Abstract
A procedure for determination of oxygen in oxides with high pressure of dissociation (NiO, CuO, CoO, Fe2O3, SnO2), including volatile (MoO3, WO3), by pulsed reductive fusion (evaporation) in carrier-gas flow at 2500 K in double graphite capsules (with Ni-Sn bath or graphite powder) on an apparatus with simultaneous IR detection of CO and CO2 is described. The validity of the protocol and its metrological characteristics were evaluated in a series of calibration experiments with a set of pure stoichiometric oxides, including a NiO certified reference material with certified oxygen content. The expanded uncertainty of analysis for the developed procedure was 0.1 wt %. The working range was 2–15 mg of oxygen.
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Original Russian Text © P.V. Krasovskii, 2013, published in Zavodskaya Laboratoriya. Diagnostika Materialov, 2013, Vol. 79, No. 11, pp. 30–35.
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Krasovskii, P.V. Determination of oxygen in oxides with high dissociation pressure by inert gas fusion method. Inorg Mater 50, 1480–1486 (2014). https://doi.org/10.1134/S0020168514150059
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DOI: https://doi.org/10.1134/S0020168514150059