Summary
A new method for high-temperature vacuum-degassing has been described and applied to the determination of very small quantities of hydrogen, oxygen and nitrogen in refractory materials as well as large amounts of these elements in hydrides, oxides and nitrides. A closed graphite capsule is used to prevent the loss of oxygen (as CO2) and the evaporation of low-melting oxides. In the analysis of highly refractory oxides addition of Si or Si alloys is required. The analysis of nitrides and hydrides does not cause any difficulties if the degassing temperature is high enough. Yet, difficulties arise with the very stable nitrides of the metals of the IVa and Va groups of the periodic system. Several samples are analyzed according to the method described and to standard techniques and the results are compared.
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Paesold, G., Müller, K. & Kieffer, R. Über die Bestimmung von Sauerstoff, Stickstoff und Wasserstoff in Oxiden und Hartstoffen durch Hochtemperatur-Vakuumentgasung. Z. Anal. Chem. 232, 31–40 (1967). https://doi.org/10.1007/BF00528799
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DOI: https://doi.org/10.1007/BF00528799