Department of Chemistry, Faculty of Science, University of Tehran, PO Box 14155-64555, Tehran, Iran.
Talanta. 2012 Aug 15;97:235-41. doi: 10.1016/j.talanta.2012.04.024. Epub 2012 May 3.
Ultrasonic-assisted emulsification microextraction (USAEME) combined with inductively coupled plasma-optical emission spectrometry (ICP-OES) was used for preconcentration and determination of aluminum, bismuth, cadmium, cobalt, copper, iron, gallium, indium, nickel, lead, thallium and zinc in real water samples. Ammonium pyrrolidine dithiocarbamate (APDC) and carbon tetrachloride (CCl(4)) were used as the chelating agent and extraction solvent, respectively. The effective parameters (factors) of the extraction process such as volume of extraction solvent, pH, sonication time, and concentration of chelating agent were optimized by a small central composite design (CCD). The optimum conditions were found to be 98 μL for extraction solvent, 1476 mg L(-1) for chelating agent, 3.8 for pH and 9 min for sonication time. Under the optimal conditions, the limits of detection (LODs) for Al, Bi, Cd, Co, Cu, Fe, Ga, In, Ni, Pb, Tl and Zn were 0.13, 0.48, 0.19, 0.28, 0.29, 0.27, 0.27, 0.38, 0.44, 0.47, 0.52 and 0.17 μg L(-1), respectively. The linear dynamic range (LDR) was 1-1000 μ gL(-1) with determination coefficients of 0.991-0.998. Relative standard deviations (RSDs, C=200 μg L(-1), n=6) were between 1.87%-5.65%. The proposed method was successfully applied to the extraction and determination of heavy metals in real water samples and the satisfactory relative recoveries (90.3%-105.5%) were obtained.
超声辅助乳化微萃取（USAEME）结合电感耦合等离子体-原子发射光谱法（ICP-OES）用于实际水样中铝、铋、镉、钴、铜、铁、镓、铟、镍、铅、铊和锌的预浓缩和测定。使用氨 基吡咯烷二硫代氨基甲酸盐（APDC）和四氯化碳（CCl4）分别作为螯合剂和萃取溶剂。通过小中心组合设计（CCD）优化了萃取过程的有效参数（因素），如萃取溶剂的体积、pH 值、超声时间和螯合剂的浓度。发现最佳条件为萃取溶剂 98μL、螯合剂 1476mgL(-1)、pH 值 3.8 和超声时间 9min。在最佳条件下，Al、Bi、Cd、Co、Cu、Fe、Ga、In、Ni、Pb、Tl 和 Zn 的检出限（LOD）分别为 0.13、0.48、0.19、0.28、0.29、0.27、0.27、0.38、0.44、0.47、0.52 和 0.17μg L(-1)。线性动态范围（LDR）为 1-1000μg L(-1)，测定系数为 0.991-0.998。相对标准偏差（RSD，C=200μg L(-1)，n=6）在 1.87%-5.65%之间。该方法成功应用于实际水样中重金属的提取和测定，获得了令人满意的相对回收率（90.3%-105.5%）。
