Microchemical Journal

Abstract

Texto completo: acesso restrito. p. 41–48The determination of impurities in titanium dioxide pigments, such as Al, Cd, Cr, Fe, Mn, P, Zn and Zr, is relevant because trace elements affect pigment properties. The critical step in the analysis of this pigment is the conversion of the solid sample to a representative solution. This study compared four acid decomposition procedures for TiO2 for the determination of Al, P and trace impurities using inductively coupled plasma optical emission spectrometry. The decomposition procedures investigated involved acid digestion with: (i) (NH4)2SO4/H2SO4; (ii) HF/H2SO4; (iii) H3PO4; and (iv) HCl/HNO3/HF. This latter mixture was tested in a microwave-assisted procedure with closed vessels. Comparing the procedures using conventional conductive heating, the procedure using (NH4)2SO4/H2SO4 was the most suitable for complete decomposition of TiO2 samples, requiring approximately 30 min. Applying a paired t-test, it was shown that all strategies led to results in agreement at a 95% confidence level with those obtained using X-ray fluorescence. The accuracy for Cr, Fe, P and Zr was also checked using a certified reference material, and again all results were in agreement at a 95% confidence level. The performance of two ICP-OESs, one based on a mini-torch using a radial view configuration, and the other based on an axial view configuration, were compared. Both plasmas are intensely affected by matrix constituents. The mini-torch plasma is less able to cope with high amounts of solids; however this parameter also negatively affects the background level when using axial-viewed ICP-OES