KR102130912B1 - Sensitive detecting method for detergent component linear alkyl benzene sulfonate utilizing methylene blue and hydrophobic silica - Google Patents

Sensitive detecting method for detergent component linear alkyl benzene sulfonate utilizing methylene blue and hydrophobic silica Download PDF

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KR102130912B1
KR102130912B1 KR1020190016178A KR20190016178A KR102130912B1 KR 102130912 B1 KR102130912 B1 KR 102130912B1 KR 1020190016178 A KR1020190016178 A KR 1020190016178A KR 20190016178 A KR20190016178 A KR 20190016178A KR 102130912 B1 KR102130912 B1 KR 102130912B1
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methylene blue
straight
hydrophobic silica
detection
alkylsulfonic acid
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오제민
목철균
김보경
이도연
이홍범
정진송
고수정
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가천대학교 산학협력단
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    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract

The present invention relates to a method of detecting a trace of linear alkyl benzene sulfonate (LABS) of a detergent component utilizing methylene blue and hydrophobic silica, configured to use a reaction in which methylene blue and linear alkyl benzene sulfonate form a hydrophobic complex to make hydrophobic C-18 silica powder to react with the hydrophobic complex, and thus, it is possible to detect 0.55 ppm or more of the linear alkyl benzene sulfonate simply by observing a change in color of the powder. Through this method, it is possible to easily detect linear alkyl benzene sulfonate in the field without the use of an organic solvent such as chloroform or a toxic solvent that were mainly used in an existing method.

Description

메틸렌블루 및 소수성 실리카를 이용한 세척제 성분 직쇄알킬술폰산의 미량 검출 방법 {Sensitive detecting method for detergent component linear alkyl benzene sulfonate utilizing methylene blue and hydrophobic silica} {Sensitive detecting method for detergent component linear alkyl benzene sulfonate utilizing methylene blue and hydrophobic silica}

본 발명은 메틸렌블루 및 소수성 실리카를 이용한 세척제 성분 직쇄알킬술폰산(Linear alkyl benzene sulfonate; LABS)의 미량 검출 방법에 관한 것이다. The present invention relates to a method for detecting trace amounts of linear alkyl benzene sulfonate (LABS) as a detergent component using methylene blue and hydrophobic silica.

세척제는 위생용품 중에서도 일상생활에서 가장 빈번하게 사용되는 위생용품으로 채소/과일부터 조리기구의 세척까지 광범위하게 사용된다. 세척제는 그 용도에 따라 세 가지 유형으로 구분되며, 1종 세척제는 사람이 그대로 먹을 수 있는 채소/과일 등을 씻는 데 사용되는 것, 2종 세척제는 가공기구, 조리기구 등 자동식기세척기를 포함한 식품 기구/용기를 씻는데 사용되는 것, 3종 세척제는 식품의 제조장치, 가공장치 등 제조/가공용 기구 등을 씻는데 사용되는 것을 말한다. The cleaning agent is the most frequently used hygiene product among daily hygiene products, and is widely used from vegetables/fruits to cleaning of cooking utensils. The cleaning agents are divided into three types according to their use, and the first type cleaning agent is used to wash vegetables/fruits that can be eaten by humans, and the second type cleaning agent is food including automatic dishwashers such as processing equipment and cooking utensils. It is used to wash utensils/containers, and three kinds of cleaning agents are used to wash utensils for manufacturing/processing such as food production equipment and processing equipment.

1종 세척제를 사용하는 경우 세척제 용액에 채소나 과일을 5분 이상 담그면 안되고, 1종 세척제로 채소, 과일, 음식기 또는 조리기구를 씻은 후에는 반드시 마시기 적합한 물로 씻어야 한다. 이 때 흐르는 물을 사용할 때에는 채소나 과일은 30초 이상, 식기류는 5초 이상 씻고 흐르지 않는 물을 사용할 때에는 물을 교환하여 2회 이상 씻어야 한다. 2종이나 3종 세척제를 사용한 후에도 음식기나 조리기구에 세척제가 잔류하지 않도록 마시기 적합한 물로 씻어야 하며, 용도 이외로 사용하거나 규정 사용량 이상을 사용하지 않도록 주의해야 한다.When using a class 1 detergent, do not immerse the vegetables or fruits in the detergent solution for more than 5 minutes, and after washing the vegetables, fruits, food or cooking utensils with the class 1 detergent, be sure to wash with water suitable for drinking. At this time, when using flowing water, wash vegetables or fruits for more than 30 seconds, and dishware for 5 seconds or more. When using non-flowing water, exchange water and wash it more than 2 times. After using two or three types of detergent, wash with water suitable for drinking so that no detergent remains on the food or cooking utensils, and be careful not to use other than intended use or use more than the prescribed amount.

그러나 이러한 세척방법이 규정상 잘 지켜지지 않거나 세척 상의 부주의, 세척제 성분의 강한 잔류 기능 등으로 인해, 잔류 세척제 성분이 채소나 과일, 조리기구 등에 잔류하고, 이들 성분이 체내에 유입되어 독성성분으로 작용하고 아토피, 알레르기 등의 피부질환을 일으키며, 환경호르몬 등으로 작용하여 성조숙증 등을 유발함으로써 내분비계를 교란시키는 등의 각종 문제원인이 되어 왔다. However, because these cleaning methods are not well adhered to by regulations, or due to carelessness in cleaning, strong residual function of the cleaning agent ingredients, residual cleaning agent ingredients remain in vegetables, fruits, cooking utensils, etc., and these ingredients enter the body and act as toxic ingredients. In addition, it causes skin diseases such as atopy and allergies, and acts as an environmental hormone to induce premature ejaculation, causing various problems such as disturbing the endocrine system.

한편, 세척제에는 매우 다양한 성분들이 존재하고 있으며, 함량도 편차가 큰 것으로 나타나고, 특정 성분은 세척 과정 중에 쉽게 씻겨 내려가서 검출이 어려울 수도 있으며, 간이 검출 키트로 분석하기 어려운 경우도 많은 것으로 분석된다. 이러한 점들을 고려하여 분석의 용이성과 세척제 내 성분의 범용성 등을 고려하여 음이온계 계면활성제인 직쇄알킬술폰산(Linear alkyl benzene sulfonate; LABS)이 세척제의 주요 성분인 계면활성제로 알려진 바, 직쇄알킬술폰산의 잔류량을 확인하는 것은 채소나 과일, 조리기구 등에서 세척제가 잘 제거되었음을 나타내는 지표로 여겨질 수 있다. On the other hand, a wide variety of components are present in the cleaning agent, the content also appears to have a large variation, and certain components may be easily washed down during the washing process, making it difficult to detect, and it is also analyzed that it is difficult to analyze with a simple detection kit. Considering these points, the anionic surfactant linear alkyl benzene sulfonate (LABS) is known as the surfactant which is the main component of the detergent, considering the ease of analysis and the versatility of the components in the detergent. Checking the residual amount can be considered as an indicator that the cleaning agent is well removed from vegetables, fruits, and cookware.

기존의 직쇄알킬술폰산 검출 방법은 유기염료인 메틸렌블루(methylene blue;MB)를 사용하여 직쇄알킬술폰산 포함 용액과 클로로포름을 혼합한 후 직쇄알킬술폰산과 메틸렌블루 혼합체를 클로로포름 층으로 분리하여 직쇄알킬술폰산 함량에 따른 흡광도를 육안으로 구분하여 확인하는 방식이었다(환경부 방법의 명칭 : 먹는물수질공정시험기준에 따른 자외선/가시선 분광법(Surfactants-UV /Visible Spectrometry). The conventional method for detecting a straight-chain alkylsulfonic acid is a mixture of a straight-chain alkylsulfonic acid-containing solution and chloroform using methylene blue (MB), an organic dye, and then the straight-chain alkylsulfonic acid and methylene blue mixture are separated into a chloroform layer to remove the straight-chain alkylsulfonic acid content. It was a method to check the absorbance according to the naked eye by the naked eye (Name of the Ministry of Environment method: UV/Visible Spectrometry according to the drinking water quality process test standard.

그러나, 종래의 방법은 독성과 휘발성이 강한 클로로포름을 사용하기 때문에 테스트를 수행하는 사람의 안전성 문제가 있으며, 실제 클로로포름을 사용하는 키트는 밀봉된 제품임에도 클로로포름 냄새가 많이 나며, 클로로포름을 이용하여 시험물들을 혼합하는 과정이 간단하지 않은 관계로 현장에서 손쉽게 잔류물을 검출하는 것이 어려운 문제점이 있어 사용이 용이하지 않았다. However, the conventional method uses chloroform, which is highly toxic and volatile, so there is a safety problem of the person performing the test, and the kit using actual chloroform has a lot of chloroform odor even though it is a sealed product, and the test products using chloroform Because the process of mixing was not simple, it was difficult to easily detect residues in the field, so it was not easy to use.

따라서, 본 발명자들은 상기 직쇄알킬술폰산 성분과 메틸렌 블루가 반응하여 발색을 일으키는 시약을 제조하여, 과일이나 채소, 각종 식기류에 잔류하는 에티드론산의 존재 유무를 검출하는 방법을 개발함으로써 본 발명을 완성하게 되었다. Therefore, the present inventors completed the present invention by developing a method for detecting the presence or absence of etidronic acid remaining in fruits, vegetables, and various dishes by preparing a reagent that causes color development by reacting the linear alkylsulfonic acid component with methylene blue. Was done.

대한민국 등록특허 제10-1503638호 (발명의 명칭 : 생활환경제품에서 유해 살균제 성분의 검출 방법 및 검출 키트, 출원인 : 영남대학교 산학협력단, 등록일 : 2015년03월11일)Republic of Korea Registered Patent No. 10-1503638 (Invention name: Method and detection kit for the detection of harmful disinfectant components in living environment products, Applicant: Yeungnam University Industry-University Cooperation Foundation, Registration Date: March 11, 2015) 대한민국 등록특허 제10-1321736호 (발명의 명칭 : ＭＩＢＫ-ＥＤＣ 혼합용매 추출법에 의한 해수 및 환경수질 시료에 함유된 음이온 계면활성제의 분광학적 정량방법, 출원인 : 강원도, 강원대학교산학협력단, 등록일 : 2013년10월18일)Republic of Korea Registered Patent No. 10-1321736 (Invention name: Spectroscopic quantitative method of anionic surfactant contained in seawater and environmental water samples by the MIP-EDC mixed solvent extraction method, Applicant: Gangwon-do, Kangwon National University Academic Cooperation Foundation, Registration Date: 2013 October 18) 대한민국 등록특허 제10-1310428호 (발명의 명칭 : 잔류 세제의 검출 방법 및 잔류 세제 검출 도구, 출원인 : 가부시키가이샤 루미카, 등록일 : 2013년09월12일)Republic of Korea Registered Patent No. 10-1310428 (Invention name: Residual detergent detection method and residual detergent detection tool, Applicant: Kabushiki Kaisha Lumica, Registration date: September 12, 2013) 대한민국 등록특허 제10-1095475호 (발명의 명칭 : 음이온 계면활성제 선택성을 갖는 폴리아세틸렌 초분자체, 이의 제조방법 및 이를 이용한 음이온 계면활성제 검출방법, 출원인 : 이화여자대학교 산학협력단, 등록일 : 2011년12월12일)Republic of Korea Registered Patent No. 10-1095475 (Invention name: Polyacetylene supramolecular sieve having anionic surfactant selectivity, manufacturing method thereof and anionic surfactant detection method using the same, Applicant: Ewha Womans University Industry-Academic Cooperation Foundation, Registration Date: December 2011 12 days)

E. Jurado , M. Fernandez-Serrano, J. Nunez-Olea, G. Luzon, M. Lechuga, Simplified spectrophotometric method using methylene blue for determining anionic surfactants: Applications to the study of primary biodegradation in aerobic screening tests. Chemosphere, 2006, 65(2) 278~285.E. Jurado, M. Fernandez-Serrano, J. Nunez-Olea, G. Luzon, M. Lechuga, Simplified spectrophotometric method using methylene blue for determining anionic surfactants: Applications to the study of primary biodegradation in aerobic screening tests. Chemosphere, 2006, 65(2) 278~285.

본 발명의 목적은 메틸렌블루 및 소수성 실리카를 이용한 세척제 성분 직쇄알킬술폰산(Linear alkyl benzene sulfonate; LABS)의 미량 검출 방법을 제공하는 데에 있다.An object of the present invention is to provide a trace detection method of linear alkyl benzene sulfonate (LABS) as a detergent component using methylene blue and hydrophobic silica.

(제1단계) 메틸렌블루(Methylene blue) 수용액, 소수성 실리카 분말 및 물을 준비하는 단계;(First step) preparing an aqueous solution of methylene blue, hydrophobic silica powder and water;

(제2단계) 소수성 실리카 분말과 메틸렌블루 수용액 및 직쇄알킬술폰산(Linear alkyl benzene sulfonate)의 잔류상태를 확인하고자 하는 세척액을 혼합하여 혼합 액상을 제조하고, 물을 더 첨가하여 혼합한 후 여과하여 소수성 실리카 반응물을 얻는 단계; 및,(Second step) A mixed liquid was prepared by mixing a hydrophobic silica powder with a methylene blue aqueous solution and a washing liquid to check the residual state of linear alkyl benzene sulfonate, and further adding water to mix and then filtering to obtain hydrophobicity. Obtaining a silica reactant; And,

(제3단계) 여과하여 얻은 소수성 실리카 반응물을 건조하여 분말의 색상을 확인하는 단계;를 포함하는 메틸렌블루 및 소수성 실리카를 이용한 세척제 성분 직쇄알킬술폰산의 미량 검출 방법에 관한 것이다. (Step 3) drying the hydrophobic silica reactant obtained by filtration to check the color of the powder; relates to a trace amount detection method of a straight-chain alkylsulfonic acid component using methylene blue and hydrophobic silica.

상기 제1단계의 메틸렌블루 수용액의 농도는 적어도 80ppm 이상, 더 바람직하게는 80~120ppm인 것이 좋다. 메틸렌블루 수용액의 농도가 80ppm 미만일 경우 직쇄알킬술폰산의 검출이 잘 되지 않을 수 있다. 메틸렌블루 수용액의 농도는 80ppm 이상만 되면 반응이 잘 일어나기는 하지만, 제조비용 면에서 120ppm 이내의 농도까지만 사용하여도 직쇄알킬술폰산의 검출이 효율적으로 잘 이루어진다. The concentration of the aqueous solution of methylene blue in the first step is at least 80 ppm or more, more preferably 80 to 120 ppm. When the concentration of the methylene blue aqueous solution is less than 80 ppm, detection of a straight chain alkylsulfonic acid may not be performed well. When the concentration of the methylene blue aqueous solution is 80 ppm or more, the reaction occurs well, but detection of a straight-chain alkylsulfonic acid is efficiently performed even when the concentration is within 120 ppm in terms of manufacturing cost.

상기 제1단계의 소수성 실리카 분말은 옥타데실실란(C-18)이 코팅된 실리카 분말을 사용하는 것이 바람직하다. 옥타실란(C-8) 또는 도데실실란(C-12)이 코팅된 실리카 분말을 사용할 경우 직쇄알킬술폰산의 검출이 잘 되지 않을 수 있다. It is preferable to use octadecylsilane (C-18) coated silica powder as the hydrophobic silica powder in the first step. When using a silica powder coated with octasilane (C-8) or dodecylsilane (C-12), detection of a straight chain alkylsulfonic acid may not be performed well.

상기 제2단계에서, 메틸렌블루 수용액 1㎖ 기준으로 소수성 실리카 분말 8~12 ㎎, 잔류상태를 확인하고자 하는 세척액을 0.5~2㎖ 준비하여, 소수성 실리카 분말에 메틸렌블루 수용액과 잔류상태를 확인하고자 하는 세척액을 혼합하고, 물을 추가하여 메틸렌블루 수용액 1㎖ 기준으로 최종 부피가 13~17㎖이 되도록 하는 것이 좋다. In the second step, based on 1 ml of methylene blue aqueous solution, 8 to 12 mg of hydrophobic silica powder, and 0.5 to 2 ml of a washing solution to check the residual state are prepared, and the aqueous solution of methylene blue and the residual state of hydrophobic silica powder are to be checked. It is good to mix the washing solution and add water to make the final volume 13 to 17 mL based on 1 mL of methylene blue aqueous solution.

이 때, 소수성 실리카 분말이 8 ㎎ 미만일 경우, 직쇄알킬술폰산의 검출이 잘 되지 않을 수 있거나, 직쇄알킬술폰산의 검출이 가능한다 할지라도 직쇄알킬술폰산의 존재 유무만 파악할 수 있을 뿐, 도 2의 결과와 같이 농도별 정량 검출이 용이하지 않을 수 있어 바람직하지 않다. 또한 이 과정에서 소수성 실리카 분말이 12 ㎎이 초과될 경우, 검출 가능한 직쇄알킬술폰산의 최저 농도가 더 높아질 수 있어 검출민감도가 저하되어 바람직하지 않다. At this time, when the hydrophobic silica powder is less than 8 mg, the detection of the straight-chain alkylsulfonic acid may not be performed well, or even if the detection of the straight-chain alkylsulfonic acid is possible, only the presence or absence of the straight-chain alkylsulfonic acid can be determined, and the result of FIG. As such, it is not preferable because quantitative detection by concentration may not be easy. In addition, when the hydrophobic silica powder exceeds 12 mg in this process, the minimum concentration of detectable straight-chain alkylsulfonic acid may be higher, which is not preferable because the detection sensitivity is lowered.

상기 제2단계에서 소수성 실리카 반응물의 여과는 거름종이나 천, 부직포 등의 통상의 여과지를 통해 여과할 수 있으며, 여과 과정은 자연적으로 여과가능하나 반응시간을 단축하기 위해 감압여과기를 이용할 수도 있다. In the second step, the filtration of the hydrophobic silica reactant may be filtered through a common filter paper such as filter paper, cloth, or non-woven fabric, and the filtration process may be naturally filtered, but a vacuum filter may be used to shorten the reaction time.

상기 제2단계에서 세척액은 과일, 채소 또는 식기의 세척액인 것을 특징으로 하며, 더 바람직하게는 직쇄알킬술폰산이 포함된 세척제로 세척된 과일, 채소 또는 식기의 표면에 잔류된 직쇄알킬술폰산을 확인하기 위해, 세척이 완료된 과일, 채소 또는 식기를 추가로 더 세척하여 얻은 세척액일 수 있다. 즉, 이러한 용이한 방법으로 검출액을 얻어 세척제가 사용된 과일, 채소 또는 식기의 표면에 잔류된 직쇄알킬술폰산을 용이하게 검출할 수 있다. The washing liquid in the second step is characterized in that it is a washing liquid of fruits, vegetables or dishes, more preferably to check the straight-chain alkyl sulfonic acids remaining on the surface of the fruits, vegetables or dishes washed with a washing agent containing a straight-chain alkyl sulfonic acid. To this end, it may be a washing solution obtained by further washing the fruits, vegetables, or dishes that have been washed. That is, it is possible to easily detect the straight-chain alkylsulfonic acid remaining on the surface of the fruit, vegetable or tableware in which the cleaning agent is used by obtaining the detection solution by this easy method.

상기 제3단계에서 소수성 실리카 반응물을 건조하는 과정은 20~35℃에서 수행될 수 있다. 이때 소수성 실리카 반응물을 건조하는 것은 감압여과를 통해 건조시 3~5분에 가능하며, 감압여과를 하지 않아도 10~15분 정도에 건조가 가능하다. The process of drying the hydrophobic silica reactant in the third step may be performed at 20 ~ 35 ℃. At this time, drying the hydrophobic silica reactant is possible in 3 to 5 minutes when drying through reduced pressure filtration, and drying is possible in about 10 to 15 minutes without filtration under reduced pressure.

또한 상기 제3단계에서 혼합액상에 직쇄알킬술폰산 표준 용액이 첨가된 표준시료군이 준비될 수 있다. 따라서 상기 제3단계에서 표준시료군을 준비하기 위해, 직쇄알킬술폰산 표준 용액을 첨가할 때도, 직쇄알킬술폰산 표준 용액(수용액)이 세척액과 동일 부피로 첨가될 수 있다. 즉, 메틸렌블루 수용액 1㎖ 기준으로 직쇄알킬술폰산 표준 용액도 농도별로 0.5~2㎖씩 첨가될 수 있다. 이 때, 직쇄알킬술폰산의 잔류유무만 확인하고자 한다면, 0.5~100ppm의 직쇄알킬술폰산 표준 용액 중 한가지 농도만 준비하여도 되며, 직쇄알킬술폰산의 농도별 정량 검출이 필요하다면 0~100ppm의 농도 구간별 수용액이 필요하다. 이 때, 검출가능한 최소농도인 0.5ppm의 직쇄알킬술폰산 수용액이 반드시 포함되는 것이 좋다. In addition, in the third step, a standard sample group in which a standard solution of linear alkylsulfonic acid is added to the mixed solution may be prepared. Therefore, in order to prepare a standard sample group in the third step, when adding a standard solution of a straight-chain alkylsulfonic acid, a standard solution of a straight-chain alkylsulfonic acid (aqueous solution) can be added in the same volume as the washing solution. That is, the standard solution of a straight-chain alkylsulfonic acid based on 1 ml of a methylene blue aqueous solution may also be added at 0.5 to 2 ml for each concentration. At this time, if only the presence or absence of a straight-chain alkylsulfonic acid is to be checked, only one concentration of a standard solution of a straight-chain alkylsulfonic acid of 0.5 to 100 ppm may be prepared, and if quantitative detection by concentration of the straight-chain alkylsulfonic acid is necessary, concentration sections of 0 to 100 ppm are required. An aqueous solution is required. At this time, it is preferable that an aqueous solution of straight-chain alkylsulfonic acid having a minimum detectable concentration of 0.5 ppm is included.

이와 같은 본 발명의 직쇄알킬술폰산 검출방법에 대한 원리는 다음과 같다. 즉, 소수성 C-18 실리카 분말의 경우 물에 녹지 않고, 친수성 메틸렌블루는 소수성 C-18 실리카와 반응하지 않는데, 메틸렌블루는 양이온성 염료이고 직쇄알킬술폰산은 음이온성 계면활성제이기 때문에 메틸렌블루와 직쇄알킬술폰산이 반응하면 소수성 복합체를 형성한다. 그리고, 메틸렌블루-직쇄알킬술폰산 복합체는 소수성인 C-18 실리카와 반응하는데, 직쇄알킬술폰산의 농도가 높을수록 메틸렌블루-직쇄알킬술폰산 복합체의 양이 많아지고 파란색 C-18 실리카 분말의 양이 많아지는 것이다. 따라서, 직쇄알킬술폰산의 농도가 높을수록 진한 파란색에 가까운 분말을 확인할 수 있고, 직쇄알킬술폰산의 존재 유무를 최소 0.5 ppm 농도에서도 확인이 가능한 것이다. The principle of the method for detecting a straight-chain alkylsulfonic acid of the present invention is as follows. That is, in the case of hydrophobic C-18 silica powder, it does not dissolve in water, and hydrophilic methylene blue does not react with hydrophobic C-18 silica. Since methylene blue is a cationic dye and linear alkylsulfonic acid is an anionic surfactant, it is linear with methylene blue. When the alkylsulfonic acid reacts, a hydrophobic complex is formed. And, the methylene blue-chain alkylsulfonic acid complex reacts with hydrophobic C-18 silica. The higher the concentration of the straight chain alkylsulfonic acid, the higher the amount of methylene blue-chain alkylsulfonic acid complex and the higher the amount of blue C-18 silica powder. Is to lose. Therefore, the higher the concentration of the straight-chain alkylsulfonic acid, the closer the dark blue powder can be confirmed, and the presence or absence of the straight-chain alkylsulfonic acid can be confirmed even at a minimum concentration of 0.5 ppm.

이에, 본 발명은 상기 방법을 이용하는 직쇄알킬술폰산 검출용 키트를 제공한다. Accordingly, the present invention provides a kit for detecting a straight-chain alkylsulfonic acid using the above method.

또 다른 양태에서, 본 발명은 메틸렌블루 수용액 및 소수성 실리카 분말을 포함하는 직쇄알킬술폰산 검출용 키트 또는 조성물을 제공할 수 있다. 상기 검출용 키트 또는 조성물에는 직쇄알킬술폰산 수용액이 표준용액으로 포함될 수 있다. In another aspect, the present invention can provide a kit or composition for detecting a straight-chain alkylsulfonic acid comprising an aqueous methylene blue solution and hydrophobic silica powder. The detection kit or composition may include a straight-chain alkylsulfonic acid aqueous solution as a standard solution.

본 발명은 메틸렌블루 및 소수성 실리카를 이용한 세척제 성분 직쇄알킬술폰산(Linear alkyl benzene sulfonate; LABS)의 미량 검출 방법에 관한 것으로서, 메틸렌블루와 직쇄알킬술폰산이 소수성 복합체를 형성하는 반응을 이용하여 소수성 C-18 실리카 분말과의 반응을 통한 분말의 색 변화를 관찰하는 것만으로도 0.5 ppm 이상의 직쇄알킬술폰산의 검출이 가능하고, 이와 같은 방법을 통해 기존 방법에서 주로 이용하였던 클로로포름 등의 유기용매나 독성 용매의 사용을 배제하며 현장에서도 손쉽게 직쇄알킬술폰산을 용이하게 검출할 수 있다. The present invention relates to a method for detecting trace amounts of linear alkyl benzene sulfonate (LABS) as a cleaning agent component using methylene blue and hydrophobic silica, wherein a hydrophobic C- is used by using a reaction in which methylene blue and a linear alkyl sulfonic acid form a hydrophobic complex. 18 It is possible to detect a straight chain alkylsulfonic acid of 0.5 ppm or more by simply observing the color change of the powder through reaction with silica powder, and through this method, it is possible to remove organic solvents such as chloroform or toxic solvents mainly used in existing methods. Excluding use, it is possible to easily detect straight-chain alkylsulfonic acids even in the field.

도 1은 본 발명의 실시예 1에 개시된 메틸렌블루(100ppm methylen blue)와 실리카(C-18 silica powder)를 이용하여 직쇄알킬술폰산(LABS)을 검출하는 방법을 나타내는 모식도이다.
도 2는 실시예 1에서 최종적으로 거름종이로 걸러낸 분말을 건조시킨 후 powder의 색(상단)을 확인한 것으로서, 분말 색상 위의 수치는 0, 0.2, 0.5, 1, 5, 10, 20, 50, 100 ppm의 직쇄알킬술폰산(LABS) 농도를 가리키며, 하단의 파란색 지표는 각 분말 색상을 기준으로 각 농도별 기준색상을 제시한 것이다. 1 is a schematic view showing a method for detecting a straight chain alkyl sulfonic acid (LABS) using methylene blue (100 ppm methylen blue) and silica (C-18 silica powder) disclosed in Example 1 of the present invention.
FIG. 2 shows the color (top) of the powder after drying the powder finally filtered with filter paper in Example 1, and the values above the powder color are 0, 0.2, 0.5, 1, 5, 10, 20, 50 , Indicates the concentration of 100 ppm of straight-chain alkylsulfonic acid (LABS), and the blue index at the bottom shows the reference color for each concentration based on the color of each powder.

이하, 본 발명의 이해를 돕기 위하여 실시예를 들어 상세하게 설명하기로 한다. 다만 하기의 실시예는 본 발명의 내용을 예시하는 것일 뿐 본 발명의 범위가 하기 실시예에 한정되는 것은 아니다. 본 발명의 실시예는 당업계에서 평균적인 지식을 가진 자에게 본 발명을 보다 완전하게 설명하기 위해 제공되는 것이다.Hereinafter, examples will be described in detail to help understanding of the present invention. However, the following examples are merely illustrative of the contents of the present invention, and the scope of the present invention is not limited to the following examples. The embodiments of the present invention are provided to more fully describe the present invention to those skilled in the art.

<실시예 1. 직쇄알킬술폰산의 검출><Example 1. Detection of straight-chain alkylsulfonic acid>

도 1에 개시된 바와 같이 다음의 실험을 수행하였다. The following experiment was performed as disclosed in FIG. 1.

100ppm 메틸렌블루(MB) 수용액, 농도별 직쇄알킬술폰산 수용액(LABS 수용액 : 0, 0.2, 0.5, 1, 5, 10, 20, 50, 100 ppm)을 제조하였다. A 100 ppm methylene blue (MB) aqueous solution and a straight chain alkylsulfonic acid aqueous solution by concentration (LABS aqueous solution: 0, 0.2, 0.5, 1, 5, 10, 20, 50, 100 ppm) were prepared.

15㎖ conical tube에 10㎎의 C-18 실리카 분말(C-18 reverse phase silica powder)을 넣고, 다음으로, 1㎖ 메틸렌블루 수용액 및 농도별 직쇄알킬술폰산(LABS) 수용액을 1㎖씩 넣고 혼합하여 C-18 실리카 분말을 염색시켰다. 최종부피가 15㎖가 되도록 물을 더 넣어주고 다시 잘 혼합한 후 감암여과 장치를 설치하고 conical tube의 내용물을 여과하였다. 거름종이를 건조시킨 후 powder의 색을 확인하였다. Add 10mg of C-18 silica powder (C-18 reverse phase silica powder) to a 15ml conical tube, and then add 1 ml of 1 ml of methylene blue aqueous solution and 1 ml of linear alkylsulfonic acid (LABS) aqueous solution by concentration and mix. The C-18 silica powder was dyed. Add more water so that the final volume was 15 ml, mix well again, install a dark filter, and filter the contents of the conical tube. After drying the filter paper, the color of the powder was confirmed.

그 결과, 도 2와 같이 직쇄알킬술폰산 (LABS)의 농도가 0, 0.2, 0.5, 1, 5, 10, 20, 50, 100 ppm 일 때 얻은 C-18 실리카 powder의 색상을 확인할 수 있었고, 직쇄알킬술폰산 (LABS)의 농도가 0.5 ppm 이상인 경우부터 육안으로 식별되는 파란색이 보이기 시작하였다. As a result, the color of the C-18 silica powder obtained when the concentration of the straight chain alkyl sulfonic acid (LABS) was 0, 0.2, 0.5, 1, 5, 10, 20, 50, 100 ppm, as shown in FIG. 2, was confirmed. When the concentration of the alkylsulfonic acid (LABS) was 0.5 ppm or more, a blue color visually recognized began to appear.

따라서 이와 같은 방법을 적어도 0.5ppm의 직쇄알킬술폰산의 존재 유무를 용이하게 검출할 수 있음이 확인된다. Therefore, it is confirmed that such a method can easily detect the presence or absence of at least 0.5 ppm of straight-chain alkylsulfonic acid.

<실시예 2. 메틸렌블루 수용액의 적정 농도 확인> <Example 2. Confirmation of the appropriate concentration of methylene blue aqueous solution>

직쇄알킬술폰산을 검출하기에 적절한 메틸렌블루 수용액의 적정 농도를 확인하기 위해 실시예 1과 동일한 방법으로 실험하되 다음의 표 1 조건으로 하여 0.5pp m과 0.2ppm의 직쇄알킬술폰산이 검출가능한지 확인하였다(혼합비는 동일함).In order to confirm the appropriate concentration of the methylene blue aqueous solution suitable for detecting a straight-chain alkylsulfonic acid, the experiment was conducted in the same manner as in Example 1, but it was confirmed whether 0.5-ppm and 0.2-ppm straight-chain alkylsulfonic acid was detectable under the following Table 1 conditions ( The mixing ratio is the same).

조건Condition 메틸렌블루 수용액
(1 ㎖)Methylene blue aqueous solution
(1 ml) 0.5 ppm LABS
검출 여부 0.5 ppm LABS
Detection 0.2 ppm LABS
검출 여부 0.2 ppm LABS
Detection 실시예 1Example 1 100 ppm100 ppm 검출detection 확인되지 않음Not confirmed 실시예 2-1Example 2-1 80 ppm80 ppm 검출detection 확인되지 않음Not confirmed 실시예 2-2Example 2-2 120 ppm120 ppm 검출detection 확인되지 않음Not confirmed 실시예 2-3Example 2-3 200 ppm200 ppm 검출detection 확인되지 않음Not confirmed 실시예 2-4Example 2-4 70 ppm70 ppm 확인되지 않음Not confirmed 확인되지 않음Not confirmed 실시예 2-5Example 2-5 60 ppm60 ppm 확인되지 않음Not confirmed 확인되지 않음Not confirmed

표 1의 결과를 참고하여, 메틸렌블루 수용액의 농도가 80 ppm 이상에서 최소 0.5ppm과 같은 낮은 농도의 직쇄알킬술폰산을 검출할 수 있었고, 그 이상의 농도이더라도 더 낮은 농도의 직쇄알킬술폰산의 검출이 더 되지는 않았다. 따라서 비용 면에서 고농도의 메틸렌블루의 사용을 할 필요 없이 적절하게 80~120 ppm 선에서 직쇄알킬술폰산을 검출할 수 있는 것으로 파악된다. Referring to the results in Table 1, the concentration of the methylene blue aqueous solution was able to detect a low concentration of straight-chain alkylsulfonic acid at a concentration of 80 ppm or more, such as at least 0.5 ppm, and even at a concentration higher than that, the detection of a lower concentration of straight-chain alkylsulfonic acid was more It didn't work. Therefore, it is understood that a straight-chain alkylsulfonic acid can be appropriately detected at 80 to 120 ppm without the need to use a high concentration of methylene blue in terms of cost.

<실시예 3. 메틸렌블루 수용액, 소수성 실리카 및 직쇄알킬술폰산 수용액의 적정 혼합비 확인> <Example 3. Confirmation of proper mixing ratio of methylene blue aqueous solution, hydrophobic silica and straight chain alkylsulfonic acid aqueous solution>

실시예 1과 동일한 방법으로 0, 0.2, 0.5, 1, 5, 10, 20, 50, 100 ppm의 직쇄알킬술폰산 검출과정을 수행하되, 메틸렌블루 수용액과 소수성 실리카의 혼합비와 소수성 실리카의 종류 등을 다음 표 2 및 표 3과 같이 달리하였다(메틸렌블루 수용액의 농도는 동일함). In the same manner as in Example 1, 0, 0.2, 0.5, 1, 5, 10, 20, 50, 100 ppm of a straight chain alkylsulfonic acid detection process was performed, but the mixing ratio of the aqueous solution of methylene blue and hydrophobic silica, the type of hydrophobic silica, etc. It was changed as shown in Table 2 and Table 3 (the concentration of the methylene blue aqueous solution was the same).

조건Condition 메틸렌블루 수용액
(100 ppm)Methylene blue aqueous solution
(100 ppm) C-18 실리카 분말C-18 silica powder LABS
각 농도별 용액LABS
Solutions for each concentration LABS 검출 여부LABS detection 0.2 ppm 0.2 ppm 0.5 ppm 0.5 ppm 5 ppm5 ppm 10 ppm10 ppm 50 ppm50 ppm 100 ppm100 ppm 정량분석 가능여부Whether quantitative analysis is possible 실시예 1Example 1 1 ㎖1 ml 10 ㎎10 mg 1 ㎖1 ml 확인되지 않음Not confirmed 검출detection 검출detection 검출detection 검출detection 검출detection 가능possible 실시예 3-1Example 3-1 1 ㎖1 ml 8 ㎎ 8 mg 1 ㎖1 ml 확인되지 않음Not confirmed 검출detection 검출detection 검출detection 검출detection 검출detection 가능possible 실시예 3-2Example 3-2 1 ㎖1 ml 12 ㎎12 mg 1 ㎖1 ml 확인되지 않음Not confirmed 검출detection 검출detection 검출detection 검출detection 검출detection 가능possible 실시예 3-3Example 3-3 1 ㎖1 ml 10 ㎎10 mg 2 ㎖2 ml 확인되지 않음Not confirmed 검출detection 검출detection 검출detection 검출detection 검출detection 가능possible 실시예 3-4Example 3-4 1 ㎖1 ml 10 ㎎10 mg 0.5 ㎖0.5 ml 확인되지 않음Not confirmed 검출detection 검출detection 검출detection 검출detection 검출detection 가능possible 실시예 3-5Example 3-5 1 ㎖1 ml 10 ㎎10 mg 0.3 ㎖0.3 ml 확인되지 않음Not confirmed 확인되지 않음Not confirmed 확인되지 않음Not confirmed 검출detection 검출detection 검출detection 농도별 색상 구분이 잘 안 되어 불가능Impossible to distinguish color by density 실시예 3-6Example 3-6 1 ㎖1 ml 20 ㎎20 mg 1 ㎖1 ml 확인되지 않음Not confirmed 확인되지 않음Not confirmed 확인되지 않음Not confirmed 검출detection 검출detection 검출detection 농도별 색상 구분이 잘 안 되어 불가능Impossible to distinguish color by density 실시예 3-7Example 3-7 1 ㎖1 ml 6 ㎎6 mg 1 ㎖1 ml 확인되지 않음Not confirmed 검출detection 검출detection 검출detection 검출detection 검출detection 농도별 색상 구분이 잘 안 되어 불가능Impossible to distinguish color by density

조건Condition 소수성 실리카 분말 종류Types of hydrophobic silica powder LABS 검출 여부LABS detection 0.5 ppm0.5 ppm 5 ppm5 ppm 100 ppm100 ppm 1000 ppm1000 ppm 실시예 1Example 1 C-18 C-18 검출detection 검출detection 검출detection 검출detection 실시예 3-8Example 3-8 C-8 C-8 확인되지 않음Not confirmed 확인되지 않음Not confirmed 확인되지 않음Not confirmed 확인되지 않음Not confirmed 실시예 3-9Example 3-9 C-12C-12 확인되지 않음Not confirmed 확인되지 않음Not confirmed 확인되지 않음Not confirmed 검출detection

그 결과, 표 2 및 표 3을 참고할 때, 메틸린블루 수용액 1 ㎖당 C-18 실리카 분말이 8~12 ㎎, LABS 각 농도별 용액(또는 세척액)이 0.5~2 ㎖ 첨가되는 것이 좋고, LABS 잔류량의 정량적 평가 또한 할 수 있었다. 또한 C-18 실리카 대신 C-12 또는 C-8 실리카를 사용하는 것에서는 LABS 검출이 잘 되지 않았다.As a result, when referring to Table 2 and Table 3, it is preferable that 8 to 12 mg of C-18 silica powder per ml of aqueous methylline blue solution, and 0.5 to 2 ml of solution (or washing solution) for each concentration of LABS be added, LABS Quantitative evaluation of the residual amount could also be made. In addition, the detection of LABS was poor in the use of C-12 or C-8 silica instead of C-18 silica.

Claims (10)

삭제delete 삭제delete 삭제delete (제1단계) 메틸렌블루(Methylene blue) 수용액, 소수성 실리카 분말로서 옥타데실실란(C-18)이 코팅된 실리카 분말 및 물을 준비하는 단계;
(제2단계) 상기 소수성 실리카 분말과 메틸렌블루 수용액 및 직쇄알킬술폰산(Linear alkyl benzene sulfonate)의 잔류상태를 확인하고자 하는 세척액을 혼합하여 혼합 액상을 제조하고, 물을 더 첨가하여 혼합한 후 여과하여 소수성 실리카 반응물을 얻는 단계; 및,
(제3단계) 제2단계에서 여과하여 얻은 소수성 실리카 반응물을 건조하여 분말의 색상을 확인하는 단계;를 포함하는 메틸렌블루 및 소수성 실리카를 이용하는 것을 특징으로 하는 직쇄알킬술폰산(Linear alkyl benzene sulfonate; LABS)의 미량 검출 방법. (First step) preparing an aqueous solution of methylene blue, silica powder coated with octadecylsilane (C-18) as hydrophobic silica powder, and water;
(Second step) A mixed liquid was prepared by mixing the hydrophobic silica powder with a methylene blue aqueous solution and a washing liquid to check the residual state of linear alkyl benzene sulfonate, and then adding more water to mix and filtering. Obtaining a hydrophobic silica reactant; And,
(Step 3) drying the hydrophobic silica reactant obtained by filtering in the second step to check the color of the powder; Linear alkyl benzene sulfonate, characterized by using methylene blue and hydrophobic silica ) Trace amount detection method. 삭제delete 제4항에 있어서,
상기 제2단계에서 소수성 실리카 반응물의 여과는 거름종이, 천 또는 부직포를 이용하며, 감압여과법으로 여과하는 것을 특징으로 하는 직쇄알킬술폰산의 미량 검출 방법. According to claim 4,
In the second step, the filtering of the hydrophobic silica reactant uses filter paper, cloth or non-woven fabric, and the trace detection method of the straight-chain alkyl sulfonic acid is characterized in that it is filtered by a vacuum filtration method. 제4항에 있어서,
상기 제2단계에서 세척액은 과일, 채소 또는 식기의 세척액인 것을 특징으로 하는 직쇄알킬술폰산의 미량 검출 방법. According to claim 4,
In the second step, the washing liquid is a method for detecting a trace amount of a straight-chain alkylsulfonic acid, characterized in that it is a washing liquid of fruits, vegetables or dishes. 제4항에 있어서,
상기 제3단계에서 소수성 실리카 반응물을 건조하는 과정은 20~35℃에서 수행되는 것을 특징으로 하는 직쇄알킬술폰산의 미량 검출 방법. According to claim 4,
The process of drying the hydrophobic silica reactant in the third step is a trace detection method of a straight-chain alkyl sulfonic acid, characterized in that performed at 20 ~ 35 ℃. 제4항에 있어서,
상기 제3단계에서 혼합액상에 직쇄알킬술폰산 표준 용액이 첨가된 표준시료군이 준비되는 것을 특징으로 하는 직쇄알킬술폰산의 미량 검출 방법. According to claim 4,
A method of detecting a trace amount of a straight-chain alkylsulfonic acid, wherein a standard sample group in which a standard solution of a straight-chain alkylsulfonic acid is added to the mixed solution in the third step is prepared. 삭제delete
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