A small-volume (∼60 μl) spectroelectrochemical cell was constructed and characterized.The working electrode is An minigrid, and the spectral window is from 170 nm to 2 μm. The solution is held in a thin layer around the working electrode, providing the advantages of thin-layer electrochemistry. The cell can be constructed from common materials in about 6-h working time. The cell also has flow-through and vacuum capabilities, with only minor modifications. Characterization of the cell was done by cyclic voltammetry and coulometry on ferri-ferrocyanide and spectroelectrochemistry on cytochrome c and o-tolidine. The optical and electrochemical windows of this cell, as well as its convenient and versatile operation, make it useful for the study of a wide variety of biological redox components. © 1979 Academic Press, Inc.