A wetting agent used to control foaming in the Chemical Processing Cell at the Defense Waste Processing Facility degrades to form compounds that could volatilize to form vapor exceeding the lower flammability limit. Three identified components of concern were hexamethyl disiloxane, trimethyl silanol, and propanal. Analytical methods were developed and implemented on a real waste sample to monitor degradation products. Using standards, an extraction method with dichloromethane and analysis by gas chromatography-mass spectrometry and hydrogen nuclear magnetic resonance was developed. Both methods had detection limits less than 1mg/L for the analytes.