Chand Vimlesh, Prasad Surendra
Division of Chemical Sciences, Faculty of Science and Technology, The University of the South Pacific, Suva, Fiji.
J Hazard Mater. 2009 Jun 15;165(1-3):780-8. doi: 10.1016/j.jhazmat.2008.10.076. Epub 2008 Oct 28.
A catalytic kinetic method is described for the determination of Se(IV), Se(VI) and total inorganic selenium in water based on the catalytic effect of Se(IV) on the reduction of bromate by hydrazine dihydrochloride in acidic media. The generated bromine decolorized methyl orange (MO) and the reaction was monitored spectrophotometrically at 507 nm as a function of time. The initial rate and fixed time methods were adopted for the determination and speciation of inorganic selenium. Under two optimum conditions, the calibration graphs are linear in the range 0-126.3 and 0-789.6 microg L(-1) of Se(IV) for the initial rate method and 0-315.8 and 0-789.6 microg L(-1) of Se(IV) for the fixed time method. The detection limits were 1.3 and 14.7 microg L(-1) for the initial rate and fixed time methods, respectively. The proposed methods were validated statistically and through recovery studies in environmental water samples. The relative standard deviation in the determination of 31.6-94.8 microg L(-1) of Se(IV) and Se(VI) was less than 6%. Analyses of standard reference materials for selenium using initial rate and fixed time methods showed that the proposed methods have good accuracy. Se(IV), Se(VI) and total inorganic selenium in environmental water samples have been successfully determined by this method after selective reduction of Se(VI) to Se(IV).
描述了一种催化动力学方法,用于测定水中的Se(IV)、Se(VI)和总无机硒,该方法基于在酸性介质中Se(IV)对盐酸肼还原溴酸盐的催化作用。生成的溴使甲基橙(MO)褪色,通过在507nm处分光光度法监测反应随时间的变化。采用初始速率法和固定时间法测定和分析无机硒的形态。在两种最佳条件下,初始速率法测定Se(IV)的校准曲线在0 - 126.3和0 - 789.6μg L(-1)范围内呈线性,固定时间法测定Se(IV)的校准曲线在0 - 315.8和0 - 789.6μg L(-1)范围内呈线性。初始速率法和固定时间法的检测限分别为1.3和14.7μg L(-1)。所提出的方法通过统计学验证并在环境水样的回收率研究中得到验证。测定31.6 - 94.8μg L(-1)的Se(IV)和Se(VI)时,相对标准偏差小于6%。使用初始速率法和固定时间法对硒标准参考物质进行分析表明,所提出的方法具有良好的准确性。通过将Se(VI)选择性还原为Se(IV)后,该方法已成功测定环境水样中的Se(IV)、Se(VI)和总无机硒。