This research deals with the quantitative formation of carbon dioxide in electrolytic oxidation reactions. The electrolytic reactions were run with barium peroxide to generate the superoxide anion at the anode. With the organic compounds used in these electrolytic studies we needed to develop a method where we could determine the amount of carbon dioxide liberated from these compounds with the superoxide anion. This method degasses an acidified solution with dry nitrogen, which carries the carbon dioxide to a standard solution of sodium hydroxide. Titration of the sodium hydroxide solution with standardized hydrochloric acid revealed the amount of carbon dioxide formed in the reaction after precipitation of the carbonate ions with barium chloride. Blank runs with the apparatus using anhydrous sodium carbonate produced 99% plus results of recovered carbon dioxide from the sodium carbonate.