采用氢化物发生-原子荧光光谱法测定黄磷中微量砷,研究了样品消化方法以及仪器工作条件、还原剂等对测定的影响,确定了最佳试验条件.在最佳试验条件下,荧光强度与砷(Ⅲ)的质量浓度在0.06~10 μg·L-1范围内呈线性关系,相关系数为0.999 4,检出限为0.03 μg·L-1,样品分析结果的相对标准偏差小于3.5%,加标回收率在93.8%~103.6%之间.

Hydride generation-atomic fluorescence spectrometry was applied to the determination of arsenic in yellow phosphorus. Optimum condition of sample digestion,working condition of the instrument and suitable concentration of reductant were studied. Under the tested conditions of analysis,linear relationship between the fluorescence intensity and concentration of arsenic was found in the range from 0.06 to 10.0 μg·L-1 (r=0.999 4),with a detection limit of 0.03 μg·L-1. Five samples of yellow phosphorus were analyzed by the proposed method,giving values of RSD less than 3.5%. Recovery was tested and the results obtained were in the range of 93.8%-103.6%.