Metilda P, Sanghamitra K, Mary Gladis J, Naidu G R K, Prasada Rao T
Inorganic and Analytical Chemistry, Regional Research Laboratory (CSIR), Industrial Estate P.O., Trivandrum 695019, India.
Talanta. 2005 Jan 15;65(1):192-200. doi: 10.1016/j.talanta.2004.06.005.
Amberlite XAD-4 resin has been functionalized with succinic acid by coupling it with dibromosuccinic acid after acetylation. The resulting resin has been characterized by FT-IR, elemental analysis and TGA and has been used for preconcentrative separation of uranium(VI) from host of other inorganic species prior to its determination by spectrophotometry. The optimum pH value for quantitative sorption of uranium(VI) in both batch and column modes is 4.5-8.0 and desorption can be achieved by using 5.0ml of 1.0moll(-1) HCl. The sorption capacity of functionalized resin is 12.3mgg(-1). Calibration graphs were rectilinear over the uranium(VI) concentrations in the range 5-200mugl(-1). Five replicate determinations of 50mug of uranium(VI) present in 1000ml of solution gave a mean absorbance of 0.10 with a relative standard deviation of 2.56%. The detection limit corresponding to three times the standard deviation of the blank was found to be 2mugl(-1). Various cationic and anionic species at 200-fold amounts do not interfere during the preconcentration of 5.0mug of uranium(VI) present in 1000ml (batch) or 100ml (column) of sample solution. Further, adsorption kinetic and isotherm studies were also carried out by a batch method to understand the nature of sorption of uranium(VI) with the succinic acid functionalized resin. The accuracy of the developed solid phase extractive preconcentration method in conjunction with Arsenazo III procedure was tested by analyzing marine sediment (MESS-3) and soil (IAEA soil-7) reference material. Further, the above procedure has been successfully employed for the analysis of soil and sediment samples.
Amberlite XAD - 4树脂经乙酰化后与二溴琥珀酸偶联，从而用琥珀酸进行功能化处理。所得树脂通过傅里叶变换红外光谱（FT - IR）、元素分析和热重分析（TGA）进行了表征，并用于在分光光度法测定之前从许多其他无机物种中对铀（VI）进行预富集分离。在分批和柱模式下，铀（VI）定量吸附的最佳pH值为4.5 - 8.0，使用5.0ml 1.0mol l⁻¹盐酸可实现解吸。功能化树脂的吸附容量为12.3mg g⁻¹。校准曲线在铀（VI）浓度5 - 200μg l⁻¹范围内呈线性。对1000ml溶液中存在的50μg铀（VI）进行五次重复测定，平均吸光度为0.10，相对标准偏差为2.56%。发现对应于空白标准偏差三倍的检测限为2μg l⁻¹。在1000ml（分批）或100ml（柱）样品溶液中对5.0μg铀（VI）进行预富集时，200倍量的各种阳离子和阴离子物种均不产生干扰。此外，还通过分批法进行了吸附动力学和等温线研究，以了解铀（VI）与琥珀酸功能化树脂的吸附性质。通过分析海洋沉积物（MESS - 3）和土壤（IAEA土壤 - 7）标准物质，测试了所开发的固相萃取预富集方法与偶氮胂III程序结合的准确性。此外，上述程序已成功用于土壤和沉积物样品的分析。
