 500 to 2,000 parts by weight of water and 1 to 10 parts by weight of a detergent based on 100 parts by weight of the fiber. When the content of each component satisfies the above numerical range, the microplastic contained in the fiber can be easily eluted, and the amount of microplastic formed by stirring can be minimized.

상기 세제는 통상적인 액체세제, 고체세제 및 종이세제에서 하나 이상 선택될 수 있다. The detergent may be one or more selected from conventional liquid detergents, solid detergents and paper detergents.

또한 상기 세제는 액체세제 및 고체세제를 동시에 사용할 수 있으며, 이때 액체세제 및 고체세제의 중량비는 60~80:20~40인 것이 바람직하고, 상기 수치범위를 만족하는 경우 섬유에 포함된 미세플라스틱을 쉽게 용출할 수 있고, 교반에 의해 형성되는 미세플라스틱의 양을 최소화 할 수 있다. In addition, as the detergent, a liquid detergent and a solid detergent can be used at the same time, and the weight ratio of the liquid detergent and the solid detergent is preferably 60 to 80: 20 to 40, and when the above numerical range is satisfied, the microplastic contained in the fiber is It can be easily eluted, and the amount of microplastics formed by stirring can be minimized.

또한 상기 세제는 액체세제, 고체세제 및 종이세제를 동시에 사용할 수 있으며, 이때 액체세제, 고체세제 및 종이세제의 중량비는 100:20~50:5~15인 것이 바람직하고, 상기 수치범위를 만족하는 경우 섬유에 포함된 미세플라스틱을 쉽게 용출할 수 있고, 교반에 의해 형성되는 미세플라스틱의 양을 최소화 할 수 있다. In addition, as the detergent, a liquid detergent, a solid detergent, and a paper detergent can be used at the same time, and the weight ratio of the liquid detergent, the solid detergent and the paper detergent is preferably 100:20-50:5-15, and satisfies the numerical range. In this case, the microplastics contained in the fibers can be easily eluted, and the amount of microplastics formed by stirring can be minimized.

상기 교반공정은 100~5,000rpm에서 30분~3시간 동안 교반을 수행할 수 있으며, 상기 수치범위를 만족하는 경우, 섬유에 포함된 미세플라스틱을 쉽게 용출할 수 있다. The stirring process can be performed for 30 minutes to 3 hours at 100 to 5,000 rpm, and when the above numerical range is satisfied, the microplastics contained in the fibers can be easily eluted.

상기 b) 단계는 상기 혼합물을 필터로 여과하는 단계로서, 대부분의 액체는 필터를 통과하며, 미세플라스틱을 포함하는 섬유는 필터에 잔류하게 된다. Step b) is a step of filtering the mixture through a filter. Most of the liquid passes through the filter, and the fibers including microplastic remain in the filter.

상기 필터는 메쉬 필터인 것이 바람직하고, 상기 메쉬 필터의 pore size는 1~100㎛인 것이 바람직하다. The filter is preferably a mesh filter, and the pore size of the mesh filter is preferably 1 to 100 μm.

상기 필터에 남겨진 잔류물은 그대로 사용하거나 건조를 진행한 후 다음 단계를 수행할 수 있다. The residue left on the filter may be used as it is, or the next step may be performed after drying.

상기 c) 단계는 상기 필터에 남겨진 잔류물 및 물을 교반하여 혼합액을 제조하는 단계로서, 이를 통해 섬유에 포함된 미세플라스틱의 용출을 보다 쉽게 하고, 용출된 미세플라스틱의 분산성을 개선할 수 있다. Step c) is a step of preparing a mixed solution by stirring the residue and water left in the filter, through which the elution of the microplastic contained in the fiber can be made easier, and the dispersibility of the eluted microplastic can be improved. .

상기 혼합액은 잔류물 100중량부에 대하여 물 1,500~5,000중량부를 사용하는 것이 바람직하다. The mixed solution is preferably used in an amount of 1,500 to 5,000 parts by weight of water based on 100 parts by weight of the residue.

상기 교반공정은 100~5,000rpm에서 30분~3시간 동안 교반을 수행할 수 있으며, 상기 수치범위를 만족하는 경우, 섬유에 포함된 미세플라스틱을 쉽게 용출할 수 있다. The stirring process can be performed for 30 minutes to 3 hours at 100 to 5,000 rpm, and when the above numerical range is satisfied, the microplastics contained in the fibers can be easily eluted.

상기 d) 단계는 상기 혼합액의 일부를 샘플링하여 필터로 여과하는 단계로서, 미세플라스틱의 정확한 정량분석을 위해 혼합액 전부를 필터링하지 않고, 혼합액의 일부만 샘플링한 후 환산을 통하여 혼합액에 포함된 미세플라스틱의 양을 확인할 수 있다. Step d) is a step of sampling a part of the mixed solution and filtering it with a filter. For accurate quantitative analysis of microplastics, the entire mixed solution is not filtered, only a part of the mixed solution is sampled, and then the microplastic contained in the mixed solution is converted. quantity can be checked.

혼합액 전부를 필터링하는 경우, 필터에 남겨진 잔류물은 응집되어 미세플라스틱의 정확한 개수를 측정할 수 없다. When all of the mixed solution is filtered, the residue left on the filter is agglomerated and the exact number of microplastics cannot be measured.

이때 상기 혼합액 부피의 1/5~1/15를 샘플링하는 것이 바람직하며, 상기 수치범위를 만족하는 경우 미세플라스틱의 정확한 개수를 측정할 수 있다. At this time, it is preferable to sample 1/5 to 1/15 of the volume of the mixed solution, and when the numerical range is satisfied, the exact number of microplastics can be measured.

본 발명은 상기 c) 단계 및 d) 단계를 1회 이상 반복할 수 있으며, 이를 통해 섬유에 포함된 미세플라스틱을 쉽게 용출할 수 있으며, 용출된 미세플라스틱의 양을 정확히 분석할 수 있다. In the present invention, steps c) and d) can be repeated one or more times, and through this, the microplastic contained in the fiber can be easily eluted, and the amount of the eluted microplastic can be accurately analyzed.

상기 e) 단계는 상기 필터에 남겨진 잔류물을 건조하는 단계로서, 통상적인 건조공정으로 상기 잔류물을 건조할 수 있다. Step e) is a step of drying the residue left on the filter, and the residue may be dried by a conventional drying process.

상기 f) 단계는 상기 건조된 잔류물을 FT-IR microscope을 사용하여 정량분석하는 단계로서, 상기 정량분석은 Chemical image를 통하여 미세플라스틱의 개수를 분석할 수 있다. Step f) is a step of quantitatively analyzing the dried residue using an FT-IR microscope. The quantitative analysis may analyze the number of microplastics through a chemical image.

이하 실시예를 통해 본 발명을 상세히 설명한다. 하기 실시예는 본 발명의 실시를 위하여 예시된 것일 뿐, 본 발명의 내용이 하기 실시예에 의하여 한정되는 것은 아니다. The present invention will be described in detail with reference to the following examples. The following examples are only exemplified for the practice of the present invention, and the content of the present invention is not limited by the following examples.

(실시예 1)(Example 1)

폴리에스테르 섬유 10g, 물 100㎖ 및 고체세제 0.1~0.5g를 500rpm에서 1시간 동안 교반하여 혼합물을 제조하였다. 10 g of polyester fiber, 100 ml of water, and 0.1 to 0.5 g of a solid detergent were stirred at 500 rpm for 1 hour to prepare a mixture.

상기 혼합물을 47mm 메쉬 필터(pore size 50㎛)로 여과하였다. The mixture was filtered through a 47mm mesh filter (pore size 50㎛).

상기 필터에 남겨진 잔류물에 물 300㎖을 첨가하고 500rpm에서 1시간 동안 교반하여 혼합액을 제조하였다. 300 ml of water was added to the residue left on the filter and stirred at 500 rpm for 1 hour to prepare a mixed solution.

상기 혼합액 부피의 1/10을 샘플링하여 47mm 메쉬 필터(pore size 50㎛)로 여과하였다. 1/10 of the volume of the mixed solution was sampled and filtered with a 47 mm mesh filter (pore size 50 μm).

상기 필터에 남겨진 잔류물을 상온에서 건조하였다. The residue left on the filter was dried at room temperature.

상기 건조된 잔류물을 FT-IR microscope(Nicolet iN 10 MX)을 사용하여 정량분석하였다. The dried residue was quantitatively analyzed using an FT-IR microscope (Nicolet iN 10 MX).

도 1은 메쉬 필터에 잔류하는 미세플라스틱의 광학 현미경 사진을 나타내고 있다. 1 shows an optical micrograph of microplastics remaining in a mesh filter.

도 2는 메쉬 필터에 잔류하는 미세플라스틱의 FT-IR microscope 분석 결과를 나타내고 있다. 2 shows the results of FT-IR microscope analysis of microplastics remaining in the mesh filter.

(실시예 2)(Example 2)

고체세제 대신에, 종이세제를 사용한 것을 제외하고는 실시예 1과 동일한 방법으로 분석을 수행하였다. The analysis was performed in the same manner as in Example 1, except that paper detergent was used instead of the solid detergent.

도 3은 메쉬 필터에 잔류하는 미세플라스틱의 FT-IR microscope 분석 결과를 나타내고 있다. 3 shows the results of FT-IR microscope analysis of microplastics remaining in the mesh filter.

(실시예 3)(Example 3)

고체세제 대신에, 액체세제를 사용한 것을 제외하고는 실시예 1과 동일한 방법으로 분석을 수행하였다. The analysis was performed in the same manner as in Example 1, except that a liquid detergent was used instead of the solid detergent.

도 4는 메쉬 필터에 잔류하는 미세플라스틱의 FT-IR microscope 분석 결과를 나타내고 있다. 4 shows the results of FT-IR microscope analysis of microplastics remaining in the mesh filter.

도 5는 FT-IR microscope 분석을 통하여 측정된 미세플라스틱의 개수를 나타내고 있다. 5 shows the number of microplastics measured through FT-IR microscope analysis.

고체세제 또는 종이세제를 사용한 경우 세제 량에 관계없이 많은 양의 미세플라스틱 개수가 확인되었고, 액체세제를 사용한 경우 미세플라스틱의 개수가 적었으며 세제 량이 증가함에 따라 미세플라스틱의 개수가 증가함을 알 수 있다. When solid detergent or paper detergent was used, a large amount of microplastics was confirmed regardless of the amount of detergent, and when liquid detergent was used, the number of microplastics was small, and it was found that the number of microplastics increased as the amount of detergent increased. have.

(실시예 4)(Example 4)

액체세제 0.3g 대신에, 액체세제 0.2g 및 고체세제 0.1g를 사용한 것을 제외하고는 실시예 3과 동일한 방법으로 분석을 수행하였다. The analysis was performed in the same manner as in Example 3, except that 0.2 g of liquid detergent and 0.1 g of solid detergent were used instead of 0.3 g of liquid detergent.

(실시예 5)(Example 5)

상기 필터에 남겨진 잔류물에 물 300㎖을 첨가하고 500rpm에서 1시간 동안 교반하여 혼합액을 제조하는 단계; 및adding 300 ml of water to the residue left on the filter and stirring at 500 rpm for 1 hour to prepare a mixed solution; and

상기 혼합액 부피의 1/10을 샘플링하여 47mm 메쉬 필터(pore size 50㎛)로 여과하는 단계를 1회 반복한 것을 제외하고는 실시예 3과 동일한 방법으로 분석을 수행하였다. Analysis was performed in the same manner as in Example 3, except that the step of sampling 1/10 of the volume of the mixed solution and filtering with a 47 mm mesh filter (pore size 50 μm) was repeated once.

(비교예 1)(Comparative Example 1)

폴리에스테르 섬유 10g, 물 100㎖ 및 액체세제 0.3g를 500rpm에서 1시간 동안 교반하여 혼합물을 제조하였다. 10 g of polyester fiber, 100 ml of water, and 0.3 g of liquid detergent were stirred at 500 rpm for 1 hour to prepare a mixture.

상기 혼합물을 47mm 메쉬 필터(pore size 50㎛)로 여과하였다. The mixture was filtered through a 47mm mesh filter (pore size 50㎛).

상기 필터에 남겨진 잔류물을 상온에서 건조하였다. The residue left on the filter was dried at room temperature.

상기 건조된 잔류물을 FT-IR microscope(Nicolet iN 10 MX)을 사용하여 정량분석하였다. The dried residue was quantitatively analyzed using an FT-IR microscope (Nicolet iN 10 MX).

(분산성)(dispersibility)

상기 건조된 잔류물의 응집도 및 분산성을 광학 현미경으로 관찰하여 탁월, 우수, 보통 및 열등으로 표기하였다. The degree of agglomeration and dispersibility of the dried residue was observed under an optical microscope and marked as excellent, excellent, average and inferior.

실시예 Example 비교예comparative example 1One 22 33 44 55 1One 미세플라스틱의 개수number of microplastics 517517 413413 315315 274274 306306 562562 분산성dispersibility 우수Great 우수Great 우수Great 탁월eminence 탁월eminence 열등inferior

상기 표 1에서 볼 수 있는 바와 같이, 본 발명의 실시예 1 내지 5는 미세플라스틱의 개수가 적고 분산성이 우수함을 알 수 있으며, 특히 실시예 4 및 5는 상기 특성이 가장 우수함을 확인할 수 있다. As can be seen in Table 1, it can be seen that Examples 1 to 5 of the present invention have a small number of microplastics and excellent dispersibility, and in particular, Examples 4 and 5 have the best properties. .

반면 비교예 1은 실시예에 비해 상기 특성이 열등함을 알 수 있다. On the other hand, it can be seen that Comparative Example 1 has inferior properties compared to Example.

Claims (6)

a) 섬유, 물 및 세제를 교반하여 혼합물을 제조하는 단계;
b) 상기 혼합물을 필터로 여과하는 단계;
c) 상기 필터에 남겨진 잔류물 및 물을 교반하여 혼합액을 제조하는 단계;
d) 상기 혼합액의 일부를 샘플링하여 필터로 여과하는 단계;
e) 상기 필터에 남겨진 잔류물을 건조하는 단계; 및
f) 상기 건조된 잔류물을 FT-IR microscope을 사용하여 정량분석하는 단계를 포함하는 섬유의 미세플라스틱 분석방법에 있어서,
상기 a) 단계는 섬유 100중량부에 대하여 물 500~2,000중량부 및 세제 1~10중량부를 사용하고,
상기 세제는 액체세제 및 고체세제를 동시에 사용하고,
상기 액체세제 및 고체세제의 중량비는 60~80:20~40 이며,
상기 d) 단계는 혼합액 부피의 1/5~1/15를 샘플링하고,
상기 정량분석은 Chemical image 을 통하여 미세플라스틱의 개수를 분석하는 것을 특징으로 하는 섬유의 미세플라스틱 분석방법.
a) agitating the fibers, water and detergent to prepare a mixture;
b) filtering the mixture with a filter;
c) preparing a mixed solution by stirring the residue and water remaining in the filter;
d) sampling a portion of the mixed solution and filtering it with a filter;
e) drying the residue left on the filter; and
f) In the microplastic analysis method of fibers comprising the step of quantitatively analyzing the dried residue using an FT-IR microscope,
Step a) uses 500 to 2,000 parts by weight of water and 1 to 10 parts by weight of detergent based on 100 parts by weight of the fiber,
The detergent uses a liquid detergent and a solid detergent at the same time,
The weight ratio of the liquid detergent and the solid detergent is 60 ~ 80: 20 ~ 40,
Step d) samples 1/5 to 1/15 of the volume of the mixed solution,
The quantitative analysis is a method for analyzing microplastics of fibers, characterized in that the number of microplastics is analyzed through a chemical image.
삭제delete 제1항에 있어서,
상기 필터는 메쉬 필터인 것을 특징으로 하는 섬유의 미세플라스틱 분석방법.
The method of claim 1,
The filter is a microplastic analysis method of fibers, characterized in that the mesh filter.
제3항에 있어서,
상기 c) 단계 및 d) 단계를 1회 이상 반복하는 것을 특징으로 하는 섬유의 미세플라스틱 분석방법.
4. The method of claim 3,
Method for analyzing microplastics of fibers, characterized in that the steps c) and d) are repeated one or more times.
삭제delete 삭제delete
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR102135690B1 (en) 2020-02-20 2020-07-20 상림이엔지 주식회사 Waste water quality monitoring system including water treatment rtu with fine plastic detection
WO2020161585A1 (en) * 2019-02-08 2020-08-13 Polygone Technologies Inc. Characterization of plastic contamination of fluids using imagery of filter media

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS62276447A (en) * 1986-05-26 1987-12-01 Matsushita Electric Works Ltd Filter paper for fluorescent x-ray quantitative analysis
KR102284023B1 (en) * 2019-05-09 2021-07-30 한국광기술원 Apparatus and Method for Detecting Micro-Particle Using Raman Spectroscopy
KR102178099B1 (en) 2020-08-19 2020-11-12 대한민국 Precision sampling device for microplastic analysis in seawater

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2020161585A1 (en) * 2019-02-08 2020-08-13 Polygone Technologies Inc. Characterization of plastic contamination of fluids using imagery of filter media
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