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首页> 外文期刊>The Analyst: The Analytical Journal of the Royal Society of Chemistry: A Monthly International Publication Dealing with All Branches of Analytical Chemistry >The electroanalytical detection and determination of copper in heavily passivating media: ultrasonically enhanced solvent extraction by N-benzoyl-N-phenyl-hydroxylamine in ethyl acetate coupled with electrochemical detection by sono-square wave strip
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The electroanalytical detection and determination of copper in heavily passivating media: ultrasonically enhanced solvent extraction by N-benzoyl-N-phenyl-hydroxylamine in ethyl acetate coupled with electrochemical detection by sono-square wave strip

机译:重钝化介质中铜的电分析检测和测定:用乙酸乙酯中的N-苯甲酰基-N-苯基-羟胺超声强化溶剂萃取,再加上声波方波带电化学检测

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摘要

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 μg 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.
机译:溶解在乙酸乙酯中的N-苯甲酰基-N-苯基-羟胺被用作溶剂萃取铜的配体。超声乳化在将铜从水相中萃取到乙酸乙酯中以及将其回收或“反萃取”到新鲜清洁的水溶液中均显示有效。报道了通过紫外/可见光谱法控制萃取过程的热力学参数的实验确定。这使得理论上对转移到最终水溶液中的铜量的预测适合于实验数据。通过声波方波阳极溶出伏安法(sono-SWASV)对从敌对的水溶液介质中进行双次声纳萃取去除的铜进行定量分析。这导致在相对干净的介质中具有很高的灵敏度。然后将该技术应用于软饮料“ Ribena Light”中的铜分析。在没有通过溶剂萃取进行样品制备的情况下,sono-SWASV会产生可测量的铜峰值电流。然而,由于钝化作用,它是不可复制的且不稳定的,这可能归因于存在的糖,天然调味剂和色素。超声溶剂萃取后,总铜浓度可以达到2μgL〜(-1)的检出限。双相超声提取与公认的技术协同结合,sono-SWASV为电极钝化介质中的铜分析提供了一种有吸引力的技术。该技术必须去除存在于测试溶液中的污染物,因为这些污染物将更倾向于保留在初始水相中,或者将转移至有机相,但不太可能被双重转移至“干净的”最终水相中。

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