过氧化氢氧化邻硝基苯基荧光酮褪色反应动力学光度法测定痕量钌  被引量:2

Kinetic spectrophotometric determination of trace ruthenium based on oxidation of o-nitrophenylfluorone with hydrogen peroxide

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作  者:周之荣[1] 张丽珍[2] 王群[3] 章淑媛[3] 张圆玲 苏志文 

机构地区:[1]广东药学院公共卫生学院,广东广州510240 [2]广东药学院附属门诊部,广东广州510240 [3]东华理工大学校医院,江西抚州344000 [4]江西省临川第一中学,江西抚州344100

出  处:《冶金分析》2008年第12期66-69,共4页Metallurgical Analysis

基  金:广东药学院科研基金资助项目

摘  要:基于NaOH碱性介质中,痕量钌(Ⅲ)催化H2O2氧化邻硝基苯基荧光酮(o-NO2-PF)的褪色反应,建立了测定痕量钌(Ⅲ)的动力学光度法。在固定加热时间段(6min)后,通过加入HCl酸化终止催化反应,于465nm处测定o-NO2-PF的吸光度降低值监控反应速率。方法检出限为0.01μg/L,校准曲线的浓度线性范围为0.0~1.0μg/L。测定0.02μg钌(Ⅲ)的相对标准偏差为2.06%(n=11)。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73.95kJ/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1.78%~2.84%,加标回收率为97.5%~104.4%。A spectrophotometric method for the determination of ruthenium(Ⅲ) is described, based on its catalytic effect on the oxidation reaction of o-nitrophenylfluorone (o-NO2-PF) with hydrogen peroxide in sodium hydroxide medium at 60 ℃. The above catalytic reaction is terminated through acidification by the addition of hydrochloric acid after a fixed time (6 min), and the reaction rate is monitored spectrophotometrically by measuring the decrease in the absorbance of o-NO2-PF at 465 nm. The calibration curve is linear in the concentration range over 0. 0-1.0μg/L ruthenium(Ⅲ)) and the detection limit of the method is 0.01 μg/L. The optimum conditions of reaction are established and some kinetic parameters are determined. The apparent activation energy of catalytic reaction is 73.95 kJ/mol. The relative standard deviation for ruthenium(Ⅲ) of 0. 02 μg in 25 mL is 2.06 % (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) of 1.78 %- 2. 84% and the recovery over 97.5%-104.4 %.

关 键 词:动力学光度法 钌(Ⅲ) 邻硝基苯基荧光酮 过氧化氢 

分 类 号:O657.32[理学—分析化学]

 

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