Al-Saidi H M, El-Shahawi M S
Department of Chemistry, University College, Umm Al-Qura University, Makkah, Saudi Arabia.
Department of Chemistry, Faculty of Science, King Abdulaziz University, P.O. Box 80203, Jeddah 21589, Saudi Arabia.
Spectrochim Acta A Mol Biomol Spectrosc. 2015 Mar 5;138:736-42. doi: 10.1016/j.saa.2014.11.050. Epub 2014 Dec 9.
A low cost and selective spectrofluorimetric method has been developed for trace determination of bromate ions in water. The method has been based upon complete extraction of the produced yellow colored ion associate of the reagent tetraphenylphosphonium iodide (TPP(+) I(-)) and bromate ions from aqueous media into chloroform and measuring the fluorescence quenching at λex/em=242/305nm. The composition, stability and the most probable mechanism of the produced associate have been determined. The plot of fluorescence intensity of TPP(+) I(-)vs. bromate concentration was linear in the range 0.86-150.0μgL(-1). The limits of detection (LOD) and quantification (LOQ) of BrO3(-) were 0.24 and 0.76μgL(-1), respectively. The method was found free from most of the interferences present in chromatographic, spectrofluorometric and spectrophotometric methods. Intra and inter-day laboratory accuracy and precision for analysis of bromate in water were determined. The method provides better performance compared to the international standard method recently issued (ISO 11206:2011). The method was applied satisfactorily for analysis of 1.0μgL(-1) bromate in the presence of high excess of chloride (50mg/L) without pretreatment with a relative standard deviation (RSD) of ±2.9%. The method was applied for analysis of bromate in various water samples. Statistical comparison of the results of the proposed method with those obtained by the standard method revealed no significant differences in the accuracy and precision.
已开发出一种低成本且具有选择性的荧光光谱法,用于水中痕量溴酸根离子的测定。该方法基于将试剂四苯基碘化鏻(TPP(+) I(-))与溴酸根离子生成的黄色离子缔合物从水介质中完全萃取至氯仿中,并在λex/em = 242/305nm处测量荧光猝灭。已确定了所生成缔合物的组成、稳定性及最可能的机理。TPP(+) I(-)的荧光强度与溴酸根浓度的曲线在0.86 - 150.0μgL(-1)范围内呈线性。BrO3(-)的检测限(LOD)和定量限(LOQ)分别为0.24和0.76μgL(-1)。该方法不受色谱法、荧光光谱法和分光光度法中存在的大多数干扰影响。测定了水中溴酸根分析的日内和日间实验室准确度及精密度。与最近发布的国际标准方法(ISO 11206:2011)相比,该方法具有更好的性能。该方法在存在高浓度过量氯离子(50mg/L)的情况下,无需预处理即可令人满意地用于分析1.0μgL(-1)的溴酸根,相对标准偏差(RSD)为±2.9%。该方法已应用于各种水样中溴酸根的分析。将该方法的结果与标准方法所得结果进行统计比较,结果表明在准确度和精密度方面无显著差异。