Students sometimes have difficulty grasping the importance of when and how basic distillation techniques, column chromatography, TLC, and basic spectroscopy (IR and NMR) can be used to identify unknown compounds within a mixture. This two-part experiment uses mixtures of pleasant-smelling, readily available terpenoid compounds as unknowns to provide upper-division undergraduate students with experience in two major areas common to organic chemistry: (1) separation of mixtures and (2) structure determination. This experiment also encourages students to use deductive reasoning skills in addition to their expanding knowledge of spectroscopy for structure determination purposes.