2-Acetylpyridine-4-methyl-3-thiosemicarbazone (APMT) gives yellow coloured water soluble complexes in aqueous medium with Coblt(II)and nickel(II) show maximum and constant absorbance in the pH range 5.0-80 respectively. The molar absorptivity and Sandell’s sensitivity of Co(II) (λmax 360) and Ni(II) (λmax 375 nm) are found to be 1.86 X 104 , 2.16 X 104 L mol-1 cm-1 and 3.2 X 10-3 , 3 X 10-3 μg cm-2 . Cobalt(II) and Nickel(II) form 1:2 complexes with APMT respectively. Second derivative spectrophotometric method has been developed and used for the determination of Co(II) and Ni(II) in alloys