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在硫酸和热水浴中,Os( Ⅳ) 催化高碘酸钾氧化偶氮胂Ⅲ褪色,建立了测定锇的新催化光度法。锇质量浓度在0 ~0-10μg/25ml 范围内符合比尔定律,检出限为9-7 ×10 - 5μg/ml。对0-050μg/25ml Os( Ⅳ) 测定的相对标准偏差为1-28 % (n = 11) 。催化反应的表观活化能为102-2kJ/mol。催化反应对Os( Ⅳ) 和偶氮胂Ⅲ分别为一级反应。试验了40 多种共存离子的影响,允许500 倍量Ag+ ,400 倍量Au( Ⅲ) 和Pt( Ⅳ) ,25 倍量Pd( Ⅱ) 、Ir( Ⅳ) 及Cu2 + 存在。该方法已用于岩矿和冶金产品中锇的测定,相对标准偏差为0-68 % ~3-92 % ,标准加入回收率为99-8 % ~103-0 % 。
Os (Ⅳ) catalyzed the oxidation of arsenazo Ⅲ by potassium periodate in sulfuric acid and hot water baths. A new catalytic spectrophotometric method was developed for the determination of osmium. Beer’s law was obeyed in the range of 0 ~ 0-10μg / 25ml with the detection limit of 9-7 × 10-5μg / ml. The relative standard deviation for the 0-050 μg / 25 ml Os (IV) assay was 1-28% (n = 11). The apparent activation energy of the catalytic reaction is 102-2kJ / mol. The catalytic reaction of Os (Ⅳ) and arsenazo Ⅲ were first-order reactions, respectively. More than 40 kinds of coexisting ions were tested to allow the presence of 500 times Ag +, 400 times the amount of Au (Ⅲ) and Pt (Ⅳ), 25 times of Pd (Ⅱ), Ir (Ⅳ) and Cu2 +. The method has been applied to the determination of osmium in rock and mine products and metallurgical products. The relative standard deviations are 0-68% ~ 3-92%, and the standard recoveries are 99-8% -103-0%.