Determination of rhenium in rhenium powder products prepared with ammonium rhenate by hydrogen reduction gravimetry
LI Kun,HE Xiao-tang,HAN Shou-li*,WANG Huan,ZHAO Yu,ZHANG Xuan-dong
State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Sino-Platium Metals Resources Yimen Co.,Ltd.,Sino-Platinum Metals Co.,Ltd.,Kunming 650106,China
Abstract：The total content of impurity elements in rhenium powder products is measured. Then the content of rhenium can be obtained by subtraction method. However, this method was complicated. During low temperature hydrogen reduction, besides of rhenium oxides (Re2O7 and ReO2), the coexisting metal impurities and their oxides will be also reduced to non-volatile metal elements, while nonmetal elements and their oxides as well as water and ammonium salt will be volatilized and removed. Based on this principle, the sample was treated by low temperature hydrogen reduction. The percentage of rhenium was calculated according to the mass ratio of sample before and after reduction. The determination method of rhenium in rhenium powder prepared with ammonium rhenate by hydrogen reduction gravimetry was established. The following experimental conditions were obtained: the sample mass was about 1.0 g; the hydrogen reduction was conducted in temperature-gradient mode (increased from room temperature to 200 ℃ and kept for 30 min, then increased to 400 ℃ and kept for 30 min, finally increased to 600 ℃ and kept for 30 min); the quartz boat containing rhenium powder after hydrogen reduction was cooled in dryer for 30 min (constant weight for one time). The experimental method was applicable for the determination of rhenium in rhenium powder (total mass fraction of non-volatile impurities was not more than 0.010%). The content of rhenium (99.824%-99.995%) in three management samples and four actual samples of rhenium powder was determined. The found results were consistent with the reference values. The relative standard deviations (RSD, n=9-22) were between 0.0012% and 0.003 3%, and the recoveries were between 99.99% and 100.01%.
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