金属中の微量炭素定量における湿式酸化分解-非水溶媒電量滴定法の改良(湿式化学分析)(<特集>分析評価・解析)

概要

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When metal samples are decomposed with mixture solution of potassium dichromate and sulfuric acid, there are a lot of chances to have serious explosions because of the reaction between the hydrogen gas generated and the oxygen gas used as carrier gas. The assembly was developed for evacuating to remove the hydrogen with a vacuum pump through a palladium membrane heated at 400℃ in order to avoid such a dangerous phenomenon. The wet chemical apparatus installed the newly developed assembly was used for the determination of traces of carbon in two kinds of high-purity iron, steels, aluminum and high-purity indium samples. Since the evolved hydrogen could be thoroughly removed from the train, the detonation was never encountered in the determination. The formed carbon dioxide was titrated coulometrically in nonaqueous medium, with a photometric end-point detection. Trace amounts of carbon [(0.4∿252 ppm (m/m)] in the metal samples could be determined in safety and with good precision and accuracy. The fluctuation of the blank value was little all through the experiment. The time taken to a single determination was 25 to 155 min.
社団法人日本鉄鋼協会の論文
1991-11-01