The reagent (S)-5-methoxy-2-[[(4-methoxy-3, 5-dimethyl-2-pyridinyle-methyle] sulfinyle]-1H-benzimidazole gives greenish yellow coloration with V (V) as well as Co (II) in basic medium. This observation is used for the simultaneous determination of both the metal ions using Zero and second order derivative spectrophotometry. Optimum conditions were established for this determination. Job’s and m...