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Plant volatiles occupy diverse roles as signaling molecules, defensive compounds, hormones, and even waste products. Exponential growth in the related literature coupled with the availability of new analytical and computational technologies has inspired novel avenues of inquiry while giving researchers the tools to analyze the plant metabolome to an unprecedented level of detail. As availability of instrumentation and the need for qualitative and especially quantitative metabolic analysis grow within the scientific community so does the need for robust, adaptable, and widely disseminated protocols to enable rapid progression from experimental design to data analysis with minimal input toward method development. This protocol describes the collection and quantitative analysis of plant volatile headspace compounds. It is intended to guide those with little to no experience in analytical chemistry in the quantification of plant volatiles using gas chromatography coupled to mass spectrometry by describing procedures for calibrating and optimizing collection and analysis of these diverse compounds.