Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, P.O. Box 14115-175, Tehran, Iran.
J Chromatogr A. 2010 Apr 16;1217(16):2358-64. doi: 10.1016/j.chroma.2009.11.046. Epub 2009 Nov 26.
A simple, rapid and efficient dispersive liquid-liquid microextraction based on the solidification of floating organic drop (DLLME-SFO) method, followed by inductively coupled plasma-optical emission spectrometry (ICP-OES) was developed for the simultaneous preconcentration and determination of heavy metals in water samples. One variable at a time method was applied to select the type of extraction and disperser solvents. Then, an orthogonal array design (OAD) with OA(16) (4(5)) matrix was employed to study the effects of different parameters on the extraction efficiency. Under the best experimental conditions (extraction solvent: 140microL of 1-undecanol; disperser solvent: 2.0mL of acetone; ligand to metal mole ratio: 20; pH: 6 and without salt addition), the enhancement factor ranged from 57 to 96. The calibration graphs were linear in the range of 0.5-250microgL(-1) for Mn, 1.25-250microgL(-1) for Cr, Co and Cu with correlation coefficient (r) better than 0.990. The detection limits were between 0.1 and 0.3microgL(-1). Finally, the developed method was successfully applied to extraction and determination of the mentioned metal ions in the tap, sea and mineral water samples and satisfactory results were obtained.
一种基于固-液萃取的分散液相微萃取（DLLME-SFO）方法，结合电感耦合等离子体发射光谱法（ICP-OES），用于同时预浓缩和测定水样中的重金属。采用单变量法选择萃取和分散溶剂的类型。然后，采用正交数组设计（OAD）和 OA(16)（4(5)）矩阵研究不同参数对萃取效率的影响。在最佳实验条件下（萃取溶剂：140μL 十一醇；分散溶剂：2.0mL 丙酮；配体与金属摩尔比：20；pH：6 且不加盐），增强因子范围为 57-96。Mn 的校准曲线在 0.5-250μg L(-1)范围内呈线性，Cr、Co 和 Cu 的校准曲线在 1.25-250μg L(-1)范围内呈线性，相关系数（r）均大于 0.990。检测限在 0.1-0.3μg L(-1)之间。最后，该方法成功应用于自来水中、海水中和矿泉水中上述金属离子的提取和测定，得到了满意的结果。
