Abstract: Sample of ore or metallurgical slag was fused with Na2O2 at 700 ℃, the melt was leached with warm water, acidified with HCl and the solution was made up to a definite volume. An aliquot of the solution was taken and Be(Ⅱ) in it was reacted with beryllon Ⅲ to form a stable complex in an ammoniacal buffer medium containing EDTA, and a sensitive polarographic adsorption wave of this complex was observed at the potential of -0.80 V (vs.SCE). Linear relationship between values of 2nd derivative of peak current and mass concentration of Be(Ⅱ) was obtained in the range of 0.004-0.20 mg·L-1, with detection limit (3S/N) of 0.3 μg·L-1. The proposed method was applied to the analysis of seven samples of ores and metallurgical slags, giving results in consistency with the known values. Tests for recovery were made by standard addition method, giving values of recovery in the range of 96.0%-105% with RSD′s (n=6) in the range of 1.3%-9.7%.