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A New Dispersive Liquid-Liquid Microextraction Method for the Preconcentration of Copper Using 4-Phenyl-3-Thiosemicarbazide and FAAS Detection

机译:4-苯基-3-硫代氨基脲化合物和FAAS检测用于铜预浓缩的分散液微萃取的新方法

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The aim of this study is to develop a new method for the preconcentration of copper via a dispersive liquid-liquid microextraction method using 4-phenyl-3-thiosemicarbazide as a ligand and determination with FAAS in different sample types such as plants, soils and natural waters such as seawater. Optimum experimental conditions were determined, and the applicability of the proposed dispersive liquid-liquid microextraction method was investigated. In the first step of the work, the parameters that affect complex formation and extraction, such as volume of extractant/ disperser solvent, pH and concentration of the chelating agent, NaCl and surfactant, were optimised. The interference effects from potential concomitants on the determination of the Cu(Ⅱ) ion were investigated in synthetic mixtures that contain high levels of these ions. These results showed the analytical applicability of the proposed method in different kinds of samples. Under the optimal conditions, the calibration curve was linear over the range 2-600 μg L~(-1) of copper, and the detection limit was 0.69 μg L~(-1) in the original solution (3 Sb/m). The accuracy of the developed method was checked by analysing certified reference materials (QCS-19 (high purity standard), LGC 6156 (harbour sediment) and NBS 1572 (citrus leaves)). Results obtained were in agreement with certified values with a t test showing that no significant differences at the 95 % confidence interval levels were found. The proposed method was applied to seawater, river water, and plant and soil samples. The recovery values for spiked water samples were between 99.7 and 117.3 %.
机译:这项研究的目的是开发一种新的方法,该方法通过使用4-苯基-3-硫代氨基脲作为配体的分散液-液微萃取方法对铜进行预浓缩,并用FAAS测定不同类型的样品,例如植物,土壤和天然样品。海水等海水。确定了最佳实验条件,并研究了所提出的分散液-液微萃取方法的适用性。在工作的第一步中,优化了影响复合物形成和萃取的参数,例如萃取剂/分散剂的体积,pH值和螯合剂,NaCl和表面活性剂的浓度。在含有高含量这些离子的合成混合物中,研究了潜在伴随物对Cu(Ⅱ)离子测定的干扰作用。这些结果表明了该方法在不同样品中的分析适用性。在最佳条件下,校正曲线在铜的2-600μgL〜(-1)范围内呈线性,在原始溶液(3 Sb / m)中的检出限为0.69μgL〜(-1)。通过分析认证的参考物质(QCS-19(高纯度标准),LGC 6156(海港沉积物)和NBS 1572(柑桔叶))来检查所开发方法的准确性。通过t检验得出的结果与标准值相符,表明在95%的置信区间水平上没有发现显着差异。该方法适用于海水,河水以及植物和土壤样品。加标水样的回收率在99.7%至117.3%之间。

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