Abstract Wet chemical methods were used in combination with in situ infrared spectroscopy to identify and quantify soluble products formed during ethylene glycol electrochemical oxidation on platinum. A small volume electrolysis technique allowed reactions to be performed in samples of 150 μl in contact with a small, bead-type single crystal electrode. Following reaction, 50–100 μl aliquots were assayed for aldehydes and carboxylic acids. Glycolaldehyde (HOCH 2CHO), and glycolic (HOCH 2COOH) and oxalic ((HOOC) 2) acids were detected following the 360 s electrolysis of 0.2 M ethylene glycol in 0.1 M HClO 4 at potentials in the range 0.0–0.6 V (vs. SCE). Determination of the carboxylic acids by ion chromatography aided the assignment of carboxylate vibrational bands in in situ infrared spectra.