Aouarram A, Galindo-Riaño M D, García-Vargas M, Stitou M, El Yousfi F
Department of Analytical Chemistry, Faculty of Science, University of Cádiz, Campus Río San Pedro, 11510 Puerto Real, Cádiz, Spain.
Talanta. 2007 Jan 15;71(1):165-70. doi: 10.1016/j.talanta.2006.03.038. Epub 2006 May 2.
The use of a permeation liquid membrane system for the preconcentration and separation of nickel in natural and sea waters and subsequent determination by atomic absorption spectroscopy is presented. 2-Hydroxybenzaldehyde N-ethylthiosemi-carbazone (2-HBET) in toluene is used as the active component of the liquid membrane. A study strategy based on a simplex design has been followed. Several chemical and physical parameters were optimized. Maximum permeation coefficient was obtained at a feed solution pH of 9.4, 0.3mol l(-1) of HNO(3) in the stripping solution and 1.66mmol l(-1) of 2-HBTE in toluene as carrier. The precision of the method was 4.7% at 95% significance level and a detection limit of 0.012microg l(-1) of nickel was achieved. The preconcentration procedure showed a linear response within the studied concentration range from 3 to 500microg l(-1) of Ni in the feed solution. The method was validated with different spiked synthetic seawater and certified reference water samples: TMDA-62 and LGC 6016, without matrix interferences and showing good concordance with the certified values, being the relative errors -5.9% and -2.2%, respectively. Under optimal conditions, the average preconcentration yield for real seawater samples was 98+/-5%, with a nickel preconcentration factor of 20.83 and metal concentrations ranging between 2.8 and 5.4microg l(-1).
介绍了一种采用渗透液膜系统对天然水和海水中的镍进行预富集和分离,随后用原子吸收光谱法进行测定的方法。甲苯中的2-羟基苯甲醛N-乙基硫代半卡巴腙(2-HBET)用作液膜的活性成分。采用了基于单纯形设计的研究策略。对几个化学和物理参数进行了优化。在进料溶液pH为9.4、反萃溶液中HNO₃浓度为0.3mol l⁻¹以及甲苯中2-HBTE浓度为1.66mmol l⁻¹作为载体的条件下,获得了最大渗透系数。该方法在95%置信水平下的精密度为4.7%,镍的检测限达到0.012μg l⁻¹。预富集过程在所研究的进料溶液中镍浓度范围为3至500μg l⁻¹内呈线性响应。该方法用不同加标合成海水和有证参考水样TMDA-62和LGC 6016进行了验证,无基体干扰,且与认定值具有良好的一致性,相对误差分别为-5.9%和-2.2%。在最佳条件下,实际海水样品的平均预富集回收率为98±5%,镍的预富集因子为20.83,金属浓度范围在2.8至5.4μg l⁻¹之间。