Métodos de análise de materiais híbridos: um estudo comparativo entre fluorescência de raios-x com detecção dispersiva em energia usando fonte tradicional e luz síncroton

Abstract

It was possible to identify and detect Ti dopant in the range of tens of mg.Kg -1 by means of Grazing Incidence X-Ray Fluorescence (GIXRF) analysis assisted by Synchrotron Radiation. In addition, Microscopic X-ray Fluorescence analysis (μ-XRF) assisted by Synchrotron Radiation enabled the identification of spatial distributions of Titanium and Zinc within ormosils. Since these XRF analyses did not employ certified materials for validation, standards were prepared at our laboratory following a similar protocol to that used to prepare the samples. The semi-quantification method based on fundamental parameters was also used, which demonstrated be very useful and efficient. X-ray fluorescence results were validated by those obtained from Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES) and Instrumental Neutron Activation Analysis (INAA). The different methods of analysis employed (μ-XRF GIXRF, EDXRF, ICP-OES, AAS) were effective regarding precision and accuracy in Tungsten and Zinc quantification. In the case of Titanium, however, only μ-XRF and ICP-OES results could be taken into account. Therefore, there is the need for additional analytical methods to validate concentration results for this element in ormosils. ICP-OES and INAA proved to be reference methods for results obtained through XRF (Laboratory and assisted by Synchrotron Radiation) for our materials.