Electrochemistry represents a powerful sustainable method for chemical synthesis; however, its widespread application is limited due to the lack of exposure and appropriate basic training of synthetic chemists and engineers in electrochemistry and electrochemical engineering. The introduction of diverse laboratory practices to the current curricula will improve the understanding of electrochemistry and the theory behind its various applications. Here, we suggest an efficient laboratory experiment on the electrochemical reduction of CO2 to CO using inexpensive and readily available materials, such as metal wires, plastic vessels, batteries, and a hand-held CO detector. Students learn to assemble a divided electrochemical cell and perform important electrochemical reactions, such as electrochemical CO2 reduction and hydrogen evolution reaction. In this experiment, students analyze the rates of CO production under different electrolysis conditions and learn to understand the effects of operating parameters (applied potential, electrolyte concentration, and nature of the electrode) on the outcome of the reaction. This new comprehensive laboratory experiment is designed for students to better understand basic principles of electrochemistry and is suitable for undergraduate students.