Bio-ferment residues (BR) are wastes produced by a biological fermentation process for the production of antibiotics. In this work, the evolution characteristics of pyrolysis products of BR were studied using TG-FTIR analysis and MS analysis. It was found that species such as H2O, NH3, CH4, carboxylic acid, aldehydes, alkanes, HCN, HNCO, CO, and CO2 were released at a temperature lower than 600A degrees C. Above 600A degrees C, the dominant products were H-2, CO, and CO2. Scarcely any acetylene or benzene was observed. HCN and HNCO were found to evolve in a small amount, while other potential pollutants such as H2S, COS, and CS2 were hardly detected.