样品溶液以1.0 mL/min的流量通过微型树脂交换柱交换分离后,样品中Cr(Ⅵ)被磷酸三丁酯(TBP)萃淋树脂吸附,用0.5 mol/L HCl和水分别进行淋洗,Cr(Ⅵ)与样品中Fe3+、Al3+、Cr(Ⅲ)等干扰测定的金属离子分离,从而实现了对Cr(Ⅵ)的分离富集.在0.05 mol/L H2SO4介质中,痕量Cr(Ⅵ)强烈催化高碘酸钾与核固红的氧化褪色反应,基于该种作用,建立了一种新的测定痕量Cr(Ⅵ)的催化光度法.体系的最大吸收波长为555 nm,Cr(Ⅵ)在0~10.0 μg/L范围内符合比尔定律,方法的检出限为2.01×10-2 μg/L.方法用于测定电镀废水中痕量Cr(Ⅵ),测定结果与电感耦合等离子体原子发射光谱法(ICP-AES)相符,6次测定值的相对标准偏差(RSD)小于4%.
The sample solution passed through micro resin exchange column for exchange and separation at flow rate of 1.0 mL/min.Cr(Ⅵ) in the sample was adsorbed by tributyl phosphate (TBP) extraction-elution resin.After elution with 0.5 mol/L HCl and water, Cr(Ⅵ) could be separated from metal ions that had interference with determination such as Fe3+, Al3+ and Cr(Ⅲ), which realizing the separation and enrichment of Cr(Ⅵ).In 0.05 mol/L H2SO4 medium, trace Cr(Ⅵ) could strongly catalyze the oxidizing decoloring reaction between potassium periodate and nuclear fast red.Consequently, a new determination method of trace chromium(Ⅵ) by catalytic spectrophotometry was established.The maximum absorption wavelength of this system was 555 nm.Beer's law was obeyed for Cr(Ⅵ) in range of 0-10.0 μg/L.The detection limit was 2.01×10-2 μg/L.The proposed method was applied to the determination of trace chromium(Ⅵ) in electroplating wastewater.The results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES).The relative standard deviation (RSD, n=6) was less than 4%.
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