Determination of rhenium in raw rhenium compounds by tetraphenylarsonium hydrochloride gravimetry
GUO Jun-mei, LI Kun, HE Xiao-tang, XIONG Qing-feng ZHENG Yun, ZHANG Xuan-dong
State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Sino Platinum Metals Resources Yi men Co., Ltd., Kunming 650106, China
Abstract：Raw rhenium compounds were the intermediate products of rhenium recovered from spent platinum-rhenium catalyst by new technology of hydrometallurgy, including perrhenic acid, potassium rhenate and ammonium rhenate. The accurate determination of rhenium content was required in production process.The perrhenic acid, potassium rhenate and ammonium rhenate sample containing about 100 mg of rhenium was transferred into beaker, respectively. After adding water to 50 mL, the solution was heated to dissolve the sample. Then, 0.2 mL of hydrogen peroxide was added to oxidize rhenium to rhenium, which was precipitated by adding 5 mL of EDTA solution for masking the interference ions, 45 mL of ammonia water and 10 mL of tetraphenylarsonium hydrochloride solution. The precipitate was dried in oven at 110 ℃ for 1 h to remove the moisture until constant weight. The determination method of rhenium in raw rhenium compounds including perrhenic acid, potassium rhenate and ammonium rhenate by tetraphenylarsonium hydrochloride gravimetry was established. The experimental results showed that rhenium could be fully precipitated by tetraphenylarsonium hydrochloride under selected conditions. Twenty coexisting ions such as platinum did not interfere with the determination. The proposed method was applied to the determination of rhenium (45.30-84.34 g/L, 40.93%-69.42%) in three control samples and six actual samples. The found results were basically consistent with the reference values. The relative standard deviations (RSD, n=7-11) were between 0.023% and 0.085%. The recoveries were between 99.8% and 100.1%.
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