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Determination of Mg and Ti in Ziegler–Natta catalysts by x‐ray fluorescence spectrometry
Author(s) -
Bichinho Kátia M.,
Pires Gilvan Pozzobon,
dos Santos João Henrique Z.,
Wolf Carlos Rodolfo
Publication year - 2004
Publication title -
x‐ray spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.447
H-Index - 45
eISSN - 1097-4539
pISSN - 0049-8246
DOI - 10.1002/xrs.777
Subject(s) - catalysis , complexometric titration , calcination , mass spectrometry , chemistry , nuclear chemistry , x ray fluorescence , titration , metal , analytical chemistry (journal) , fluorescence spectrometry , fluorescence , materials science , inorganic chemistry , chromatography , organic chemistry , physics , quantum mechanics
The metal content in Ziegler–Natta catalysts based on Ti and Mg derivatives could not be determined directly by x‐ray fluorescence (XRF) spectrometry owing to the instability of the catalyst. The samples were then calcined and the resultant Mg and Ti oxides were characterized by x‐ray diffraction (XRD). A series of synthetic standards were prepared with high‐purity MgO and TiO 2 , since there were no available certified standards for the catalysts. Samples and standards were compressed with high‐purity H 3 BO 3 flux. This protocol was shown to be reproducible, having a correlation coefficient of 0.9999. The metal contents determined by XRF were in accordance with those obtained by a complexometric titration (Mg) and a UV–visible spectrophotometric method (Ti). Copyright © 2004 John Wiley & Sons, Ltd.