Abstract:This paper establishes a new method for the determination of rhenium in ammonium rhenate,determines electrolysis current, electrolyte composition and content, electrolyte temperature, stirring speed and electrolysis time as the optimum experimental conditions. The optimum experimental conditions is room temperature, no stirring, 4.0 a current, (1+368) sulfuric acid solution, 20 g/L ammonium sulfate solution and electrolysis time of 7.6 hours. The interference test shows that that the influence of lead, arsenic, mercury and iron on the electrodeposition of rhenium is negligible,and the influence of copper can be eliminated by impurity removal. The method has been applied to the determination of rhenium in ammonium rhenate samples. The results are in good agreement with those of tetraphenylarsine hydrochloride gravimetric method. The relative standard deviation (RSD, n = 5) is less than 0.14%, and the recovery is 99.2% - 102%.The method is accurate and reliable, which meets the requirements of daily analysis.