Odors from livestock operations are a complex mixture of volatile carbon, sulfur, and nitrogen compounds. Currently, detailed volatiles analysis is both time consuming and requires specialized equipment and methods. This work describes a new method that utilizes a dynamic flux chamber, solid-phase microextraction (SPME), and gas chromatography-mass spectroscopy (GC-MS) to describe and compare the odorous compounds emitted from cattle and swine feces. Evaluation of method parameters produced a protocol for comparing relative emissions based on fixed sample temperature (20 degrees C) and exposed surface area (approximately 523 cm(2)), air flow rates (1 L min(-1) or 16 cm s(-1)), SPME exposure time (5 min), and chamber cleaning procedures (70% ethanol rinse and drying for 30 min at 105 degrees C) to minimize cross-contamination between samples. A variety of volatile organic compounds (VOCs) including alcohols, volatile fatty acids, aromatic ring compounds, ketones, esters, and sulfides were routinely detected and the relative emissions from fresh and incubated (37 degrees C overnight) swine and cattle feces were compared as a measure of potential to produce odorants during manure storage. Differences in the types and relative quantities of volatiles emitted were detected when animal species (cattle or swine), diet, fecal incubation, or sample storage conditions (20, 4, or -20 degrees C) were varied.