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퇴적물 중 다환방향족탄화수소의 실험실간 비교시험에 관한 연구

Interlaboratory Comparison Study on Polycyclic Aromatic Hydrocarbons in Sediment

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초록

The purpose of this study was to establish national standard method of polycyclic aromatic hydrocarbons (PAHs) in sediment. The samples were extracted using Soxhlet extraction or accelerated solvent extraction (ASE) and injected with benzo[e]pyrene-d12 as a surrogate internal standard. Napthalene-d8, acenaphthene-d10, phenanthrene-d10, chrysene-d12, Benzo(a)pyrene-d12, Indeno(1,2,3-c,d)pyrene-d12 were used as internal cleanup standards. P-terphenyl-d14 was injected as a recovery internal standard and analyzed using gas chromatograph-mass spectrometer (GC-MS). An interlaboratory comparison study was conducted, in which the three selected participating laboratories quantitatively analyzed several PAHs in certified sediment samples: IAEA-383, IAEA-417, IAEA-408, NIST-1944. Internal quality control was conducted individually. The results reported for PAHs by the three laboratories were acceptable, with a range of relative standard deviations (RSD) of 4.0-24.0% in IAEA-383(16.0 ng/g-290.0 ng/g). Results obtained for the IAEA-417 (150.0 ng/g-7,700.0 ng/g) and NIST-1944 samples (390.0 ng/g-9,700.0 ng/g) were also found acceptable with a range of RSD of 5.4-27.9% and 2.4-25.3%, respectively. Although the results of IAEA-408(3.3 ng/g-84.0 ng/g) were slightly higher than those of other RSDs, they were acceptable with a ranged of 2.5-38.7% at two of the laboratories. The limit of quantification of this method was found to be 0.003 mg/kg, and recovery rates ranged from 50.0% to 120.0%. The RSD was less than 25%, and the accuracy ranged from 60.0% to 135.0% in sediment.

Abstract

The purpose of this study was to establish national standard method of polycyclic aromatic hydrocarbons (PAHs) in sediment. The samples were extracted using Soxhlet extraction or accelerated solvent extraction (ASE) and injected with benzo[e]pyrene-d12 as a surrogate internal standard. Napthalene-d8, acenaphthene-d10, phenanthrene-d10, chrysene-d12, Benzo(a)pyrene-d12, Indeno(1,2,3-c,d)pyrene-d12 were used as internal cleanup standards. P-terphenyl-d14 was injected as a recovery internal standard and analyzed using gas chromatograph-mass spectrometer (GC-MS). An interlaboratory comparison study was conducted, in which the three selected participating laboratories quantitatively analyzed several PAHs in certified sediment samples: IAEA-383, IAEA-417, IAEA-408, NIST-1944. Internal quality control was conducted individually. The results reported for PAHs by the three laboratories were acceptable, with a range of relative standard deviations (RSD) of 4.0-24.0% in IAEA-383(16.0 ng/g-290.0 ng/g). Results obtained for the IAEA-417 (150.0 ng/g-7,700.0 ng/g) and NIST-1944 samples (390.0 ng/g-9,700.0 ng/g) were also found acceptable with a range of RSD of 5.4-27.9% and 2.4-25.3%, respectively. Although the results of IAEA-408(3.3 ng/g-84.0 ng/g) were slightly higher than those of other RSDs, they were acceptable with a ranged of 2.5-38.7% at two of the laboratories. The limit of quantification of this method was found to be 0.003 mg/kg, and recovery rates ranged from 50.0% to 120.0%. The RSD was less than 25%, and the accuracy ranged from 60.0% to 135.0% in sediment.

참고문헌 (6)

  1. 이봉민, "부산 수영강 하구역의 퇴적물과 어류에서 다환방향족탄화수소 및 폴리염화비페닐의 농도분포와 인체 위해도 평가", 환경분석과 독성보건, 21(4), pp.252~263 (2018), 한국환경분석학회
  2. 정지윤, "유류 오염지역의 수산물 중 다환방향족탄화수소류 (PAHs) 분석 및 위해평가", 분석과학, 23(2), pp.187~195 (2010), 한국분석과학회
  3. "하천 · 호소 등 퇴적물측정망 운영계획", 환경부고시 제2011-92호, ~ (2011)
  4. 김기용, "부산지역 다매체 육상환경 중 다환방향족탄화수소의 분포특성", 환경분석과 독성보건, 18(2), pp.121~130 (2015), 한국환경분석학회
  5. 허인애, "퇴적물 환경질 평가체계 구축(III)" (2013), 국 립환경과학원
  6. D. D. MacDonald, "Development and Evaluation of Consensus-Based Sediment Quality Guidelines for Freshwater Ecosystems", Arch. Environ. Contam. Toxicol, 39, pp.20~31 (2000)

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