The complexes of thiosemicarbazide (HTS) have been prepared and characterized by spectral, thermal and magnetic studies. The deprotonation constant of HTS and the formation constants of its complexes were evaluated pH-metrically. The Cu(II) acetate-HTS system gave high stability. The catalytic activity of Co(II), Ni(II) and Cu(II) complexes was tested to decompose H 2 O 2 . The Co(II) complex has no activity whereas the Cu(II) complex was found to be more active than Ni(II). The different Cu(II) complexes were tested; [Cu 2 (TS)(OH) 2 (OAc)] was highly active. All parameters affecting the reaction rate (concentration of H 2 O 2 , weight of catalyst, temperature and pH) were studied and the optimum conditions were evaluated. Attempts to increase the activity of [Cu 2 (TS)(HO) 2 (OAc)] by mixing with superconducting cuprate sample, Nd 0.1 Y 0.9 Ba 2-Cu 3 O 7-d , will be the subject of further studies.