Department of Chemistry, University of Jabalpur, Jabalpur Manuscript received 1 October 1973; accepted 13 February 1974 A procedure has been described for the determination of some simple organic compounds by oxidation with potassium diperiodato and ditellurato cuprate (III). Samples were treated at 30° to 100°, in alkaline medium with an excess of the oxidant, which was back estimated after completion of reaction, by titration with a standard solution of arsenite. The results are precise to about 0.5%. An adverse effect of high alkalinity, on the stability of the reagent, has also been demonstrated.