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Comparative study of the selectivity of a kinetic-catalytic method: the determination of Cr (VI) by oxidation of the o-dianisidine by hidrogen peroxide

机译:动力学催化方法选择性的比较研究:过氧化氢通过邻二苯胺氧化氧化法测定六价铬

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摘要

Selectivity studies for the determination of Cr(VI) using the catalytic oxidation of the o-dianisidine by hydrogen peroxide showed two distincts situations. In the first, when interferents were studied by a univariate procedure, Cr(III) and Cu(II) cause serious interferences even at the 2:1 proportion, relative to Cr(VI), while Fe(III) interfered at the 15:1 ratio and EDTA at the 10:1 ratio. On the other hand, when a multivariate investigation was performed, Cr(III) did not present any significant principal effects and its significant interaction effects were negative, in contrast to EDTA, that presented positive interaction effects although, like Cr(III), did not show significant interaction effects. In view of the interferent's action it become necessary to separate Cr(VI) by extraction with methylisobutylketone in a chloridric acid medium before its determination in vegetals and in wastewater from a cellulose industry samples. Using this procedure, the method precision is ±0,5% at the 10 ng/mL Cr(VI) concentration level. The detection and quantification limits, calculated by means of absorbance measurements of ten replicates of blank reagents were 1,1 and 3,2 ng/mL, respectively. The results obtained with real samples showed a relative standard deviation between 1,2% and 3,0% relative to their reference values.
机译:用过氧化氢催化邻二苯胺催化氧化测定六价铬的选择性研究表明了两种不同的情况。首先,当采用单变量方法研究干扰物时,相对于Cr(VI),Cr(III)和Cu(II)甚至以2:1的比例也会造成严重干扰,而Fe(III)在15:比率为1,EDTA比率为10:1。另一方面,当进行多变量研究时,Cr(III)没有表现出任何显着的主效应,并且与EDTA相比,Cr(III)表现出了积极的交互作用,而与Cr(III)一样,它具有显着的交互作用。没有显示出明显的交互作用。考虑到干扰物的作用,在植物和纤维素工业样品的废水中测定甲基之前,需要先在氯酸介质中用甲基异丁酮萃取分离出六价铬。使用此程序,在10 ng / mL Cr(VI)浓度水平下,方法精度为±0.5%。通过十次重复空白试剂的吸光度测量得出的检测限和定量限分别为1.1 ng / mL和3.2 ng / mL。实际样品获得的结果表明,相对于参考值,相对标准偏差在1,2%和3.0%之间。

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