Mixed-ligand complexes of Cu(II), Ni(II), Co(II) and Zn(II) with 8-hydroxyquinoline and thiophene-2-carboxylic acid as two different ligands, have been isolated in pure state. The formation of these complexes has been inferred potentiometrically. The isolated complexes have been characterized by their elemental analyses, IR and electronic spectra, conductivity and magnetic measurements. Solid state dehydration of the hydrated complexes and sub-'sequent decomposition of the anhydrous complexes have been studied by simultaneous DTA and TG techniques. The thermal stability order of the hydrated compounds is Cu > Co > Ni > Zn, but in the decomposition process the trend observed is Co > Zn > Ni > Cu. Some parameters like activation energy and order of reaction for each process have been computed.Antifungal antibacterial properties of some mixed-ligand complexes of transition and inner-transition metal ions have been reported [1,2] in the literature. The compounds containing nitrogen and sulphur atoms play an important role in many process of biological importance [3]. 8-hydroxyquinoline and its derivatives have long been used as potential antimicrobiol agents and drugs [4,5]. The role of mixed-ligand complexes in biological process has well recognized [6]. In the present communication, synthesis, structural and thermal decomposition characteristics of the aforesaid mixedligand chelates have been discussed with a view to study their stability behaviour.