The overall research goal is to develop in situ scanning electrochemical microscopy (SECM) to improve the microscopic understanding of how gas bubbles nucleate, form, grow, and migrate at solid–liquid interfaces. An important subset of gas-involving or gas-evolving, interfacial electrochemical reactions produces gas molecules dissolved in solution that can nucleate as small nanobubbles on electrode surfaces. These bubbles can grow to macroscopic sizes and interfere with chemical processes by blocking reactants from reaching the electrode-electrolyte interface, or by increasing turbulent mixing via leaving the surface. SECM is used to map the bubble formation mechanisms on the interface and to quantify the chemical species (reactant and product) concentration profile within the diffusion layer of the electrode surface. Here we will use oxygen reduction reaction (ORR) to hydrogen peroxide and nitrate reduction reaction (NO3RR) to ammonium as two model systems to investigate how SECM could help us understand chemical reaction mechanisms at aqueous electrochemical interfaces.