Hardcastle J L, Compton R G
Physical and Theoretical Chemistry Laboratory, University of Oxford, UK.
Analyst. 2001 Nov;126(11):2025-31. doi: 10.1039/b106402a.
N-benzoyl-N-phenyl-hydroxylamine dissolved in ethyl acetate was employed as a ligand for the solvent extraction of copper. Ultrasonic emulsification was shown to be effective both in the extraction of copper from an aqueous phase into ethyl acetate and its recovery or "back extraction" into a fresh clean aqueous solution. Experimental determination of thermodynamic parameters governing the extraction process via UV/visible spectroscopy is reported. This permitted theoretical predictions for the amount of copper transferred into the final aqueous solution to be fitted to experimental data. Quantitative analysis of copper removed via double sono-extraction from an aqueous medium hostile to voltammetric analysis proceeded via sono-square wave anodic stripping voltammetry analysis (sono-SWASV). This resulted in very high sensitivity in the relatively clean medium. The technique was then applied to the analysis of copper in the soft drink 'Ribena Light'. In the absence of sample preparation by solvent extraction sono-SWASV yields a measurable peak current for copper. However it is irreproducible and erratic due to passivating effects, possibly attributed to the sugars, natural flavourings and colourings present. Following sono-solvent extraction, the overall copper concentration could be obtained with a detection limit of 2 microg L(-1). Biphasic sono-extraction synergistically coupled with the recognized technique sono-SWASV presents an attractive technique for copper analysis in electrode passivating media. The technique necessarily removes contaminants present in the test solution since these will prefer to remain in the initial aqueous phase, or will transfer to the organic phase but are unlikely to be doubly transferred into the 'clean' final aqueous phase.
溶解于乙酸乙酯中的N-苯甲酰基-N-苯基羟胺被用作溶剂萃取铜的配体。结果表明,超声乳化在将铜从水相萃取到乙酸乙酯中以及将其回收或“反萃取”到新鲜干净的水溶液中均有效。报道了通过紫外/可见光谱法对萃取过程的热力学参数进行实验测定。这使得对转移到最终水溶液中的铜量的理论预测能够与实验数据相拟合。通过超声-方波阳极溶出伏安法(sono-SWASV)对从不利于伏安分析的水介质中通过双超声萃取去除的铜进行定量分析。这在相对干净的介质中产生了非常高的灵敏度。然后将该技术应用于软饮料“Ribena Light”中铜的分析。在不通过溶剂萃取进行样品制备的情况下,sono-SWASV可产生可测量的铜峰电流。然而,由于钝化效应,它是不可重复且不稳定的,钝化效应可能归因于其中存在的糖、天然香料和色素。经过超声-溶剂萃取后,可获得总铜浓度,检测限为2 μg L⁻¹。双相超声萃取与公认的sono-SWASV技术协同结合,为电极钝化介质中的铜分析提供了一种有吸引力的技术。该技术必然会去除测试溶液中存在的污染物,因为这些污染物更倾向于留在初始水相中,或者会转移到有机相中,但不太可能再次转移到“干净”的最终水相中。