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Kinetic Spectrophotometric Method for the Determination of Selenium (IV) by Its Catalytic Effect on the Reduction of Arsenazo III with Sodium Hypophosphite in Micellar Media

机译:动力学分光光度法,用于测定硒(IV)的催化作用对胶束介质中次磷酸钠减少砷胂III的催化作用

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A simple and sensitive kinetic spectrophotometric method for the determination of trace selenium (IV) is described, based on its catalytic effect on the reduction arsenazo III (AsA III) with sodium hypophosphite (NaH_2PO_2) in a solution of 0.02 mol/L sulfuric acid and in the presence of cationic micellar media. The reaction rate is monitored spectrophotometrically by measuring the decrease in absorbance of AsA III at 550 nm with a fixed-time method. The decrease in the absorbance of AsA III is proportional to the concentration of Se(IV) in the range 0.16-1.0μg/L after a fixed time of 4-10 min from the initiation of the reaction. The limit of detection is 0.049μg/L Se(IV). The influence of the factors such as acidity, concentration of reactants, type and concentration of surfactants, reactive time, temperature and co-existing ions on the reaction is discussed. The optimum reaction conditions of reaction are established and some kinetic parameters are determined; the apparent activation energy of catalytic reaction is 59.51 kJ/mol. The relative standard deviation for eleven replicate determination of 0.02, and 0.01μg/25 mL Se(IV) was 2.0% and 2.4%, respectively. Combined with sulphydryl dextrane gel (SDG) separation and enriching, the method has been successfully applied to the determination of Se (IV) in foodstuff and human hair samples with the relative standard deviation of 2.1%-5.8% and the recovery of 97.0%-103.3%, the results are in good agreement with those provided by ICP-AES method.
机译:基于其在0.02mol / L硫酸的溶液中,基于其对次磷酸钠(NaH_2PO_2)的催化作用,描述了用于测定痕量硒(IV)的简单敏感的动力学分光光度法。在存在阳离子胶束介质。通过用固定时间方法测量550nm处的ASA III的吸光度降低,通过测量分光光度法进行分光光度法监测反应速率。 ASA III的吸光度降低与0.16-1.0μg/ L的SE(IV)的浓度比例在4-10分钟的21-1.0μg/ L源于反应的固定时间后。检测限为0.049μg/ L SE(IV)。讨论了酸度,反应物浓度,表面活性剂浓度,反应性时间,温度和共同存在于反应中的影响的影响。确定反应的最佳反应条件,确定一些动力学参数;催化反应的表观活化能量为59.51 kJ / mol。 11重复测定0.02和0.01μg/ 25mL SE(IV)的相对标准偏差分别为2.0%和2.4%。结合硫酰葡聚糖凝胶(SDG)分离和富集,该方法已成功应用于食品中SE(IV)的测定,相对标准偏差为2.1%-5.8%,回收率为97.0% - 103.3%,结果与ICP-AES方法提供的结果良好。

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