Analytical Science and Technology (분석과학)

The Korean Society of Analytical Sciences (한국분석과학회)
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Development of soil certified reference material for determination of the hazardous elements

유해원소 측정용 토양 인증표준물질 개발

  • Kim, In-Jung (Division of Metrology for Quality of Life, Korea Research Institute of Standards and Science) ;
  • Min, Hyung-Sik (Division of Metrology for Quality of Life, Korea Research Institute of Standards and Science) ;
  • Suh, Jung-Ki (Division of Metrology for Quality of Life, Korea Research Institute of Standards and Science) ;
  • Han, Myung-Sub (Division of Metrology for Quality of Life, Korea Research Institute of Standards and Science) ;
  • Lim, Myung-Chul (Division of Metrology for Quality of Life, Korea Research Institute of Standards and Science) ;
  • Kim, Young-Hee (Environmental Measurement Standards Department, Korea Institute for Environmental Research) ;
  • Shin, Sun-Kyoung (Environmental Measurement Standards Department, Korea Institute for Environmental Research) ;
  • Cho, Kyung-Haeng (Division of Metrology for Quality of Life, Korea Research Institute of Standards and Science)
  • 김인중 (한국표준과학연구원 삶의질측정표준본부) ;
  • 민형식 (한국표준과학연구원 삶의질측정표준본부) ;
  • 서정기 (한국표준과학연구원 삶의질측정표준본부) ;
  • 한명섭 (한국표준과학연구원 삶의질측정표준본부) ;
  • 임명철 (한국표준과학연구원 삶의질측정표준본부) ;
  • 김영희 (국립환경과학원 환경측정기준부) ;
  • 신선경 (국립환경과학원 환경측정기준부) ;
  • 조경행 (한국표준과학연구원 삶의질측정표준본부)
  • Received : 2010.06.14
  • Accepted : 2010.10.18
  • Published : 2010.10.25
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Abstract

A certified reference material (CRM) of KRISS 109-03-SSD was developed for the analysis of hazardous elements in soil. The target elements were As, Cd, Cr, Cu, Hg, Ni, Pb, Zn being regulated by the Soil Environment Conservation Act. Starting material was collected from tailing dump of an unworked tungsten mine at Sangdong (Gangwon-do, Korea). The starting material under-went through a series of fabricating process steps of screening, drying, grinding, sieving, blending, bottling, sterilization and was certified according to the ISO Guide 35. Isotope dilution-inductively coupled mass spectrometry (ID-ICP/MS) and instrumental neutron activation analysis (INAA) were used for the measurement. Homogeneity was tested according to ISO 13528 annex B. The certified values were determined using the results from two different methods or from two independent measurements using a method. Finally, certified values of seven elements of arsenic, cadmium, chromium, copper, lead, nickel and zinc were determined. Mercury did not satisfied the criteria of homogeneity and the result would be provided for information only, together with iron and tungsten. It was also studied, the extractable fraction of elements by aqua regia according to the ISO 11466 protocol being frequently studied for the purpose of environmental monitoring. It was performed as a inter-laboratory study by 6 laboratories of a public institute and universities. Standard deviation among the laboratories was much bigger than the uncertainty of the certified value. The result of inter-laboratory study on the extractable fraction will be provided for information, only.

토양 중 유해원소 분석용 인증표준물질 KRISS CRM 109-03-SSD를 개발하였다. 인증 대상 원소는 현행 토양환경보전법에서 규제하고 있는 비소, 카드뮴, 크로뮴, 구리, 수은, 니켈, 납, 아연이다. 인증표준물질 제조를 위한 출발물질은 강원도 상동의 텅그스텐 폐광 광미 더미에서 채취하였다. 출발물질은 선별, 건조, 분쇄, 체거름, 혼합, 병입, 살균의 일련의 과정을 거쳐 제조한 다음 ISO Guide 35의 절차를 준용하여 인증하였다. 측정에는 동위원소희석 질량분석법(ID-ICP/MS) 및 기기중성자방사화분석법(INAA)을 이용하였다. 균질도 평가는 ISO 13528의 부속서 B를 준용하여 실시하였다. 인증값은 서로 다른 두 가지 측정방법에 의한 분석 결과 또는 동일한 방법이지만 독립적으로 2회 반복 시행된 분석의 결과로부터 결정하였다. 최종으로 비소, 카드뮴, 크로뮴, 구리, 납, 니켈, 아연 7개 원소에 대한 인증값을 결정하였다. 수은은 낮은 농도로 인해 균질도 요건을 만족시키지 못해 철, 텅그스텐과 함께 참고값으로 제공된다. 환경감시목적으로 많이 이용되는 ISO 11466에 따른 왕수에 의한 용출시험 또한 실시하였다. 용출시험은 공립시험소 및 대학 시험소 등 6개 기관의 공동분석으로 수행되었다. 용출시험의 실험실간 편차는 인증값의 불확도에 비해 크게 나타났다. 용출시험에 대한 공동분석 결과는 참고값으로 제공된다.

Keywords

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