Abstract：In the determination of tungsten in nickel base alloy by thiocyanate spectrophotometry, the high content of nickel would interfere with tungsten as nickel base alloy are usually difficult to dissolve. The samples were dissolved by the mixture of nitric acid-hydrofluoric acid, and nickel was separated from tungsten through producing nickelous hydroxide from nickel and sodium hydroxide. With stannous chloride as reductant, tungsten was reduced into yellow complex of tungsten and thiocyanate in the medium of hydrochloric acid. Thus, a thiocyanate spectrophotometric analysis of tungsten in nickel base alloy was established. The selection of the sample decomposition method and the method of eliminating the interference of the matrix element nickel were analyzed and discussed. The results showed that, Beer’s law was obeyed for tungsten within the range of 0.096-19.24 μg/mL, with the correlation coefficient of R2=0.999 6. The detection limit was 0.025%, while the low limit of determination was 0.084%. The proposed method had been applied to determine tungsten in two nickel base alloy. The relative standard deviation was (RSD,n=8) was less than 0.50%. The results of tungsten in six nickel base alloy samples were consistent with those of inductively coupled plasma atomic emission spectrometry(ICP-AES).
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