Reduction in 1 M H(2)SO(4) with liquid zinc amalgam and extraction with isopentanol from 3M H(2)SO(4), separates rhenium from almost all the interfering elements of importance in rhenium determination. The small amounts of Mo, U, Fe and Ru still accompanying rhenium are removed by the thiocyanate-pentyl acetate or the oxine-chloroform extraction. The method is simple, rapid and of very wide applicability. It is particularly useful in the determination of rhenium in various alloys and tungsten-containing samples.