A full-scale composting plant treating in two parallel lines sewage sludge and the source-selected organic fraction of municipal solid waste (OFMSW or biowaste) has been completely monitored. Chemical routine analysis proved not to be suitable for an adequate plant monitoring in terms of stabilization and characterization of the process and final compost properties. However, the dynamic respiration index demonstrated to be the most feasible tool to determine the progression of the degradation and stabilization of organic matter for both sewage sludge and OFMSW lines. Both lines exhibited an important degree of stabilization of organic matter using rapid and cumulative respiration indices. Pyrolysis-GC/MS was applied to the most important inputs, outputs, and intermediate points of the plant It proved to be a powerful tool for the qualitative characterization of molecular composition of organic matter present in solid samples. A full characterization of the samples considered is also presented. (C) 2010 Elsevier Ltd. All rights reserved.