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Solid sampling electrothermal atomic absorption spectrometry for analysis of high-purity tungsten trioxide and high-purity tungsten blue oxide
Institution:1. Institute for Chemical Technology of Inorganic Materials, Johannes Kepler University Linz, Altenberger Str. 69, 4040 Linz, Austria;2. Christian Doppler Laboratory for Combinatorial Oxide Chemistry at the Institute for Chemical Technology of Inorganic Materials, Johannes Kepler University Linz, Altenberger Str. 69, 4040 Linz, Austria;1. College of Physics and Electronic Information, Anhui Key Laboratory of Energetic Materials, Huaibei Normal University, Huaibei 235000, PR China;2. Key Laboratory of Materials Physics and Anhui Key Laboratory of Nanomaterials and Nanotechnology, Institute of Solid State Physics, Hefei Institutes of Physical Science, Chinese Academy of Sciences, Hefei 230031, PR China;1. State Key Laboratory of Crystal Materials, Shandong University, Jinan, 250100, China;2. College of Chemistry, Chemical Engineering and Materials Science, Shandong Normal University, 250014, China;1. Nikolaev Institute of Inorganic Chemistry, Siberian Branch of the Russian Academy of Sciences, Lavrentyev Av., 3, RU-630090 Novosibirsk, Russian Federation;2. Boreskov Institute of Catalysis, Siberian Branch, Russian Academy of Sciences, Lavrentyev Av., 5, RU-630090, Novosibirsk, Russian Federation;1. Institute of Physics, Faculty of Mechanical Engineering and Mechatronics, West Pomeranian University of Technology in Szczecin, Al. Piastow 17, 70-310, Szczecin, Poland;2. Institute of Physics PAS, Al. Lotników 32/46, 02-668 Warsaw, Poland
Abstract:A solid sampling ETAAS method for the direct determination of Ca, Co, Cr, Cu, Fe, K, Mg, Mn, Na, Ni and Zn in high-purity tungsten trioxide and tungsten blue oxide powders using a modern spectrometer with transversely heated graphite tube and a solid sampling system is described. The extremely high background caused by the vaporizing tungsten oxides could be eliminated by the reduction to tungsten metal using hydrogen as purge gas during pyrolysis. Quantification of all elements was performed using calibration curves measured with aqueous standard solutions. The analyte contents determined were between 0.033 (Cu) and 12.6 (Fe) μg/g for tungsten trioxide and between 0.001 (Co) and 0.5 (Na) μg/g for tungsten blue oxide. The accuracy was checked by comparing the results with those obtained by ETAAS in analysis of HF/HNO3 sample digests and by other methods. Extremely low limits of detection being between 0.07 (Mg, Na, Zn) - 2 (Ni) and 0.01 (Mg, Na, Ni) - 1.7 (Fe) ng/g for tungsten trioxide and tungsten blue oxide, respectively, could be achieved due to almost complete freedom of blank and unusually high applicable sample amounts (5–15 mg for tungsten trioxide and 5–70 mg for tungsten blue oxide).
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