LDPE 중 PFOS의 분석법 개발과 비교숙련도 결과
Determination of PFOS in LDPE and the Result for Proficiency Testing
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전기전자 부품 및 제품상에서 주로 사용되는 Plastic 중 함유된 Perfluorooctanesulfonic acid (PFOS)의 정량 분석법을개발하기 위해 LDPE 시료를 대상으로 soxhlet 용매추출과 액체크로마토그래피/질량분석법(LC/MS)을 사용하여 시험방법 유효화를 진행하였다. 그 결과 검출한계(LOD)와 정량한계(LOQ)는 각각 2.58 μg/L, 7.82μg/L였으며, 회수율은 96−102%를 나타내었다. LC/MS의 검량선은 7.82−100 μg/L 농도범위에서 r2값 0.9992의 직선성을 확인하였다. 또한 EU 환경규제 대응을 위한 전기전자 제품 중의 PFOS 분석법 표준화를 위해서 국내외 시험기관을 대상으로 비교숙련도 시험을 실시하였다. 그 결과 참여한10개 시험기관 중 3개 시험기관이 이상값을 제출하였다. 이에 19F 핵자기공명분광분석법(19F NMR)을 사용하여 이상값의 원인을 규명한 결과 그 주요 원인이 표준시약 및 시료 중에 존재하는 PFOS 이성질체들에 대한 결과처리의 오류였음을 확인하였다
Abstract
In order to develop a quantitation method for Perfluorooctanesulfonic acid(PFOS) contained in plastics that are mainly used in electric and electronic equipment, this study consisted of conducting method validations with LDPE samples using soxhlet solvent extraction and LC/MS. As a result, the limits of detection and quantitation (LOD, LOQ) were 2.58 μg/L and 7.82 μg/L, respectively. Additionally, the recovery was 96-102%. For the correlation coefficient of LC/MS, the r2 value was 0.9992 in the concentration range of 7.82-100 μg/L, which confirmed its linearity. Furthermore, for the standardization of the analysis method for PFOS in electric and electronic equipment to correspond to EU environmental regulations, we conducted a proficiency test with a number of domestic and international testing laboratories. Three of the ten testing laboratories that participated in the proficiency test submitted outliers. Accordingly, we examined the cause of the outliers using the 19F NMR, finding that the main cause was an error in the processing of the results for isomers in PFOS that existed in standard solutions and samples.
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