【摘要】 取10.00 mL水样,于60～70℃加热蒸发至近干,加入硝酸-高氯酸（1+1）混合酸2.0mL,继续加热至白烟冒尽,加入盐酸2.0 mL,摇匀,加热保持微沸3～5 min,冷却后转移至10mL比色管中,用去离子水定容,使用氢化物发生-原子荧光光谱仪测定总硒的含量。另取10.00mL水样,加入盐酸2.0mL,于60～70℃加热至溶液体积小于5mL,转移至10mL比色管中,用去离子水定容,使用氢化物发生-原子荧光光谱仪测定无机硒（即四价硒和六价硒的总和）的含量。另取水样5.00mL于10mL比色管中,加入盐酸2.0mL,用去离子水定容,使用氢化物发生-原子荧光光谱仪测定四价硒的含量。用总硒含量减去无机硒含量即为有机硒含量,无机硒含量减去四价硒含量即为六价硒含量。在最佳仪器工作条件下,硒的质量浓度在1.00～20.0μg·L^-1内与其对应的荧光强度呈线性关系,硒的检出限（3s）和测定下限（10s）分别为0.11,0.36μg·L^-1。采用本方法测定某地区水中的总硒、无机硒和四价硒,加标回收率在95.7%～104%之间,相对标准偏差（n=6）在1.9%～3.2%之间。采用本方法测定了不同地区水中的总硒、无机硒和四价硒,利用差减法计算得有机硒和六价硒的含量。更多还原

【Abstract】 10.00 mL of water sample were taken and heated to evaporate to near dry at 60-70℃,2.0 mL of mixed acid of nitric acid and perchloric acid（1+1）were added,and the mixture was heated until white smoke was exhausted.After 2.0 mL of hydrochloric acid was added,the mixture was shaked well and heated to keep slight boiling for 3-5 minutes.After cooling,the solution was transferred to a colorimetric tube and made up to 10.00 mL with deionized water.The total selenium content was determined by hydride generation-atomic fluorescence spectrometry.Another 10.00 mL of water sample were taken,and 2.0 mL of hydrochloric acid were added.After the mixture was heated at 60-70℃ until the solution volume were less than 5 mL,the solution was transferred to a colorimetric tube and made up to 10.00 mL with deionized water.The content of inorganic selenium（the sum of tetravalent selenium and hexavalent selenium） was determined by hydride generation-atomic fluorescence spectrometry.Another 5.00 mL of water sample was taken into a 10 mL colorimetric tube,2.0 mL of hydrochloric acid was added,and the volume was made up to 10.00 mL with deionized water to determine the content of tetravalent selenium by hydride generation-atomic fluorescence spectrometry.The total selenium content minus the inorganic selenium content was the organic selenium content,and the inorganic selenium content minus the tetravalent selenium content was the hexavalent selenium content.Under the optimal working conditions of the instrument,the mass concentration of selenium was linearly related to the corresponding fluorescence intensity in the range of 1.00-20.0μg·L^-1.The detection limit（3 s）and the lower limit of determination（10 s）of selenium were 0.11,0.36μg·L^-1,respectively.The method was applied to determination of total selenium,inorganic selenium and tetravalent selenium in water of an area,giving recovery obtained by standard addition method between95.7% and 104%,and RSDs（n=6）in the range of 1.9%-3.2%.The total selenium,inorganic selenium and tetravalent selenium in water from different regions were determined by this method,and the contents of organic selenium and hexavalent selenium were obtained by calculating with subtraction method.更多还原