초록
수용액 내에서 환원제인 sulfurous acid와 휘발성이 강한 Os(III)을 반응시킨 후 생성된 비휘발성 Os(IV)을 inductively coupled plasma atomic emission spectrometry (ICP-AES)로 분석하였다. pH 2-10의 수용액에서 sulfurous acid와 Os(VIII)의 정량적 반응에 의하여 생성된 Os(VI)을 ICP-AES로 분석하였다. 동축형 분무기(concentric type nebulizer)에 의한 시료 도입 방법에서 sulfurous acid와 osmium은 반응 직후부터 안정한 신호를 나타내었으며 다양한 ICP-AES 조건에서 3회 반복 측정했을 때 재현성은 0.5-4.5%였으며, 검출 한계는 2.5-57.7 ng/g이었다.
In this study, a convenient, fast and accurate inductively coupled plasma atomic emission spectrometry (ICP-AES) method has been optimized for the determination of osmium in aqueous solutions. The method makes use of the reaction of sulfurous acid with osmium to quantitative conversion of volatile Os(VIII) to non-volatile Os(IV) in the pH range 2-10. The response was found to be stabilized immediately after sulfurous acid reacted with osmium. The precision was calculated to be 0.5-4.5 % (RSD) under various ICP-AES conditions. The detection limit was 2.5-57.7 ng/g based on $3{\sigma}$ of the blank response (n=3) using a concentric flow nebulization.