A method was developed and tested to identify and measure volatile components generated from sweet-potato bread as it baked for the purpose of determining if hazardous chemicals identified by the National Space and Aeronautical Agency (NASA)’s maximum allowable concentrations list (SMACs) were present. A 14.5kL enclosed chamber made of polyethylene and polyvinylchloride was constructed to mimic conditions of a small enclosed food preparation space on board a NASA spacecraft. Volatiles generated from sweet-potato bread as it baked in a portable bread machine inside the enclosed chamber were extracted by thermal desorption tubes containing polydimethylsiloxane foam plugs and a portable pump. Tubes were thermally desorbed and components were analyzed by gas chromatography-mass spectrometry. Results indicated sweet-potato bread baked in a portable bread machine produced compounds identified as potentially hazardous including aliphatic alkanes, saturated C3-C8 aldehydes, ethanol, limonene, and furan containing components. The next step is to measure the concentrations of potentially hazardous compounds and determine if they exceed limits delineated by SMACs.