氢化物发生-原子荧光光谱法对水中总硒含量测试方法改进研究

Determination of Total Selenium in Water by Hydride Generation Atomic Fluorescence Spectrometry

为探寻简单可靠的水中硒测试方法,在采用国标中氢化物发生-原子荧光光谱法测定水样中的硒含量时,对影响水中硒消解的因素如消解温度和盐酸用量等进行了比较,并且确定了一种简易可行的新方法,即水样在100℃消解时加入3mL盐酸。采用3,6和10μg.L-1硒标液测定了方法的精密度和准确度,测试的结果分别是2.96,5.43和9.66μg.L-1,回收率在90.50%～98.67%。同时,用不同方法测试了29个水样中的硒含量,国标中氢化物发生-原子荧光光谱法测定水样中的硒含量的标样的误差为8.95%～25.46%,新方法测定标样的误差为1.33%～3.40%。新方法相对于中华人民共和国标准GB/T 5750.6-2006水中硒测试方法而言,具有操作过程简单、易控制和可靠性强、经济等特点。

In order to establish a rapid and accurate hydride generation-atomic fluorescence spectrometry method for the determination of selenium content in water samples,the influence factors on Se nitrolysis in the water such as nitrolysis temperature and the amount of hydrochloric acid were studied.The authors determined a simple and practical test method that is to add 3 mL hydrochloric acid at 3 ℃.We measured the precision and accuracy of the method by the standard liquid of 3,6 and 10 μg·L-1,and the test results were 2.96,5.43 and 9.66 mg·L-1.The recovery varied from 90.50% to 98.67%.Meanwhile we tested 29 water samples by different methods.The error of standard sample was 8.95%～25.46%by hydride generation-atomic fluoresence spectrometry in the GB/T 5750.6—2006,and the error of standard sample was 1.33%～3.40% by new method.Compared with the national standards of GB/T 5750.6—2006,the method has the advantages of operating simplicity and and easy control,and it is also reliable and economical.