Faculty of Chemistry, Tarbiat Moallem University, Tehran, Iran.
Spectrochim Acta A Mol Biomol Spectrosc. 2012 Dec;98:70-5. doi: 10.1016/j.saa.2012.08.027. Epub 2012 Aug 23.
A cloud-point extraction process coupled to ICP-OES by using 3-nitro benzaldehyde thiosemicarbazone (3-NBT) as complexing agent was developed for the simultaneous preconcentration and determination of copper and mercury in water samples. The variables affecting the complexation and extraction steps were optimized. Under the optimum conditions (i.e. 1.5×10(-5) mol L(-1) ligand, 0.3% (v/v) Triton X-114, 55 °C equilibrium temperature, incubation time of 30 min) the calibration graphs were linear in the range of 5-120 and 10-100 ng mL(-1) with enhancement factor of 82.7 and 51.3 for Cu(2+) and Hg(2+), respectively. The preconcentration factors were 28.6 in both cases and detection limits were obtained 0.48 for Cu and 1.1 ng mL(-1) for Hg. The precisions (R.S.D.%) for five replicate determinations at 50 ng mL(-1) of copper and mercury were better than 1.8% and 3.2%, respectively. The accuracy of the proposed method is validated by analyzing a certified reference material of water (RTC-QCI-049) with satisfactory results. Finally, the proposed method was utilized successfully for the determination of copper and mercury in surface water (river), tap water and bottled mineral water samples.
一种采用 3-硝基苯甲醛缩硫代卡巴腙（3-NBT）作为络合剂的浊点萃取-ICP-OES 联用方法被开发出来，用于同时预浓缩和测定水样中的铜和汞。优化了影响络合和萃取步骤的变量。在最佳条件下（即 1.5×10(-5) mol L(-1) 配体，0.3%（v/v）Triton X-114，55°C 平衡温度，30 分钟孵育时间），Cu(2+)和 Hg(2+)的校准曲线在 5-120 和 10-100 ng mL(-1)范围内呈线性，增强因子分别为 82.7 和 51.3。两种情况下的预浓缩因子均为 28.6，检测限分别为 0.48 ng mL(-1) 和 1.1 ng mL(-1)。在 50 ng mL(-1)铜和汞的五个重复测定中，精密度（R.S.D.%）均优于 1.8%和 3.2%。该方法的准确性通过分析一种水的认证参考物质（RTC-QCI-049）得到了验证，结果令人满意。最后，该方法成功用于地表水（河流）、自来水和瓶装矿泉水样品中铜和汞的测定。
