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目的建立了赶酸器浓缩-湿法消解-原子荧光法测定生活饮用水中硒的分析方法。方法水样于赶酸器上220℃加热浓缩,冷却后加入2.0ml HNO3+H2O2(1+1)混合溶液,220℃加热消解,冷却后加入6 mol/L盐酸2.5 m L,140℃继续加热至微沸,持续约5 min,以2.00%盐酸作为载流液,以15 g/L硼氢化钾溶液(含0.20%氢氧化钾)为还原剂,采用原子荧光法测定水中硒浓度。结果硒在1.0~20μg/L的线性范围内线性关系良好,所得回归方程为If=76.34c-7.74,r=0.999 9。该方法的检出限为0.033μg/L,平均回收率为96.5%~100.0%,RSD均小于2.0%。结论该方法操作简便,安全,快速,精密度、准确度均较高,适用于生活饮用水中痕量硒的测定。
OBJECTIVE To establish an analytical method for the determination of selenium in drinking water by concentration-digestion-wet digestion-atomic fluorescence spectrometry. Method The water samples were heated and concentrated on an acid catcher at 220 ° C. After cooling, 2.0 ml of HNO3 + H2O2 (1 + 1) mixed solution was added and digested at 220 ° C. After cooling, 2.5 ml of 6 mol / L hydrochloric acid was added and heating was continued at 140 ° C To slightly boiled for about 5 min. The concentration of selenium in water was determined by atomic fluorescence spectrometry with 2.00% hydrochloric acid as carrier fluid and 15 g / L potassium borohydride solution (containing 0.20% potassium hydroxide) as reducing agent. Results Selenium had a good linearity in the range of 1.0 ~ 20μg / L. The regression equation was obtained as If = 76.34c-7.74, r = 0.999 9. The detection limit of the method was 0.033μg / L, the average recovery was 96.5% ~ 100.0%, RSD were less than 2.0%. Conclusion The method is simple, safe, rapid, accurate and accurate. It is suitable for the determination of trace selenium in drinking water.