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Journal of the Korean Chemical Society (JKCS)

ISSN 1017-2548(Print)
ISSN 2234-8530(Online)
Volume 55, Number 3
JKCSEZ 55(3)
June 20, 2011 

 
Title
Analysis of Selenium in Grain with ORC Collision-Removal of Br Interference using Mathematical Calibration

ORC ICPMS에서의 곡류중의 셀레늄 분석-수학적 보정을 이용한 Br의 간섭제거
Author
Heon Hong Cho, Yong Nam Pak*

조헌홍, 박용남*
Keywords
셀렌, 팔중극자 ICPMS, 동위원소 희석법, 수학적 보정, 곡물, 브롬의 간섭제거 , Selenium, ORC ICPMS, Isotope dilution, Mathematical correction, grain, Br interference
Abstract
팔중극자 반응셀 유도결합플라즈마 질량분석법(ORC ICPMS; Octapole Reaction Cell Inductively Coupled Plasma Mass Spectrometry)에서 동위원소 희석법을 이용하여 곡류 중의 셀레늄을 정확히 분석하였다. 충돌기체는 헬륨보다 수소 가 더 효율적이었고 최적 흐름속도는 4.0 mL min-1 이었다. ORC는 다원소 이온화학종들의 간섭을 충분히 제거하였으나 시료매트릭스에 브롬이 존재하는 경우, 충돌기체인 H2에 의해 BrH+가 생성되어 m/z 80, 82에 방해를 주었다. 브롬의 화 학적 제거는 매우 어려웠으며 82Se의 신호세기에 대한 수학적 보정을 사용하고 동위원소 희석법을 적용하였다. 정확도를 검증하기 위하여 표준검정 물질(NIST SRM 1566, 1567)을 분석한 결과, 좋은 일치도를 얻었고, 이를 바탕으로 실제시료인 곡류 중의 셀레늄을 분석하여 계산한 결과, 백미 0.034±0.001 μg g-1, 현미 0.059±0.0025 μg g-1, 흑미 0.029±0.0014 μg g-1 그리고 보리 0.034±0.002 μg g-1를 얻었다. 셀레늄 분석에 대한 검출한계(3σ)는 0.012 ng g-1 이었다.

The concentration of selenium in grain samples was determined using isotope dilution method in ORC-ICPMS. The experimental conditions were optimized to H2 mode and the flow rate was 4.0 mL min-1. ORC in H2 mode proved to eliminate most of polyatomic interferences except BrH+ when Br is present in sample matrix. Chemical removal of Br was very difficult and the mathematical correction was successfully employed. The fraction of BrH+ generated from Br at the current experimental condition was 14.1%. The signal on m/z 82 was corrected and calculated for isotope dilution. The analytical reliability of the propose method was successfully evaluated by analyzing the certified standard reference material NIST SRM 1566 and 1567. The method was applied to real samples and the results are 0.034±0.001 μg g-1 for white rice, 0.059±0.0025 μg g-1 for brown rice, 0.029±0.0014 μg g-1 for black rice, and 0.034±0.002 μg g-1 for barley. The detection limits (3σ) for Se was 0.012 ng g-1.

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