Chemistry Department, Faculty of Science, Tanta University, Tanta, Egypt.
Spectrochim Acta A Mol Biomol Spectrosc. 2012 Nov;97:284-9. doi: 10.1016/j.saa.2012.06.019. Epub 2012 Jun 17.
A simple, selective and sensitive spectrophotometric method for the determination of trace amounts of Zr(IV) in aqueous samples was performed, based on complexation reaction between Zr(IV) and 4-chloro-N-(2,6-dimethylphenyl)-2-hydroxy-5-sulfamoylbenzamide (xipamide). The important analytical parameters and their effects on the reported system were investigated. Zr(IV) react with xipamide in the ratio 1:1 in the pH range 8 to form a complex with an absorption maximum 333 nm. The apparent stability constant (logβ(n)) and the free energy change (ΔG) of formation of the complex was calculated using the results of mole ratio and continuous variation methods. Beer's law was obeyed in the concentration range 0.2-3.6 μg/mL. For more accurate analysis, Ringbom optimum concentration range was found from 0.3 to 3.5 μg/mL. The molar absorptivity, Sandell sensitivity, detection and quantification limits were also calculated. Taking a constant concentration of Zr(IV) and determining its concentration in the presence of large number of foreign ions tested the effect of foreign ions. The practical applicability of the elaborated method was examined using for determination of mentioned ion in water samples, biological, plant leaves and soil samples where excellent agreements between reported and obtained results were achieved. The relative standard deviation (n=6) were 0.195%. The precision and accuracy of the results were comparable via F and t test at the 95% confidence level.
基于 Zr(IV)与 4-氯-N-(2,6-二甲基苯基)-2-羟基-5-磺酰胺基苯甲酰胺(西普酰胺)之间的络合反应,建立了一种测定水样中痕量 Zr(IV)的简单、选择性和灵敏的分光光度法。研究了重要的分析参数及其对所报道体系的影响。Zr(IV)在 pH 8 范围内与西普酰胺以 1:1 的比例反应,形成一个在 333nm 处有最大吸收的络合物。使用摩尔比和连续变化方法的结果计算了络合物的表观稳定常数(logβ(n))和形成自由能变化(ΔG)。在 0.2-3.6μg/mL 的浓度范围内遵守比尔定律。为了更准确的分析,从 0.3 到 3.5μg/mL 范围内找到了里彭最佳浓度范围。还计算了摩尔吸光系数、桑德尔灵敏度、检测限和定量限。取一定浓度的 Zr(IV),在存在大量测试的外来离子的情况下测定其浓度,考察了外来离子的影响。该方法的实际适用性通过在水样、生物、植物叶片和土壤样品中测定上述离子进行了检验,获得了令人满意的结果。相对标准偏差(n=6)为 0.195%。通过 F 和 t 检验,在 95%置信水平下,结果的精密度和准确度相当。