Mirzaei Mohammad, Behzadi Mansoureh
Shahid Bahonar University of Kerman, Department of Chemistry, Kerman, Iran.
J AOAC Int. 2013 Mar-Apr;96(2):441-6. doi: 10.5740/jaoacint.11-105.
A simple and rapid dispersive liquid-liquid microextraction based on solidification of floating organic drop method prior to flame atomic absorption spectrometry was developed for preconcentration and determination of copper. In this technique, simultaneous complex formation and extraction was performed with rapid injection of a mixture containing ethanol, 1-undecanol, and 1-(2-pyridylazo)-2-naphthol into a water sample spiked with Cu(II). After centrifugation, the test tube was cooled in an ice bath, and solidified extract transferred into a conical vial. Finally, it was dissolved into ethanol and copper concentration was determined. Some effective parameters of extraction and complex formation, such as extraction and disperser solvent type and volume, pH, concentration of the chelating agent, salt effect, and extraction time, were optimized. Under the optimum conditions, the calibration graph was linear in the range of 0.50 ng/mL to 0.30 microg/mL, with an LOD of 0.16 ng/mL. The RSD for 10 replicate measurements of 50.0 ng/mL of copper was +/- 1.4%. Two certified reference materials were analyzed, and the determined values were in good agreement with the certified values.
建立了一种基于漂浮有机滴固化法的简单快速分散液液微萃取方法,用于火焰原子吸收光谱法之前对铜的预富集和测定。在该技术中,将含有乙醇、1-十一醇和1-(2-吡啶偶氮)-2-萘酚的混合物快速注入加有Cu(II)的水样中,同时进行络合物形成和萃取。离心后,将试管在冰浴中冷却,固化的萃取物转移至锥形瓶中。最后,将其溶解于乙醇中并测定铜的浓度。对萃取和络合物形成的一些有效参数,如萃取剂和分散剂的类型及体积、pH值、螯合剂浓度、盐效应和萃取时间进行了优化。在最佳条件下,校准曲线在0.50 ng/mL至0.30 μg/mL范围内呈线性,检出限为0.16 ng/mL。对50.0 ng/mL的铜进行10次重复测量的相对标准偏差为±1.4%。分析了两种有证标准物质,测定值与认定值吻合良好。