This learning module is written for undergraduate chemistry researchers who are already familiar with fundamentals of separation mechanisms, separation efficiency and figures of merit, as well as basic aspects of operation of a capillary electrophoresis system including sample introduction, the development of operating protocol, and anticipation of experimental outcome. These concepts are covered in Learning Modules I and II. The experiment outlined in this Module may be completed using a commercial or custom-built capillary electrophoresis instrument. The first 2 steps of this learning module require the user to describe fundamentals of MEKC separations. Step 3 requires the user to formulate protocol for quantitative and qualitative analysis by MEKC. The last step (4) requires the user to perform triplicate MEKC separations using set run conditions. This exercise outlined in step 4 provides the user an opportunity to apply her or his laboratory skill and knowledge of the operation of MEKC. The experiment outlined here is performed with recommended chemicals (tolmetin, dimethylformamide). 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 III assists the user in acquiring the skills necessary for a new practitioner of MEKC.