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Oxo-vanadium (V) has been precipitated quantitatively from the solution in the pH range 3.5-6.5 with 2-hydroxy-5-chloro acetophenone oxime and determined by weighing the complex VO(OH) (C/sub 8/H/sub 7/CINO/sub 2/)/sub 2/ after drying at 110-120/sup 0/. The reagent has been used in the separation and gravimetric determination of vanadium (V) in its binary mixture with copper. The interference due to other ions has been avoided either using suitable masking agent or by working at controlled pH. I.R. spectral studies have also been carried out to assign a tentative structure to the complex.