Shariati Shahab, Yamini Yadollah, Zanjani Mohammadreza Khalili
Department of Chemistry, Faculty of Sciences, Tarbiat Modares University, Tehran, Iran.
J Hazard Mater. 2008 Aug 15;156(1-3):583-90. doi: 10.1016/j.jhazmat.2007.12.061. Epub 2008 Feb 20.
A simple cloud point extraction method followed by inductively coupled plasma-optical emission spectrometry (ICP-OES) was developed for simultaneous preconcentration and determination of trace amounts of U(VI), Th(IV), Zr(IV) and Hf(IV) ions in aqueous samples. The metal ions in 50 ml of aqueous solution (containing 0.1 M sodium acetate, pH 6.0) were formed complexes with dibenzoylmethane (DBM). Then, Triton X-114 (0.2%, w/v) was added to the solution. By increasing the temperature of the solution up to 50 degrees C, a phase separation occurred. After centrifugation at 4000 rpm for 6 min, the surfactant-rich phase (sediment phase) was diluted with 1.0 ml of 20:80 (v/v) of methanol/1 M HNO(3). The metal ions were then determined using ICP-OES. Finally, the main factors affecting the cloud point extraction were evaluated and optimized. Under optimized conditions, enhancement factors in the range of 37.0-43.6 were obtained. The calibration graphs were linear in the range of 0.5-1500 microg l(-1) for Th and Zr, 0.5-500 microg l(-1) for Hf and 2.5-1240 microg l(-1) for U with correlation coefficients (r(2)) better than 0.9926. The detection limits were between 0.1 and 1.0 microg l(-1) and the R.S.D. values for seven replicates were lower than 6.1%.
建立了一种简单的浊点萃取法,结合电感耦合等离子体发射光谱法(ICP-OES),用于同时预富集和测定水样中痕量的U(VI)、Th(IV)、Zr(IV)和Hf(IV)离子。50 ml水溶液(含0.1 M醋酸钠,pH 6.0)中的金属离子与二苯甲酰甲烷(DBM)形成络合物。然后,向溶液中加入Triton X-114(0.2%,w/v)。将溶液温度升至50℃,发生相分离。在4000 rpm下离心6 min后,用1.0 ml 20:80(v/v)的甲醇/1 M HNO₃稀释富含表面活性剂的相(沉淀相)。然后用ICP-OES测定金属离子。最后,对影响浊点萃取的主要因素进行了评估和优化。在优化条件下,获得了37.0 - 43.6范围内的富集因子。钍和锆的校准曲线在0.5 - 1500 μg l⁻¹范围内呈线性,铪在0.5 - 500 μg l⁻¹范围内呈线性,铀在2.5 - 1240 μg l⁻¹范围内呈线性,相关系数(r²)优于0.9926。检测限在0.1 - 1.0 μg l⁻¹之间,七次重复测定的相对标准偏差(R.S.D.)值低于6.1%。