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作 者:周之荣[1] 毋福海[1] 黄丽玫[1] 白研[1] 陈红红[1] 杨冰仪[1] 颜戊利[1] 陈海珍[1]
机构地区:[1]广东药学院公共卫生学院,广东广州510240
出 处:《冶金分析》2009年第12期42-46,共5页Metallurgical Analysis
基 金:广东省高等学校人才引进专项资金资助项目(粤财教[2009]109号);广东药学院科研基金资助项目(2007GGW03)
摘 要:基于稀硫酸介质中,反应温度为80℃时,痕量钌(Ⅲ)阻抑H2O2氧化酸性品红的褪色反应,通过乳化剂OP增敏,建立了测定痕量钌㈣的表面活性剂增敏阻抑反应动力学光度法。在固定加热时间段(10min)后,于546nm处测定酸性品红的吸光度增加值监控反应速率。方法的检出限为0.01μg/L,校准曲线的浓度线性范围为0.03~1.0μg/L。在25mL溶液中,测定0.02gg钌㈣的相对标准偏差为2.1%(n=11)。讨论了酸度、反应物浓度、表面活性剂的种类和用量、温度、反应时间、干扰离子等因素的影响。研究了反应的最佳条件,并测定了一些动力学参数,催化反应的表观活化能为65.60kJ/mol。方法用于矿样和冶金产品中钌(Ⅲ)的测定,结果与推荐值相符,相对标准偏差为2.8%~3.6%,加标回收率为98%~102%。In sodium hydroxide medium,trace ruthenium(Ⅲ) could inhibit the oxidation of acid fuchsine with hydrogen peroxide at the temperature of 80℃. On the basis of this phenomenon,a kinetic spectrophotometric method was established for determining ruthenium(Ⅲ) through sensitizing with OP emulsifier. The reaction rate is monitored spectrophotometrically by measuring the increase in the absorbance of acid fuchsine at 546 nm after a fixed heating time (10 min). The calibration curve for the recommended method is linear in the concentration range over 0.03-1.0μg/L ruthenium (Ⅲ), and the detection limit of the method is 0. 01 μg/L. The influence of the factors, such as acidity, concentration of reactants, types and concentration of surfactants, reaction time, temperature and co-existing ions, on the reaction is discussed. The optimum conditions of reaction are established, and some kinetic parameters are determined. The apparent activation energy of catalytic reaction is 65. 60 kJ/mol. The relative standard deviation for 0.02 μg/25 mL ruthenium (Ⅲ) is 2.1% (n=11). The method has been successfully applied for the determination of trace ruthenium in some ores and metallurgy products with the relative standard deviations (RSD) over 2.8 %--3.6%, and the recovery over 98%- 102%.
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