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Preconcentration of Arsenic in Water Samples Using the Composition-Induced Phase Separation Method and Determination by ETAAS

机译:使用组合物诱导的相分离方法和Etaas测定的水样中砷在水样中的前浓度

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A new phase transition microextraction method was developed for determination of trace amount of arsenic ions in water samples in this work. The method is based on the critical point of miscibility of solvents. In this method the mixed solution of sample and organic solvent is initially homogeneous but is separated into two phases by adding a secondary solvent (modifier). In acidic medium As(V) was complexed with ammonium molybdate, this complex was quantitatively extracted to the mixture of organic solvent (acetonitrile/methyl isobutyl ketone) before ETAAS determination. Total inorganic arsenic (III, V) was extracted similarly after oxidation of As(III) to As(V) with nitric acid. Concentration of As(III) was calculated by difference in the concentration between total arsenic and As(V). Optimization of the experimental conditions and instrumental parameters was investigated in detail. A detection limit of 0.05 μgL~(-1) with enrichment factor of 85 was achieved for only 5 mL of sample. The analytical curve was linear in the concentration range of 0.25-4.00 μgL~(-1). Relative standard deviation (RSD) for 10 replicate determinations of 2.0 μgL~(-1) of As(V) was 4,1%. The method was successfully applied to preconcentration and determination of arsenic in real water samples.
机译:开发了一种新的相转移微萃取方法,用于测定这项工作中的水样中的少量砷离子。该方法基于溶剂的混溶性的临界点。在该方法中,样品和有机溶剂的混合溶液最初是均匀的,但通过加入二次溶剂(改性剂)分离成两相。在酸性培养基中作为(V)络合钼酸铵络合,在EtAAS测定之前定量地萃取该配合物以在有机溶剂(乙腈/甲基异丁基酮)的混合物中。在用硝酸氧化为(III)以在氧化为(v)后,在硝酸氧化后同样地提取无机砷(III,V)。浓度为(III)通过总砷和AS(V)之间的浓度差来计算。详细研究了实验条件和仪器参数的优化。只有5ml样品,实现了富集富集为85的0.05μg〜(-1)的检出限。分析曲线在0.25-4.00μg1(-1)的浓度范围内是线性的。对于10μg(-1)的10重复测定的相对标准偏差(RSD)为(v)为4,1%。该方法已成功应用于预浓缩和实际水样中砷的测定。

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