Characterization and quantification of livestock odorants is one of the most challenging analytical tasks because odor-causing gases are very reactive, polar and often present at very low concentrations in a complex matrix of less important or irrelevant gases. The objectives of this research is to develop a novel analytical method for characterization of the livestock odorants including their odor character, odor intensity, and hedonic tone and further quantitative analysis of the key odorants responsible for livestock odor emissions. Sorbent tubes packed with Tenax TA were employed for sampling. The automated one-step thermal desorption coupled with multidimensional gas chromatography-mass spectrometry-olfactometry system was developed for simultaneous chemical and odor analysis. Fifteen odorants identified from different livestock species operations are quantified. In addition, odor character, odor intensity and hedonic tone associated with each of the target compounds are also analyzed. The method developed in this research is being used on a multistate, multispecies project focused on quantifying odor and chemical analysis of odor.