In recent years, many college and university instructors have introduced new experiments to revitalize the general chemistry curriculum and attract and retain students in the sciences. In particular, laboratory experiments using modern instrumentatal techniques, normally reserved for upper-level students, are becoming more widely adopted in the first-year course because modern instrumentation can be used to demonstrate theoretical concepts taught in the lecture. Many of these laboratory exercises involve spectroscopy, which is ubiquitous in all fields of chemistry. We describe here a spectroscopy experiment developed at Providence College in which students utilize IR and NMR spectroscopy to identify the structures of three unknowns from a list of 15 carefully chosen simple organic molecules. In taking IR and NMR spectra, students learn to use state-of-the-art instrumentation that is used by practicing chemists. The unknown determination provides a framework upon which students can practice their deductive reasoning skills, as they must think carefully about the three-dimensional structures of the molecules as they determine the identity of the unknowns. Students also have a chance to practice their writing skills as they logically present their rationale for their unknown determination. The use of modern instrumentation also communicates the excitement associated with chemistry laboratory work.