Cuprammonium sulfate was prepared by an organic solvent method, in which NH3 content was determined by titration method on the measurement principle which was explained in the paper; Preparation of [ Cu (NH3 ) 4] SO4 crystals, NH3 content of 27.90%, and its results consistent with the theoretical value. Compared with traditional methods the new one had a zlightly measurement error, and a higher speed.%用有机溶剂法制备硫酸四氨合铜，再用返滴定法对NH3含量进行测定，阐述了该方法的测定原理；制备的[Cu（NH3）4]SO4．晶体中，NH3含量为27．90％，其结果与理论值基本吻合。与传统方法相比，新方法测定误差略高，但测量速度提高。
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