Recently, the possibility of using a column of packed graphite as a thin-layer electrode was investigated by Polutanovich (1). This design is similar to the one presented by Voorhies (2) and to the one presented by Blaedel and Strohl (3). In this type of cell, electroactive material is electrolyzed within the column at a working electrode which is nonplanar and is of very large surface area. The effective solution thickness, 1, in the packed graphite electrolysis cell classifies this type of electrolysis as thin-layer as long as 12≪τD. In this study thin layer chronopotentiometry is used for the quantitative analysis of some organic compounds. A procedure for identifying organic electrolysis products is also presented. © 1969, American Chemical Society. All rights reserved.