Four new azo ligands, L1 and HL2-4, of sulfa drugs have been prepared and characterized. [MX(2)(L1)(H(2)O)(m)].nH(2)O; [(MX(2))(2)(HL2 or HL3)(H(2)O)(m)].nH(2)O and [M(2)X(3)(L4)(H(2)O)].nH(2)O; M=Co(II), Ni(II) and Cu(II) (X=Cl) and Zn(II) (X=AcO); m=0-4 and n=0-3, complexes were prepared. Elemental and thermal analyses (TGA and DTA), IR, solid reflectance spectra, magnetic moment and molar conductance measurements have accomplished characterization of the complexes. The IR data reveal that HL1 and HL2-3 ligands behave as a bidentate neutral ligands while HL4 ligand behaves as a bidentate monoionic ligand. They coordinated to the metal ions via the carbonyl O, enolic sulfonamide S(O)OH, pyrazole or thiazole N and azo N groups. The molar conductance data reveal that the chelates are non-electrolytes. From the solid reflectance spectra and magnetic moment data, the complexes were found to have octahedral, tetrahedral and square planar geometrical structures. The thermal behaviour of these chelates shows that the water molecules (hydrated and coordinated) and the anions are removed in a successive two steps followed immediately by decomposition of the ligand in the subsequent steps. The activation thermodynamic parameters, such as, E*, DeltaH*, DeltaS* and DeltaG* are calculated from the TG curves applying Coats-Redfern method.