title: Development of X-ray Fluorescence Quantitative Methodologies To Analyze Aqueous and Acid Extracts from Building Materials Belonging to Cultural Heritage.
abstract: Energy dispersive X-ray fluorescence spectrometry (ED-XRF) is widely used in art and cultural heritage for direct measurements and elemental quantification of solid samples. However, in the literature there are not works dealing with the quantitative application of ED-XRF to liquid extracts coming from samples belonging to cultural heritage. In this work, a novel methodology based on the use of ED-XRF spectrometry after thin film deposition on special sample retainers and a subsequent evaporation was developed to quantify light elements (Z ≤ 20) in aqueous extracts and heavy elements (Z > 20) in acid extracts, coming from materials and degradation products belonging to built heritage (mortars, black crusts, and calcium carbonate formations). For this purpose, special sample retainers were used instead of more common adsorbent filter papers. Three different ED-XRF calibration methodologies were designed as elemental quantification tools and "green chemistry" alternatives to conventional techniques. On the one hand, the developed external ED-XRF calibration methodology for elements with Z ≤ 20 was proposed as an alternative to ion chromatography to obtain information about the degradation processes that the building materials suffered. On the other hand, the external ED-XRF calibration for elements with Z > 20 in acid extracts was optimized as a faster and cleaner quantification alternative to inductively coupled plasma mass spectrometry (ICPMS). Finally, with the aim to reduce the matrix effect and to improve the quantitative results for elements with Z > 20 in acid extracts, a novel ED-XRF calibration methodology based on standard additions was successfully designed and applied to real samples belonging to built heritage.
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of Basque Country UPV/EHU , P.O. Box 644, 48080 Bilbao, Basque Country, Spain.
authors.forename: Cristina
authors.identifier: 0000-0002-0329-8012
authors.initials: C
authors.lastname: García-Florentino
authors.affiliation: Department of Analytical Chemistry, Faculty of Pharmacy, University of the Basque Country UPV/EHU , P.O. Box 450, 01080, Vitoria-Gasteiz, Basque Country, Spain.
authors.forename: Maite
authors.initials: M
authors.lastname: Maguregui
authors.affiliation: Department of Chemistry, University of Girona, Faculty of Sciences , C/M.Aurèlia Campmany, 69, Girona, Spain.
authors.forename: Eva
authors.initials: E
authors.lastname: Marguí
authors.affiliation: Institute of Environmental Assessment and Water Research, IDAEA-CSIC, Jordi Girona 18-26, 08034 Barcelona, Spain.
authors.forename: Ignasi
authors.initials: I
authors.lastname: Queralt
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of Basque Country UPV/EHU , P.O. Box 644, 48080 Bilbao, Basque Country, Spain.
authors.forename: Jose Antonio
authors.initials: JA
authors.lastname: Carrero
authors.affiliation: Department of Analytical Chemistry, Faculty of Science and Technology, University of Basque Country UPV/EHU , P.O. Box 644, 48080 Bilbao, Basque Country, Spain.
authors.forename: Juan Manuel
authors.identifier: 0000-0002-1685-6335
authors.initials: JM
authors.lastname: Madariaga