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Abstract The thesis comprises three chapters. The first one concerend mainly with the literature survey on the structural and analytical chemistry of azo-pyrazolone compounds and their complexes. The second chapter is related to the experimental part. Syntheses of [3-amino-4-(substituted phenylazo)-5-(1H)pyra- zolones] ligands containing groups with different electronic characters (-H, p-OCHz, p-COOH, m-Cl, m-COOH, m-NO2, -CH3, m-OH and o-COOH) and their transition metals (Co, Ni, Cu and Pd) complexes are described. Different standardized instruments (UV-Vis, nmr, ir, ESR, magnetic susceptibilty, pH and conduc- tivity) are used. The preparation of the solutions (ligands, buffers and metal ions) and purification of solvents are explained. The results and their discussions are given in the third chapter. The 1H-NMR in d6-DMSO proved that all the ligands are predominating mainly in the enol form. The KBr- IR of 3-amino-5-(1H)pyrazolone and their m-COOH, p-COOH azo compounds proved their existence in dimeric structures mainly in the keto skeleton. This structure is not presented for the o-COOH azo derivative. The effect of pH on the electronic spectra of the ligands assigned the electronic transitions (mainlyn- and π) and to explain the mode of ioniz ation (through the evaluation of pk values). Two sets of pK’s. |