This learning module is written to help undergraduate researchers to understand practical aspects of the operation of a capillary electrophoresis system and combines information about fundamentals of the method and standard construction and operation of a capillary electrophoresis instrument. The experiment may be accomplished with a commercial or custom-built capillary electrophoresis system. The first 21 steps of this learning module are a dry-lab, and therefore may completed without access to a capillary electrophoresis instrument. The last step requires a capillary electrophoresis separation and knits together the background information formulated in the dry lab to demonstrate the need for a practical understanding of the methodology. These experiments are outlined with recommended chemicals (tolmetin, atenolol, and mesityl oxide). The experiment may be completed with other compounds, and alternative chemicals are outlined in the instructor’s manual accompanying this material. Successful completion of Learning Module I requires you: (1) identify and name components of the system; (2) define and describe figures of merit that are frequently invoked in capillary electrophoresis; (3) document protocol for making standards and recording information in your notebook; and (4) formulate strategies for qualitative and quantitative analyses.