Abstract
Mechanisms of atomization of molybdenum in graphite furnace atomic absorption spectrometry have been investigated using platform technique along with X-ray diffraction spectrometry, scanning electron micrography, energy dispersive X-ray and Auger electron spectrometry. Three molybdenum oxides: MoO 2(s), MoO 3(s) and Mo 4O 11(s), have been identified—all formed at relatively low temperatures (< 1500 K). Crystallites of MoO 2 of relatively large size are formed on the pyrolytic graphite surface. When molybdenum is atomized from a pyrolytic graphite surface, the charring curve of molybdenum shows a dip in absorbance in the temperature range 1200–1800 K. Hence, a charring temperature < 1200 K should be used for determination of molybdenum when a pyrolvtically coated graphite tube or a platform made of pyrolytic graphite is used. Mo s, MoC s and Mo 2C (s) have been found on both pyrolytic graphite and electrographite surfaces in the charring step. Formation of Mo g, by direct sublimation of Mo (s) and/or dissociation of MoC (g) are all spontaneous reactions at the temperatures considered.
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