高碘酸盐氧化耐尔蓝动力学光度法测定锇  

Kinetic Spectrophotometric Method for Osmium Determination Based on Oxidation of Nile Blue by Periodate

作　　者：李祖碧[1] 王加林[1] 李立新[2] 徐其亨[3] 

机构地区：[1]云南大学成人教育学院,昆明650091 [2]昆明贵金属研究所,昆明650221 [3]云南大学化学系,昆明650091

出　　处：《分析试验室》2000年第2期1-4,共4页Chinese Journal of Analysis Laboratory

摘　　要：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。The catalytic action of Os(Ⅳ) on the oxidation of nile blue (NB) by periodate was observed in concentration 0.010 mol/L H 2SO 4 on a hot water bath.The dependence of the reaction rate on the acidity,concentration,temperature,and ionic strength was studied.A temperature increase was followed by an increase in the sensitivity of the reaction.The rate of the reaction depended little on the ionic strength of the reaction mixture.The calibration graph of Os oxidation is linear for 0～10 ng/mL of Os(Ⅳ).The detection limit is 0.08 ng/mL .The relative standard deviation for the determination of 4 ng/mL for Os(Ⅳ) is 1.02% ( n =11).A kinetic equation was derived.The majority of metal ions at a 400-fold amounts did not interfere with Os determination,Ru(Ⅲ) and Fe 3+ >10 fold amounts did not interfere.The method was applied to the determination of Os in real samples with satisfactory reusults.

关 键 词：锇 耐尔蓝 高碘酸盐 金属 冶金样品 光度法 

分 类 号：TG115.33[金属学及工艺—物理冶金] O614.824[金属学及工艺—金属学]