Gas Chromatography/Mass Spectrometry (GC/MS) gives the chemist a powerful tool for analyzing mixtures of compounds and monitoring reactions as they progress. The use of GC/MS in the undergraduate laboratory gives students experience with current instrumental methods for molecular analysis and demonstrates, by experiment, the concepts of sample preparation, data acquisition, and data manipulation. This ILI award from the Chemistry Shared Instrumentation Program will help the Department of Chemistry at Virginia Commonwealth University to acquire GC/MS instrumentation that will be used to enhance undergraduate laboratory instruction.