National Centre for Compositional Characterisation of Materials (CCCM), B. A. R. C., E.C.I.L. (P.O.), Hyderabad 500062, India.
Anal Chim Acta. 2010 Feb 19;661(1):17-9. doi: 10.1016/j.aca.2009.12.010. Epub 2009 Dec 21.
A dry ashing procedure is developed for the determination of As in organic rich matrices such as wheat flour, lichen and tobacco leaves. The volatility of As during dry ashing is avoided by the addition of palladium nitrate [Pd(NO(3))(2)]. The recovery of both As(III) and As(V) is found to be near quantitative. The residue after dry ashing is dissolved in nitric acid (HNO(3)) and analysed by inductively coupled plasma-mass spectrometry (ICP-MS). The process blank and limit of detection (LOD) are 11 and 6.6 ng g(-1), respectively. The procedure is applied for the determination of As in certified reference materials namely wheat flour NIST SRM 1567a (National Institute of Standards and Technology Standard Reference Material), lichen BCR CRM 482 (Institute for Reference Materials, European Commission) and Virginia tobacco leaves CTA-VTL-2 (Poland Academy of Sciences). The results obtained by the present procedure are in good agreement with the certified values and also determined after complete dissolution of samples using closed microwave digestion.
开发了一种干灰化程序,用于测定富有机基质如面粉、地衣和烟叶中的砷。通过添加硝酸钯[Pd(NO(3))(2)]避免了砷在干灰化过程中的挥发。发现砷(III)和砷(V)的回收率接近定量。干灰化后的残渣用硝酸(HNO(3))溶解,并用电感耦合等离子体质谱法(ICP-MS)分析。该过程的空白和检测限(LOD)分别为 11 和 6.6 ng g(-1)。该程序用于测定经认证的参考材料中的砷,即美国国家标准与技术研究院标准参考物质(NIST)面粉 NIST SRM 1567a(美国国家标准与技术研究院标准参考物质)、地衣 BCR CRM 482(欧盟委员会参考材料研究所)和波兰科学院弗吉尼亚烟叶 CTA-VTL-2。本程序得到的结果与认证值吻合良好,也与使用密闭微波消解完全溶解样品后得到的结果一致。