封管燃焼および検圧法を用いるデシミリグラム炭水素定量

概要

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Decimilligram determination of carbon and hydrogen with the sealed tube combustion method has been attempted using manometric finishes of CO2 and H2O produced in the combustion tube. In the method, organic sample is burned in a small sealed tube involving pure oxygen, copper net and Ag-Co2O3 catalyst as halogens- and sulfur-eliminator. The combustion tube is then partially broken in the manometric system which has been evacuated preliminarily so that the combustion gas diffuses towards the U-tube manometer as illustrated in Fig.1. Two freezing traps situated between the combustion tube and the U-tube temporarily retain the CO2 and H2O, while N2, if present, is swept out of the system through the vacuum pump. After the system has been closed, CO2 and H2O are evaporated in this sequence for the manometry. Operative conditions, e.g. viscosity of the manometer fluid, freezing and evaporation times, degree of vacuum and blank values due to the reagents in the combustion tube, have been optimized so that the standard deviations of σC=0.18% and σH=0.19% have been attained from a series of analytical data with several standard organic samples ranging 200500μg.
社団法人日本分析化学会の論文