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本文首次报道了碱性条件下微量俄(Ⅳ)对KIO_4氧化2-[(3,5-二溴-2-吡啶)-偶氮]-5-二乙氨基苯酚褪色具有显著的催化作用,并以此反应为指示反应建立了测定微锇的催化光度法.此反应的最佳实验条件为:25.0 mL溶液中含0.10 mol/L NaOH 2.0 mL、0.040%2-[(3,5-二溴-2-吡啶)-偶氮]-5-二乙氨基苯酚1.5 mL、1.0X10~(-2)mol/L KIO_43.5mL、沸水浴加热16min.该方法的检测限为0.004μg/mL,饿(Ⅳ)含量在0.0080~0.052μg/mL范围内服从比耳定律.此方法已用于贵金属样品中微锇的测定,结果令人满意.
In this paper, we report for the first time that trace amounts of rumen (Ⅳ) catalyze the fading of KIO_4 2 - [(3,5-dibromo-2-pyridyl) -azo] -5-diethylaminophenol under alkaline conditions A catalytic spectrophotometric method was established for the determination of osmium by this reaction.The optimum conditions for this reaction were as follows: 2.0 mL of 0.10 mol / L NaOH, 25 mL of 0.040% 2 - [(3,5-dibromo 2-pyridyl) -azo] -5-diethylaminophenol and 1.0 × 10 ~ (-2) mol / L KIO_43.5mL, heated in a boiling water bath for 16min.The detection limit of the method was 0.004μg / mL, (Ⅳ) content obeys Beer’s Law in the range of 0.0080 ~ 0.052μg / mL.This method has been applied to the determination of micro osmium in precious metal samples with satisfactory results.