Abstract
A correct determination of the mineral and chemical composition of specimens is of the utmost importance to answer questions regarding the Cultural Heritage field. Because of the preciousness and often very low quantity of sample available, with textures and sizes in the nano-to-micrometric range, scanning electron microscopy (SEM) combined with energy-dispersive X-ray spectroscopy (EDS) is one of the most suited and exploited nano-microanalytical techniques. In these cases, to avoid severe mistakes and quantification errors in SEM-EDS, it is mandatory to consider several effects related to the transport of electrons and X-rays in the material, which in turn are dependent on the SEM-EDS setup. In the present work, a Monte Carlo SEM-EDS nano-microanalytical simulation strategy is proposed and applied to a practical selected case. The Egyptian blue mineral pigment, which is found in Pompeian murals, is used here as an example and model system to show the effects of real size variations (0.1–10 µm), basic geometrical shapes of the pigment (prismatic and spherical) and typical SEM setups, sample holders and substrates. The simulations showed a great—sometimes not intuitive—dependence of the X-ray intensity on the thickness and shape of the samples and SEM-EDS parameters, thereby influencing the analysis and quantification. The critical overview of the results allowed the determination of the correct procedure and technical SEM-EDS parameters and indicated how to apply the Monte Carlo simulation strategy to other Cultural Heritage cases.
Highlights
Since the middle of the last century and especially over the last few decades, the analytical methods used in experimental sciences have received and are receiving more and more applications in the study of materials in the Cultural Heritage field, contributing in different ways to the scientific and historical–archaeological knowledge and advancement
We show the usefulness and practicality of the Monte Carlo simulation to specimen would result in an erroneous estimation of the chemistry of the sample, because its thickness establish a correct microanalysis strategy
A correct determination of the mineralogical and chemical composition at the nano- and micro-scale is nowadays fundamental in microstructural studies of specimens belonging to the Cultural Heritage field, since it helps in guiding the resolution of the nature, genetic and thermodynamic questions concerning the object of study and how to establish restoration and conservation protocols
Summary
Since the middle of the last century and especially over the last few decades, the analytical methods used in experimental sciences have received and are receiving more and more applications in the study of materials in the Cultural Heritage field, contributing in different ways to the scientific and historical–archaeological knowledge and advancement. Different questions such as composition, chronology, origin or production technology have been solved with the use of this experimental technology. The latest advances in these systems and the quality of the chemical quantification data they produce have expanded their relevance upstream in the field of mineral characterization, because with SEM-EDS, it is possible to determine the mineral phases according to their stoichiometry, shape and texture, stratigraphic section sequences, sizes, and other parameters [2,3]
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