공산품 함유 PAHs 분석법에 관한 연구
Study on analysis of PAHs in consumer products
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발암성 및 잔류성을 갖는 다환방향족탄화수소(Polycyclic aromatic hydrocarbons, 이하 PAHs)의법적인 규제가 공산품 함유에로 확장된 현황에서, 본 연구에서는 속슬렛 추출에 의한 전처리 및 GC-MS분석에 의한 공산품에 함유된 18종 PAHs의 정량 분석법을 확립하고 공산품 4종에서의 18종 PAHs 함유 여부를 분석하였다. GC-MS SIM 크로마토그램의 머무름 시간 및 피크 면적의 정밀도는 각 0.00%~0.05%및 1.16%~3.69%의 RSD로 측정되었고 각 PAH의 농도 범위 0.3125 mg/L~5.00 mg/L에서 얻은 검정곡선은 상관계수 R2값이 18종 모두 0.999 이상으로 산출되었다. 본 검정곡선을 이용한 18 종 PAHs의 GCMS기기분석의 정량 한계는 0.327 mg/L (Benzo[ghi]perylene)~0.464 mg/L (Acenaphthylene)로 산출되었다. 스파이킹에 의한 18종 PAHs의 속슬렛 추출에 의한 회수율은 DCM, 헥세인, 혹은 톨루엔 사용 시 모두95%~105%로 측정되었고, 이상의 조건에서 국내에서 유통되는 공산품 4종에서 18종 PAHs를 분석한 결과, 3개 시료에서는 Phenanthrene이 정량한계 근방의 소량으로 검출되었고, 망치(손잡이 부분) 시료에서는 Phenanthrene을 비롯한 15종 PAHs가 최대 83.4 mg/kg~최소 8.5 mg/kg 범위로 검출되었다.
Abstract
Polycyclic aromatic hydrocarbons (PAHs) that are carcinogenic and persistent will be restricted inconsumer products from December 27, 2015 by EU REACH regulation. Pretreatment using Soxhlet extractionand quantitative analysis by GC-MS were studied to develop the method for analyzing 18 PAHs in consumerproducts as well as to detect the amounts and the kinds of PAHs in consumer products such as grips of abag and a hammer, a cable and a plastic sandal. Linearity and precisions were evaluated by analyses of thestandard PAH solutions ranging from 0.3125 mg/L to 5.00 mg of each of 18 PAHs. Linearity of resulting standardcurves for all 18 PAHs were obtained with R2 above 0.999. Precisions of the retention times and the peakareas were found to be 0.00%~0.05% and 1.16%~3.69% of relative standard deviations, respectively. Therecoveries for spiked samples were all around 95%~105% after Soxhlet extration using three different solventssuch as dichloromethane, hexane and toluene. The limits of quantitation for 18 PAHs in solutions and polymersamples by GC-MS were evaluated to be 0.327 mg/L (Benzo[ghi]perylene)~0.464 mg/L (Acenaphthylene) and1.635 mg/kg (Benzo[ghi]perylene)~2.32 mg/kg (Acenaphthylene) based upon dilution factor of 5, respectively. Under the developed analytical method, only trace amounts of phenanthrene were detected in three sampleswhile 15 kinds of PAHs including phenanthrene were detected in a grip of hammer with concentrations ofmaximum 83.4 mg/kg of Phenanthrene and minimum 8.5 mg/kg of Acenaphthylene. Further studies are neededto decrease the quantitation limit and to check the feasibility of decreasing Soxhlet time as well as to demonstratecases that the clean up is required.
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