In order to analyze the C-14 inventory and leaching rate for safety evaluation of transuranic waste disposal, it is necessary to establish an analytical method that can measure C-14 with sufficient precision . Oxidative decomposition of organic compounds containing C-14 is carried out to absorb carbon dioxide (CO2) in an alkaline solution, which is mixed with a liquid scintillation cocktail, and the amount C-14 is quantified by measuring a beta ray spectrum with a liquid scintillation counter. It has been difficult to completely decompose carbon compounds in a sample, even to CO2, by using conventional oxidizing agents. In the work described here, we improved the method of oxidative decomposition used to completely decompose carbon compounds using peroxydisulfuric acid (K2S2O8). When C-14 in the form of CO2 was absorbed in a sodium hydroxide (NaOH) aqueous solution, only 80% of the actually used quantity was detected. Total organic carbon measurements showed that the entire quantity of CO2 was absorbed by NaOH. When NaOH aqueous solution was used, it was found that only the analytical value was 80%. The entire quantity of the actually used carbon could be measured by absorbing the CO2 in Carbo-Sorb®. An anion form and a neutral molecule exist in the organic compound released from activated metals. In order to identify organic compounds efficiently, fractionation into an anion and a neutral molecule and separation by high performance liquid chromatography (HPLC) are necessary. Here, we propose the combined use of an ion exchange resin and HPLC as an improved technique for identification of the chemical species.