The chemical speciation and analysis of trace elements in sediment with neutron activation analytical method(NAA) and atomic mass spectrometry

중성자 방사화분석법과 원자질량분석법을 이용한 침전물 시료속에 존재하는 미량원소들의 화학종 분류 및 분석

  • Received : 2003.07.25
  • Accepted : 2003.08.08
  • Published : 2003.10.25

Abstract

In this research, first of all, the analytical methods for the determination of major elements in sediment have been developed with ICP-MS (Inductively Coupled Plasma Mass Spectrometry). The analytical results of major elements (Al, Ca, K, Fe, Mg) with Cool ICP-MS were much better than those with normal ICP-MS. The analytical results were compared with those of NAA (Neutron Activation Analysis). NAA were a little superior to ICP-MS for the determination of major elements in sediment as a non-destructive trace analytical method. The analytical methods for the determination of minor elements (Cr, Ce, U, Co, Pb, As, Se) have been also developed with ICP-MS. The analytical results by standard calibration curve with ICP-MS were not accurate due to the matrix interferences. Thus, the internal standard method was applied, then the analytical results for minor elements with ICP-MS were greatly improved. The analytical results obtained by ICP-MS were compared with those obtained by NAA. It showed that the two analytical methods have great capabilities for the determination of minor elements in sediments. Accordingly, the NAA will play an important role in analysis of environment sample with complex matrix. ICP-MS also will play an important role because it has a great capability for the determination of Pb that could not be determined by NAA.

이 연구는 먼저 침전물 속에 major 원소 (Al, Ca, K, Fe, Mg)를 측정하기위해 ICP-MS를 이용하여 분석방법을 개발하였다. Cool ICP-MS로 major원소를 분석한 결과 Normal ICP-MS보다 더 좋은 분석 결과를 얻었다. 또한 그 결과를 NAA의한 분석 결과와 비교해 보았다. NAA는 고체시료의 비파괴 미량분석법이며 침전물 속에 major원소들에 대한 측정 결과는 ICP-MS보다 더 좋은 결과를 얻었다. 또한 침전물 속에 minor 원소 (Cr, Ce, U, Co, Pb, As, Se)를 측정하기 위해 ICP-MS를 이용하여 분석방법을 개발하였다. 표준 검정곡선으로 분석한 결과 모체방해효과 때문에 정확도가 좋지 않았다. 그래서 ICP-MS를 이용하여 내부표준물법으로 minor 원소들을 분석했을 때 결과값이 향상됨을 알 수 있었다. 그 결과를 NAA분석법과 비교해도 ICP-MS를 이용한 방법이 더 좋은 결과였음을 알 수 있었다. 두 가지의 분석방법은 침전물 속에 존재하는 minor 원소를 충분히 측정할 수 있다. 그러므로 NAA 분석법이 모체가 복잡한 환경시료를 분석하는데 중요한 역할을 하며, ICP-MS 또한 NAA 분석법으로는 분석 할 수 없는 납을 검출할 수 있기 때문에 환경시료를 분석하는데 두 분석법은 상호 보완할 수 있는 중요한 분석법이다.

Keywords

References

  1. A. L. Gray, Analyst, 100, 289-299 (1975)
  2. R. S. Houk, V. A. Fassel, G. D. Flesch, H. J. Svec, A. L. Gray, C. E Taylor, Anal. Chem. 52, 2283(1980)
  3. K. E. Jarvis, A. L Gray, R. S. Houk, 'Handbook of Inductively Coupled Plasma Mass Spectrometry', Chapman and Hall, New York, 1992
  4. Akbar Montaser and D. W. Golightly, 'Inductively Coupled Plasmas in Analytical atomic Spectrometry', Second Edition
  5. T. Gasparics, I. Csato, and Gy. Zaray, 'Analysis of Antarctic Marine Sediment by Inductively Coupled Plasma Atomic Emission And Total Reflection X-Ray Fluorescence Spectrometry', J. Microchem., 55, 56, 63 (1997)
  6. H. M. Kingston, J. B. Jassie, 'Introduction to microwave Sample Preparation Theory and Practice', American Chemical Soc., Washington, DC, 1988
  7. P. J. Lamothe, T. L. Fries, J. Consul, J. Anal. Chem., 58, 1881(1986)
  8. R. A. Nadkami, Anal. Chem., 56, 2233 (1984)
  9. M. Thompson, J. N. walsh, 'A Handbook of Inductively Couple Plasma Atomic Spectrometry', Chapman & Hall, New York, 1983
  10. J. B. Worthington, H. L. Pardue, Anal. Chem, 42, 1157 (1970)
  11. Paul Kruer, 'principles of activation analysis', Wiley-Interscience, John Wiley & Sons, 1971
  12. Z. B. Alfassi, 'Chemical analysis by nuclear method', John Wiley & Sons, 1994
  13. Y. S. Chung, Y. J. Chung, E. S. Jung and S. Y. Cho, 'Comparison and determination of environmental standard samples by instrumental neutron activation analysis', J. Radioanal. & Nucl. Chem., 217(1), 71-76 (1997)
  14. Y. S. Chung, J. H. Moon, Y. J. Chung, Y. J. Park, K. Y. Lee, Y. Y. Yoon, S. H. Lee, K. T. Kim, 'ntercomparison and Determination of Sediment by Instrumental Neutron Activation Analysis', Journal of the Korean Socirty of Groundwater Environment, 5(2), 116 (1998)
  15. IAEA, 'Handbook on nuclear activation analysis data', IAEA Tec. Rep. No. 273, 1987
  16. Michael D. Glascock, 'Table for neutron activation analysis', The University of Missouri, 4th edition, 1996
  17. 정용삼, 문종화, 김선하, 백성열, 강상훈, '중성자 방사화분석 이용기술 개발', KAERI/RR- 2356/2002, 한국원자력연구소, 2002
  18. 남상호. 김민재, 정용삼, 김선하, Analytical Science & Technology, 15(6), (2002)