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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