电解-电感耦合等离子体原子发射光谱(ICP-AES)法测定铼酸铵中铼

建立了一种测定铼酸铵中铼主品位含量的全新检测方法。确定了电解电流、电解液成分和含量、电解液温度、搅拌速度、电解时间等最佳实验条件,即:在室温、不搅拌、4.0 A电流、5 g/L硫酸溶液、20 g/L硫酸铵溶液和电解时间为7.6 h条件下进行检测。干扰实验表明,铼酸铵样品中铅、砷、汞、铁等共存元素对铼的电解沉积影响可忽略;铜的影响可通过扣杂的方式予以消除。将实验方法用于铼酸铵实际样品中铼的测定,测得结果与四苯砷氯盐酸盐重量法基本一致,相对标准偏差(RSD,n=5)小于0.14%,回收率为99.2%~102%。方法准确、可靠,能满足日常分析要求。

Determinnation of Rhenium Content in Ammonium Rhenate by Electrolysis and Inductively Coupled Plasma Atomic Emission Spectroscopy

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.