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A simple method is described for the microdetermination of deuterium in organic compounds. It involves a flash combustion of the weighed sample in a hot empty chamber at 950-1050 degrees and swept by oxygen at 60 ml/min. Together with this combustion in the gaseous phase, an oxidation of the primary combustion gases on cupric oxide at 850 degrees is necessary. Oxidation products containing halogens and sulphur are retained on silvered alumina at 750-800 degrees . Combustion water containing deuterium oxide and hydroxide is frozen out from the combustion gases in a special trap with two five-way stop-cocks which make possible the simultaneous flow of oxygen and hydrogen; the latter is used as a carrier-gas in the apparatus from the trap downwards. The frozen water is then vaporized by heating in a hydrogen flow of 30 ml/min and reduced on magnesium at 600 degrees . Deuterium is obtained as deuterium hydride in hydrogen; it is measured versus pure hydrogen, with a thermal conductivity detector. A Determination within a series can be completed in 15 min. The precision of the results is that obtained in classical organic microanalysts.
Fraisse
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Service Central de Microanalyse du Centre National de la Recherche Scientifique, 2, rue Henry Dunant, 94320 Thiais, France.
Girard
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Levy
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