Elimination of the interference of molybdenum in determination of rhenium in raw potassium rhenate by thiourea spectrophotometry
ZHOU Yu1, TAN Yan-shan1, ZHU Li-ya 1, 2, NIU Chun-lin1, TANG Yun-zheng1, LI Yu-xian1, LI Mei-ju1, WAN Zhong-jian1, WANG Qian-hui1
1. Yunnan Copper Co., Ltd., Dali 675600, China; 2. State Key Laboratory of Advanced Technologies for Comprehensive Utilization of Platinum Metals,Sino Platinum Metals Resources Yi men Co., Ltd., Kunming 650106, China
Abstract：A method for selective determination of rhenium in raw potassium rhenate containing molybdenum was proposed by thiourea-rhenium(Ⅱ)-stannous chloride spectrophotometry after masking molybdenum with hydroxylamine hydrochloride-molybdenum (Ⅴ)-EDTA complex.The conditions for masking molybdenum with hydroxylamine hydrochloride-molybdenum (Ⅴ)-EDTA and the coloring conditions for thiourea-rhenium (Ⅱ)-stannous chloride were optimized. The results showed that, in weak hydrochloric acid, 3.0 mg of molybdenum could be masked with 4 mL of EDTA solution and 3 mL of hydroxylamine hydrochloride solution in water bath at 80 ℃ for 35 min. Moreover, the complexation masking system had no influence on the coloring complex. In 3.0 mol/L hydrochloric acid medium, the Beer’s law was obeyed for mass concentration of rhenium in range of 0-20 μg/mL at λ440 nm. The detection limit was 1.91×10-8 μg/mL. The proposed method was applied to the determination of rhenium (10%-20%) in raw potassium rhenate sample containing molybdenum (40%-50%). The relative standard deviation (RSD, n=7) was 0.15%-0.25%, and the recoveries were 100%.
周煜，谭艳山，朱利亚，牛春林，汤云正，李玉仙，李美菊，万仲建，王前会. 硫脲光度法测定粗铼酸钾中铼时钼干扰的消除[J]. 冶金分析, 2013, 33(9): 57-60.
ZHOU Yu, TAN Yan-shan, ZHU Li-ya, NIU Chun-lin, TANG Yun-zheng, LI Yu-xian, LI Mei-ju, WAN Zhong-jian, WANG Qian-hui. Elimination of the interference of molybdenum in determination of rhenium in raw potassium rhenate by thiourea spectrophotometry. , 2013, 33(9): 57-60.
