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目的建立微波消解-氢化物发生原子荧光法测定生活饮用水中硒的分析方法。方法以智能样品处理器对水样进行前处理,对加热参数、仪器条件、还原剂浓度、载流浓度和铁氰化钾掩蔽效果等试验条件进行研究和优化;在最佳条件下,采用原子荧光法进行测定。结果硒标准曲线的回归方程为If=78.72ρ+9.244,方法的检出限为0.033μg/L,在0~20μg/L范围内线性关系良好,相关系数r=0.999 6。方法加标回收率为95.0%~99.0%,相对标准偏差(RSD)为0.8%~1.5%。结论该方法操作简便,安全,快速,精密度、准确度较高,适用于生活饮用水中微量硒的测定。
Objective To establish a method for the determination of selenium in drinking water by microwave digestion - hydride generation atomic fluorescence spectrometry. Methods The samples were pretreated with an intelligent sample processor to study and optimize the experimental conditions such as heating parameters, instrument conditions, concentration of reducing agent, carrier concentration and masking effect of potassium ferricyanide. Under the optimal conditions, Fluorescence assay. Results The regression equation of selenium standard curve was If = 78.72ρ + 9.244. The detection limit was 0.033μg / L. The linearity was good in the range of 0 ~ 20μg / L with the correlation coefficient r = 0.999 6. The recoveries were 95.0% ~ 99.0% with relative standard deviations (RSDs) of 0.8% ~ 1.5%. Conclusion The method is simple, safe, rapid, accurate and accurate. It is suitable for the determination of trace selenium in drinking water.