在500~550℃马弗炉中采用氢氧化钾-硝酸钾熔融样品1 h,热水浸出熔融物后加盐酸酸化,选择Ru 240.272 nm、Ir 212.681 nm为分析线,通过基体匹配法配制标准溶液系列消除基体效应的影响,采用电感耦合等离子体原子发射光谱法(ICP-AES)测定溶液中钌和铱,由此建立了电感耦合等离子体原子发射光谱法测定金属阳极涂层中钌和铱的分析方法.钌和铱在0.50~10 m g/L范围内,其校准曲线线性相关系数均大于0.999;钌和铱的检出限分别为0.03和0.09 g/m2.按照实验方法测定金属阳极涂层样品中钌和铱,结果的相对标准偏差(RSD,n=10)分别为0.69%和1.5%,与原子吸收光谱法(AAS)的测定结果基本吻合.%The sample was fused with potassium hydroxide-potassium nitrate in muffle furnace at 500-550 ℃ for 1 h .After leaching the melt with hot water ,hydrochloric acid was added for acidification .Ru 240. 272 nm and Ir 212. 681 nm were selected as the analytical lines .The influence of matrix effect was eliminated by preparing standard solution series with matrix matching method .The content of ruthenium and iridium in solution was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES ) .Thus ,a determination method of ruthenium and iridium in metal anode coating by ICP-AES was established .As the mass concentration of ruthenium and iridium was in range of 0. 50-10 mg/L ,the linear correlation coefficients of calibration curves were higher than 0.999 ,and the detection limit of ruthenium and iridium was 0. 03 g/m2 and 0. 09 g/m2 ,respectively .The content of ruthenium and iridium in metal anode coating sample was determined according to the experimental method .The relative standard deviation (RSD ,n = 10)was 0. 69% and 1. 5% ,respectively .The results were basically consistent with those obtained by atomic absorption spectrometry (AAS) .
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