doiSerbia

Improvement and modification of energy-dispersive X-ray fluorescence method for the determination of metal elements in cement leachates: A chemometric approach

Mijatović Nevenka N. (Institute for Testing of Materials IMS, Belgrade, Serbia), nevenka.mijatovic@institutims.rs
Terzić Anja M. (Institute for Testing of Materials IMS, Belgrade, Serbia)
Pezo Lato L. (Institute of General and Physical Chemistry, University of Belgrade, Belgrade, Serbia)
Miličić Ljiljana R. (Institute for Testing of Materials IMS, Belgrade, Serbia)
Živojinović Dragana Z. (Faculty of Technology and Metallurgy, University of Belgrade, Belgrade, Serbia)

A modification of an analytical procedure for the energy-dispersive X-ray fluorescence (EDXRF) quantification of ten chemical elements (As, Ba, Cd, Co, Cr, Cu, Mo, Ni, Pb and Zn) in the leachates obtained from cement binders was developed. Twenty-nine testing samples were used in the experiment. All samples were based on Portland cement. Fly ash of different origin, zeolite and bentonite were employed as mineral additives in the cement binders. Distilled water was used as the leachate. Validation of the modified EDXRF procedure was conducted in terms of limits of detection and quantification, working range, linearity, selectivity, precision, trueness, and robustness. Traceability of the procedure was established using certified reference materials. Uncertainty of measurement was confirmed via an “in-house” laboratory validation approach. The expanded uncertainties for the ten analysed elements were obtained for the entire working range of the EDXRF method. Robustness of the modified EDXRF procedure was assessed by means of a chemometric in-house approach. The results obtained by the modified X-ray fluorescence method were additionally correlated to those acquired by inductively coupled plasma optical emission spectrometry to confirm that EDXRF could be used as an effective and reliable alternative method for analysis of cement leachates.

Keywords: in-house validation, mineral additives, cluster analysis, ICP-OES, EDXRF, building materials

Project of the Serbian Ministry of Education, Science and Technological Development, Grant no. 451-03-68/2020-14/200012