Analysis of whiskey samples prepared by a green microextraction technique, dispersive liquid-liquid microextraction (DLLME), before analysis by a qualitative gas chromatography-mass spectrometry (GC/MS) method, is described as a laboratory experiment for an upper division instrumental methods of analysis laboratory course. Here, aroma compounds in whiskey samples (n = 11) were extracted using ultrasound-assisted DLLME with chloroform (as extraction solvent). The chloroform extract was analyzed by GC/MS with data manipulation by AMDIS (automated mass spectral deconvolution and identification system) to allow for comparisons between whiskey samples. Aroma compounds commonly reported in the literature (furfural, isoamyl acetate, 5-methyl furfural, ethyl esters, phenylethyl alcohol, whiskeylactone, and vanillin) were tentatively identified based upon the match to the MS library. This unique laboratory allows students to engage in a real-world analysis of a high-value product and to explore the use of AMDIS to tentatively identify compounds and compare chromatographic profiles of various whiskey samples for identification of common and unique constituents. Students also use the literature to provide sensory information for these identified semivolatile compounds.