Validation of energy-dispersive X-ray fluorescence procedure for determination of major and trace elements present in the cement based composites

Abstract

Adjustment and subsequent validation of energy-dispersive X-ray fluorescence (ED-XRF) method for cement based binders with addition of mineral raw materials (fly ash, zeolite and bentonite) was conducted. Eighteen chemical elements present in the material composition were analyzed: ten major elements (Si, Al, Fe, Ca, Mg, S, Na, K, Ti, P) and eight trace elements (Cr, Zn, Cu, As, Ni, Pb, Sr, Mn). Thirty-five samples of either certified reference materials or reference materials of cement, fly ash and clay were utilized during adjustment and optimization of the investigated ED-XRF procedure. The method was consecutively validated in terms of selectivity, precision, working range, linearity, accuracy, robustness, limits of detection and quantification. Thirty-two samples in total, i.e. three certified reference materials and twenty-nine reference materials, were simultaneously analyzed by ED-XRF and inductively coupled plasma optical emission spectrometry (ICP-OES). Comparison of the outputs of monitored methods showed infinitesimally small differences, as correlation coefficients were extremely good (≈1), which highlighted ED-XRF as highly satiable alternative for ICP-OES for the chemical analysis of cement binders.