EX-SITU PORTABLE X-RAY FLUORESCENCE SPECTROMETRY FOR THE MAJOR ELEMENTS DETERMINATION IN SILICATE GEOLOGICAL SAMPLES USING MATRIX-MATCHING STANDARDS FOR CALIBRATION
DOI:
https://doi.org/10.24193/subbchem.2021.2.10Keywords:
X-ray fluorescence, major element, zeolite, instrument calibration, matrix-matching calibration, ex-situ procedure.Abstract
An ex-situ method for determining the major elements in the high silicate matrix using portable XRF spectrometry (pXRF) was developed. The calibration is based on the dilution of a matrix-matched certified reference material BCS-CRM No. 376/1 Potash Feldspar with analytical grade SiO2. Significant correlation coefficients for linear regressions were obtained for all major oxides. This approach of instrument calibration has as the principal advantage the use of a single certified reference material, which reduce the cost of analysis. The limits of detection were evaluated from measurement of SiO2 considered as blank. The method accuracy of the developed calibration was checked in the recovery study of two certified reference materials (BCS-CRM No. 309 Sillimanite and BCS-CRM No. 375/1 Soda Feldspar), with geological matrix, and the recoveries rate were in the range of 85 – 110 %. The relative expanded uncertainties (k = 2, P = 95%) calculated from CRM analysis were of 6.99% for Al2O3, 3.56% for Fe2O3, 4.82% for CaO and 4.31% for K2O. The proposed methodology is a green analytical method, allowing fast and accurate analysis of geological samples without use of chemical reagents.
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