A new series of complexes of palladium(ll), oxovanadium(IV) and zinc(II) ions with N-(3,4-dihydroxy salicylidene)-3,5 -di(tert-butyl)-4-hydroxyaniline(HL) and N-(4,6-dihydroxy- salicylidene-3,5-di(tert-butyl)-4-hydroxyaniline (HL1) have been prepared and characterized by elemental analyses, electronic absorption spectral data, infrared, magnetic moment and molar conductance data. In order to determine the structures of the ligands with their palladium(ll) and zinc(il) complexes,H-1 and C-13 NMR spectra were obtained. All compounds were found to be non-electrolytes in DMSO (similar to 1 mM). The thermal behaviour of the ligands and their complexes have been investigated using thermogravimetric techniques (TG and DTA). The thermogravimetric data agree with the results of the analytical and spectral analyses. The degradation of the hydrated complexes occurs in several steps with the dehydration reaction followed by complete decomposition to the corresponding metal oxides.