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The first part of this study concerns the characterization of organic matter transformation during olive mill wastes composting by monitoring different physico-chemical parameters (temperature, C/N ratio, moisture, ash, pH, lipids, fiber, total polyphenols), biological parameters (germination test), humification parameters (humic substance contents and humification index) and spectroscopic analysis (FTIR). The obtained results permit to highlight the optimal conditions of olive mill wastes composting. The second part of this work concerns the study and the characterization of humic substances (humic and fulvic acids), during composting, by complementary analyses (Gel Sephadex Chromatography, Fourier Transform InfraRed (FTIR), 13 Carbon-Nuclear Magnetic Resonance(13C-NMR), Fluorescence and Differential Calorimetry). The whole humic and fulvic characteristics, during olive mill wastes composting, shows that the nature of these acids is young, so they can be listed among the IIIrd class of soil humic and fulvic acids.