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在磷酸介质和热水浴中,Ru(Ⅲ)催化溴酸钾氧化棉红褪色,由此建立了动力学光度法测定痕量钌的新方法。钌的质量浓度在0.00—0.10μg/mL范围内与lgA0/A呈良好的线性关系,其线性回归方程为:lgA0/A=0.2926CRu-0.003,相关系数r=0.9997,检测限为4.06×10-8g/mL。实验考察了影响催化反应的因素,确定了反应的最佳条件,测定了催化动力学参数,反应的表观活化能Ea′=53.02kJ/moL,表观速率常数k′=1.75×10-4s-1,确立了反应速率方程,探讨了反应机理,试验了20多种共存离子的影响,方法用于合成水样和矿样中钌的测定,回收率94.8%—104.0%,相对标准偏差0.6%—2.4%。
In phosphoric acid medium and hot water bath, Ru (Ⅲ) catalyzes the discoloration of cotton red by potassium bromate, and thus a new method for the determination of trace ruthenium by kinetic spectrophotometry was established. The linear regression equation of ruthenium in the range of 0.00-0.10μg / mL with lgA0 / A was linear regression equation: lgA0 / A = 0.2926CRu-0.003, correlation coefficient r = 0.9997, the detection limit was 4.06 × 10 -8g / mL. The factors influencing the catalytic reaction were investigated experimentally to determine the optimum reaction conditions. The catalytic kinetic parameters were determined. The apparent activation energy Ea ’was 53.02kJ / mol and the apparent rate constant k’ was 1.75 × 10-4s -1, the reaction rate equation was established, the reaction mechanism was discussed and the effect of more than 20 kinds of coexisting ions was tested. The method was applied to the determination of ruthenium in synthetic water samples and ore samples with the recovery of 94.8% -104.0% and the relative standard deviation of 0.6 % -2.4%.