Biodiesel is an important alternative fuel synthesized by the trans-esterification of vegetable oils, animal fats, and recycled greases. In this experiment, students prepared biodiesel through the base-catalyzed trans-esterification of several vegetable oils, which were subsequently analyzed in comparison with conventional petroleum-based fuels to assess their physical properties and to obtain a thermochemical profile. The experiment as described here could be employed by university faculty as a project in a major's level laboratory course, but we envision the ideal fit to be a module within an advanced or integrated laboratory course. Students completing the project gain valuable experience in chemical synthesis and in extensive product characterization and analysis. This project reinforces critical skills in isolation of pure products from complex mixtures and in the careful preparation of samples for chemical analysis. Finally, students are afforded the opportunity to compare theoretical predictions from chemical modeling in combination with GC-MS analysis with the practical results gained by performing bomb calorimetry.