The copper, nickel, palladium and vanadium complexes of tetradentate ligand bis(salicylaldehyde)tetramethylethylenediimine(H2SA2Ten) are prepared and their DTA and TGA are recorded. Nickel complex indicates reasonable volatility and thermal stability with loss in weight upto 98.7%, but copper, palladium and vanadium complexes leave significant residue behind with loss in weight in the range from room temperature to 500-degrees-C. The metal complexes elute on GLC column (6' x 0.085) packed with OV101, 3% on Chromosorb WHP 80-100 size with detection limits at sub-mu-g level of metal complexes and complete separation palladium from copper, nickel and vanadium complexes. The spectrophotometric studies of metal complexes indicate reasonable sensitivity within UV region and their adsorption HPLC column (250 x 4 mm) packed with Licrosorb Si100, 5-mu, connected with UV detector demonstrated complexes. The complexes were eluted isocratically with binary mixture of chloroform 1,2-di-chlorethane and detection limits were found at sub ng levels of metal complexes. The reagent has been applied for the determination of nickel in nickel-aluminium alloy using both GLC and adsorption HPLC. The result agree to each other and the expected value.