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基于钒(V)对二溴邻苯三酚红-偶氮胂与溴酸钾反应的催化作用,用动力学分光光度法测定痕量钒(V)。

Kinetic-spectrophotometric determination of trace amounts of vanadium(V) based on its catalytic effect on the reaction of DBM-arsenazo and potassium bromate.

作者信息

Zhai Qing-Zhou, Zhang Xiao-Xia, Huang Chong

机构信息

Research Center for Nanotechnology, Changchun University of Science and Technology, Weixing Road, Changchun 130022, PR China.

出版信息

Spectrochim Acta A Mol Biomol Spectrosc. 2008 Mar;69(3):911-6. doi: 10.1016/j.saa.2007.05.054. Epub 2007 May 25.

Abstract

A simple and sensitive kinetic-spectrophotometric method is developed for the determination of trace vanadium(V), based on the catalytic effect of vanadium(V) on the oxidation of DBM-arsenazo by potassium bromate in 0.0138 moll(-1) phosphoric acid medium and at 100 degrees C in the presence of citric acid as activator. The absorbance is measured at 528 nm with the fixed-time method. The optimization of the operating conditions regarding concentrations of the reagents, temperature and interferences are also investigated. The working curve is linear over the concentration range 0-20 ngml(-1) of vanadium(V) with good precision and accuracy and the detection limit was down to 3.44 ngl(-1). The relative standard deviation for a standard solution of 14 ngml(-1) is 0.28% (n=11). The apparent activity energies of the catalytic reaction and the non-catalytic reaction are 73.48, 113.5 kJ/mol, respectively. The proposed method proved highly sensitive, selective and relatively rapid for the assay of vanadium at low-level range of 0-20 ngml(-1) without any pre-concentration step. Thw method was applied to the determination of vanadium(V) in steels, rice, flour, cabbage, potato, fish, shrimp and tea samples with satisfactory results. The obtained results for the steel samples were excellent agreement with the standard reference values. The analytical results of the rice, flour, cabbage, potato, fish, shrimp and tea samples were excellent agreement with those of atomic absorption spectrometry. The recovery experiments have been made for the rice, flour, cabbage, potato, fish, shrimp and tea samples except the steels; excellent results were obtained. The relative standard deviations were over the range of 0.18-2.60% and the recoveries were over the range of 98.00-102.4%, respectively. The analytical results obtained were satisfactory.

摘要

基于在0.0138 moll(-1)磷酸介质中,100℃条件下,以柠檬酸为活化剂时钒(V)对溴酸钾氧化二溴邻苯三酚红砷酸锆的催化作用,建立了一种简单灵敏的动力学分光光度法测定痕量钒(V)。采用固定时间法在528 nm处测量吸光度。还研究了试剂浓度、温度和干扰等操作条件的优化。钒(V)浓度在0-20 ngml(-1)范围内工作曲线呈线性,精密度和准确度良好,检出限低至3.44 ngl(-1)。14 ngml(-1)标准溶液的相对标准偏差为0.28%(n=11)。催化反应和非催化反应的表观活化能分别为73.48、113.5 kJ/mol。所提出的方法在0-20 ngml(-1)的低水平范围内测定钒时具有高灵敏度、高选择性且相对快速,无需任何预浓缩步骤。该方法应用于钢、大米、面粉、卷心菜、土豆、鱼、虾和茶叶样品中钒(V)的测定,结果令人满意。钢样品的测定结果与标准参考值吻合良好。大米、面粉、卷心菜、土豆、鱼、虾和茶叶样品的分析结果与原子吸收光谱法的结果吻合良好。除钢样品外,对大米、面粉、卷心菜、土豆、鱼、虾和茶叶样品进行了回收率实验,结果良好。相对标准偏差在0.18-2.60%范围内,回收率在98.00-102.4%范围内。获得的分析结果令人满意。

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