Extraction behaviour of the chelates of group VB–VIIB and VIII elements using 1-(2-pyridylazo)-2-naphthol (PAN) has been studied as a function of pH. Studies have been made to back-extract the metal ions from the organic phase into the aqueous solution containing the optimum concentration of KCN and HClO4 and buffers of appropriate pH. The masking agents such as citrate, cyanide, thiosulphate, fluoride and thiourea were used to achieve more specific separations. The studies indicate the potentiality of PAN as a useful solvent extracting reagent in devising group chemical separation procedures for activation analysis.