It has previously been shown that the resistance of supercritical C02 Is too high for voltammetry, even with microelectrodes, unless electrolytes and/or polar modifiers are present In the fluid. In a supercritical fluid flow system, such as chromatography, the use of an added electrolyte Is not desirable. As an alternative, a film of an Ionically conducting polymer, Nafion, placed over an electrochemical probe consisting of both a microdisk working electrode and a quasireference electrode, has been used. Undlstorted voltammograms of ferrocene, 4-methylcatechol and 3,4-dlhydroxybenzylamlne dissolved In supercritical C02 In the presence of small quantities of H20 have been obtained without the use of added supporting electrolyte. Experiments carried out In a supercritical fluid flow stream demonstrate the potential utility of membrane coated microelectrodes as chromatographic detectors.