The design of a versatile, thin-layer cell to perform in situ spectroelectrochemistry is discussed. The cell is lowvolume, leak-tight, and easily disassembled. It is constructed of chemically resistant materials and can be used to probe the electrochemical reactions of corrosives as well as moisture-and air-sensitive materials. The use of this cell to monitor the electrochemical reactions of oxyhalide electrolytes by in situ infrared spectroelectrochemistry and pyridine by surface-enhanced Raman scattering spectroscopy is demonstrated.