The report deals with the detection and quantitation of acrylonitrile, vinylidene chloride, and vinyl bromide, which are used as monomers in the production of acrylic and modacrylic fibers. The amounts of monomers evolved from samples of carpets, fibers, and fabrics at 50C and 50% relative humidity were determined by gas chromatography with a flame ionization detector and by direct insertion probe mass spectroscopy. The results of the gas chromatographic studies indicate that detectable amounts of residual acrylonitrile, vinylidene chloride, and vinyl bromide were not released from the carpet, fiber, and fiber samples under the conditions selected for analysis. Direct insertion mass spectrometry indicated that methyl bromide was evolved from all of the fiber samples and from two of the three carpet samples. From the remaining carpet sample, three halogenated compounds--dibromo-dichloroethanol, tetrabromoethanol, and tribromochloroethanol--were identified. Traces of fatty acids were found in all of the samples, and sulfur dioxide was evolved from all of the samples except the fabric sample.