This manual introduces advanced chemistry students to a variety of techniques which are used in research, including the most useful instrumental analysis (NMR, capillary GC, and GC-MS). Experiments illustrate the power of modern instrumentation, particularly capillary GC and NMR. Interesting experiments require students to perform -detective work- and in the -Exploring Further- sections, students are encouraged to explore optional ideas for more in-depth and independent studies.