水素化物原子吸光法による大気粉じん中のアンチモンの定量

概要

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Antimony in ambient particulates was digested with HF/HNO_3/H_2SO_4/KMnO_4, and determined by hydride generation atomic absorption spectrometry. The recommended procedure is as follows : 0.05〜0.1 g of particulate sample, 15 ml of nitric acid, 1 ml of sulfuric acid, 10ml of 46% hydrofluoric acid and 2 ml of 2% potassium permanganate solution were taken in a teflon beaker and heated for 1 h on a hot plate at 250℃. Then the solution was evaporated to nearly dryness. After cooling, the residue was dissolved with 20 ml of 6 M hydrochloric acid, and the solution was diluted to 50 ml with water. Twenty milliliter of this solution (containing less than 0.3μg of antimony) was transfered to a reaction vessel, then 4 ml of hydrochloric acid, 1 ml of 40% potassium iodate solution and 1 ml of 20% L-ascorbic acid solution were added, and the reaction vessel was attached to a hydride generation apparatus. After the air in the reaction vessel was flushed out with nitrogen stream, 7 ml of 1 % sodium borohydride solution was injected. The generated stibine was collected in the vessel for 30 s, and then the generated gas was introduced by nitrogen stream into the quartz cell heated at 1000℃. The proposed method was also applied for the determination of antimony in Urban Particulate Matter of NBS SRM-1648.
社団法人日本分析化学会の論文
1985-10-05