Abstract：EDTA and tartaric acid were added in sample solution to eliminate the interference of coexisting ions, a large number of fluorine ions and sulfuric acid. In alkaline medium at pH 12-13, trichloromethane was added to extract tetraphenylarsonium thioperrhenate complex formed by tetraphenylarsonium chloride hydrochloride and rhenium. Then, hydrochloric acid (1+1) was used to re-extracted rhenium. Stannous chloride was added for reducing rhenium to rhenium, and potassium thiocyanate was added to react with rhenium to form potassium thiocyanate-rhenium orange yellow complex. Ethyl acetate was added to extract this complex and the solution was diluted to constant volume. Thus, a method was established for determination of rhenium in smelting waste acid of copper concentrate by potassium thiocyanate spectrophotometry. The results showed that the Beer's law was obeyed for rhenium in range of 0-50 μg/10 mL in 6 mol/L hydrochloric acid at wavelength of 430 nm. The correlation coefficient (R2) was 1.000 0. The detection limit of method was 1.59×10-6 μg/mL. The proposed method was applied to the determination of rhenium ranged from 4.0 to 16.0 mg/L in the synthetic samples of smelting waste acid of copper concentrate, and the results were consistent with the theoretical values. When the proposed method was applied to determine actual samples, the relative standard deviation (RSD, n=22) was 0.72%-2.2%, and the recoveries were between 99.8%-100%.
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