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ICP-AES detection of silicon carbide impurities volatilized in a graphite furnace with the use of carbon tetrachloride vapour
Authors:Gyula Záray  Tibor Kántor  Gerhard Wolff  Zdravka Zadgorska  Hubertus Nickel
Affiliation:(1) Department of Inorganic and Analytical Chemistry, L. Eötvös University, P.O. Box 32 BP 112, H-1518 Budapest, Hungary;(2) Institute for Reactor Materials, Research Center Jülich (KFA), P.O. Box 1913, D-W-5170 Jülich, Federal Republic of Germany
Abstract:The analytical capability of high-temperature halogenation with carbon tetrachloride vapour in a graphite furnace was investigated for silicon carbide powder with known chemical composition and particle size. Intensity vs heating time curves were determined for analytical lines of Al, B, Ba, Ca, Cr, Cu, Fe, Mg, Mn, Ti, V and Si constituents, volatilized with and without the presence of CCl4 vapour in the furnace atmosphere. Igniting 10 mg SiC at 2100 °C for 60 s in chlorinating atmosphere, the evaporated fraction of most of the constituents was higher than 90% (for Al about 50%). The line intensity vs sample mass (4–26 mg) relationships were linear for all impurities studied, while the intensity of silicon line showed a relatively small change with the sample mass. BEC (background equivalent concentration) values for this solid sampling technique (10 mg loaded sample) were 2–20 fold lower than those calculated for the conventional solution sample introduction method.
Keywords:solid sampling  electrothermal vaporization  halogenation  ICPAES  silicon carbide
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