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在硫酸介质和热水浴中 ,Os( )对高碘酸盐氧化耐尔蓝有催化作用。研究了反应速率对酸度、浓度、温度和离子强度的依赖关系 ,采用 0 .0 1 0mol/ L硫酸 ,反应的灵敏度随温度升高而增大 ,反应速率对反应混合物的离子强度依赖较小。线性范围为 0～ 0 .2 5μg/ 2 5m L;检出限为 8.0 2× 1 0 -5 μg/ m L;对质量浓度为 0 .1 0 μg/ 2 5m L 的 Os( )测定的相对标准偏差为 1 .0 2 % ( n=1 1 ) ;导出了催化反应的动力学方程 ;探讨了反应机理。4 0 0倍量以上常见金属离子不干扰锇的测定 ,1 0倍量以上的 Ru( )、Fe3 +有干扰。本法已用于贵金属冶金样品中锇的测定。
Os () catalyzes the periodate oxidation of nile blue in sulfuric acid and hot water baths. The dependence of reaction rate on acidity, concentration, temperature and ionic strength was studied. The sensitivity of the reaction increased with the increase of temperature with 0.001mol / L sulfuric acid, and the reaction rate had little dependence on the ionic strength of the reaction mixture. The linear range was 0 ~ 0.525μg / 2 5m L; the detection limit was 8.0 × 10 -5 μg / m L; for Os () 0 with mass concentration of 0.1 μg / The standard deviation was 1.02% (n = 1 1). The kinetic equation of the catalytic reaction was derived. The reaction mechanism was also discussed. More than 400 times the amount of common metal ions do not interfere with the determination of osmium, 10 times the amount of Ru (), Fe3 + interference. This method has been used for the determination of osmium in precious metal samples.