在计算机上运用自编程序绘出苯胺的三维荧光光谱，确定苯胺的特征荧光峰，提出了三维荧光光谱法测定苯胺的分析方法。苯胺浓度在２．０×１０－７－５．０×１０－６ｍｏｌ／Ｌ范围内与相对荧光强度呈良好的线性关系。该法相对标准偏差为２．５％，检出限为１．０×１０－７ｍｏｌ／Ｌ。用于工业废水中苯胺的测定，结果令人满意。 In the computer, a self-programmed program was used to draw the three-dimensional fluorescence spectrum of aniline, and the characteristic fluorescence peak of aniline was determined. An analytical method of three-dimensional fluorescence spectrometry for the determination of aniline was proposed. The aniline concentration in the range of 2.0 × 10-7-5.0 × 10-6mol / L showed a good linear relationship with the relative fluorescence intensity. The relative standard deviation of the method was 2.5%, the detection limit was 1.0 × 10-7mol / L. For the determination of aniline in industrial wastewater, the results are satisfactory.