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외부표준법을 적용한 토양시료의TXRF 정량분석 정확도 개선

Improvement of accuracy in quantitative TXRF analysis of soil sample by applying external standard method

  • 박진규 (원자력화학연구부, 한국원자력연구원) ;
  • 박난희 (원자력화학연구부, 한국원자력연구원) ;
  • 한선호 (원자력화학연구부, 한국원자력연구원) ;
  • 임상호 (원자력화학연구부, 한국원자력연구원) ;
  • 이치규 (원자력화학연구부, 한국원자력연구원) ;
  • 송규석 (원자력화학연구부, 한국원자력연구원)
  • Park, Jinkyu (Nuclear Chemistry Research Division, Korea Atomic Energy Research Institute) ;
  • Park, Ranhee (Nuclear Chemistry Research Division, Korea Atomic Energy Research Institute) ;
  • Han, Sun Ho (Nuclear Chemistry Research Division, Korea Atomic Energy Research Institute) ;
  • Lim, Sang Ho (Nuclear Chemistry Research Division, Korea Atomic Energy Research Institute) ;
  • Lee, Chi Gyu (Nuclear Chemistry Research Division, Korea Atomic Energy Research Institute) ;
  • Song, Kyuseok (Nuclear Chemistry Research Division, Korea Atomic Energy Research Institute)
  • 투고 : 2016.05.30
  • 심사 : 2016.11.04
  • 발행 : 2016.12.25

초록

TXRF는 시료전처리 없이 분말상 시료의 정량분석이 가능하여 토양시료를 효율적으로 분석할 수 있다. 기존의 내부표준법을 이용한 분석법은 매질 효과 및 형광신호의 겹침으로 인한 간섭 효과로 인해 정확도가 떨어진다. 이를 개선하기 위해 외부표준법을 적용하여 용액화한 토양시료와 분말상 토양시료를 분석하였다. 용액화한 토양시료의 경우 개별표준물질로 만든 표준용액으로 작성한 검량선으로 분석하였는데, 내부 및 외부표준법 간 유의미한 차이가 없었다. 반면 분말상 토양시료로 부유용액을 만들어 검량선을 작성한 후 이를 이용하여 분말상 토양시료를 분석한 결과, 전반적으로 외부표준법을 적용한 결과가 내부표준법의 그것에 비해 정확도가 높았다. 두 가지 표준토양시료로 교차검증한 결과, Al, Fe, K, Ca, Ti, Ba, Mn, Sr, Rb, Cu 등 10개의 원소들에 대해 ${\pm}20%$ 내외의 상대오차가 측정되었다.

TXRF is a powerful technique for the soil sample analysis due to its ability to conduct quantitative analysis of powder sample without complicated pre-treatment processes. The conventional internal standard method used for this technique suffers from relatively low accuracy because of varying matrix effects of soil. In order to improve the accuracy, external standard method was applied to analyze two types of soil samples; acid-dissolutionized soil solution and detergent-suspended soil powder. Individual ICP-AES/MS grade standards were mixed, diluted and measured to create standard curves, but applying these curves for analyzing the soil solution sample did not make any improvement in comparison with the internal standard method. On the other hand, standard curves were created with using standard soil powders for the analysis of soil powder samples, and we found that this method increased the accuracy significantly relative to the internal standard method. Especially, Al, Fe, K, Ca, Ti, Ba, Mn, Sr, Rb, Cu was measured with relatively high accuracy (relative error = ${\pm}20%$).

키워드

참고문헌

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