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The organic matter (OM) of a green waste and bio waste compost was characterised over 8months and the observed evolution was correlated with physico-chemical parameters (temperature, pH, carbon content, C/N ratio). Thermochemolysis and thermodesorption were used to monitor bacterial activity (stability) whereas diffuse reflectance infrared fourier transform spectroscopy (DRIFTS) and thermodifferential analysis (TDA) permitted to determine the degree of OM humification (maturity). DRIFT spectroscopy and TDA provide two indicators of maturity since, with these two techniques, the signals associated with the biodegradable organic matter decrease relatively to the signals associated with refractory organic matter. This increase in R(TG) and R(IR) ratios between aromatic to aliphatic signals constitutes a proof for OM complexification. It correlates with humic acids/fulvic acids ratio known to be a maturity index. Pyrolysates are mainly constituted of lignin moieties, terpenoids, nitrogen containing compounds, carbohydrates (furanosic moiety), mono- and diacids (as methyl esters), and methoxyesters. The R(branched/linear) ratio between branched to linear acids traduces the evolution of the bacterial activity during composting. Moreover the R(di/mono) ratio between aliphatic mono to diacids correlates with the latter showing that diacids can occur from the biological oxidation of monoacids. These two ratios determined by thermochemolysis are useful to monitor the stability of compost. VOC, observed by thermodesorption are mainly constituted of terpenes, light acids, aldehydes and ketone. An unexpected result was obtained since the amount of phytol increases relatively to the isoprenoid ketone considered to originate from the latter.