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Study of thermal decompositions of cotton and flame-retardant cotton fabrics can assist understanding of fire-resistant functions of the materials. In this research, differential scanning calorimeter (DSC), thermogravimetric analysis (TGA) and pyrolysis–gas chromatography–mass spectroscopy (PY–GC–MS) were employed to investigate decomposition processes and decomposed products of flame-retardant treated (using an organo-phosphorus compound) and untreated cotton fibers in the pyrolysis. The thermal decomposition temperatures, weight losses and potential reactions of the pyrolysis as well as resulted fragments, were analyzed. The results are helpful in understanding of mechanisms of flame-retardant cotton fabrics.