Rapid determination of multi-elements in geochemical samples by microwave acid digestion ICP-AES

被引:5
作者
Minakawa, M
Uematsu, M
机构
[1] Univ Tokyo, Ocean Res Inst, Nakano Ku, Tokyo 1648639, Japan
[2] Japan Sci & Technol Corp, Kawaguchi, Saitama 3320012, Japan
关键词
microwave; acid digestion; ICP-AES; multi-elements; soil; aerosols and marine sediment;
D O I
10.2116/bunsekikagaku.50.273
中图分类号
O65 [分析化学];
学科分类号
070302 ; 081704 ;
摘要
A method involving chemical decomposition and analysis using microwave acid digestion and inductively coupled plasma atomic emission spectrometry (ICP-AES) is proposed for the rapid determination of multi-elements in geochemical samples. Samples of less than 0.3 g were placed in a Teflon pressure vessel, to which 3 mi each of HNO3 and HClO4 were added. The vessel was sealed and irradiated under stepwise stages: 1 min at 250 W, 1 min at 0 W, 5 min at 250 W, 5 min at 400 W and 10 min at 650 W. The vessel was cooled fbr 30 min in a water bath. The vessel was carefully opened and 4 mi of HF was added. Irradiation was repeated once again under another set of stepwise stages: 1 min at 250 W, 1 min at 0 W, 5 min at 250 W, 5 min at 400 W, 10 min at 650 W and 30 min at 500 W. After cooling, the acid solution was evaporated down to several mi using an acid recovery module, and then to drl ness in a Teflon dish. The residue was dissolved in 1.25 mi of 12 M HCl rind diluted with pure water in a 25 mi Teflon volumetric flask. The entire procedure took less than ii hours, including 2.5 to 4.0 hours digestion. Thirty elements in soil, aerosols and marine sediment were determined by; ICP-XES. The analytical results were in good agreement with reference values for the sample material.
引用
收藏
页码:273 / 279
页数:7
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