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Fourier transform infrared spectroscopy is a powerful analytical technique to study organic materials. However, in Cultural Heritage, since the sample under analysis is always a complicated matrix of several materials, data analysis performed through peak-by-peak comparisons of sample spectra with those of standard compounds is a tedious method that does not always provide good results. To overcome this problem, a chemometric model based on principal component analysis was developed to classify and identify organic binding media in artworks. The model allows the differentiation of five families of binders: drying oils, waxes, proteins, gums, and resins, taking into account the absorption bands in two characteristic spectral windows: C-H stretching and carbonyl band. This new methodology was applied in the characterization of binders in three kinds of artworks: papers of historical, archeological, and artistic value, easel paintings, and polychromed stone-based sculptures. [Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

The uniqueness and limited amounts of forensic samples and samples from objects of cultural heritage together with the complexity of their composition requires the application of a wide range of micro-analytical methods, which are non-destructive to the samples, because these must be preserved for potential late revision. Laboratory powder X-ray micro-diffraction (micro-XRD) is a very effective non-destructive technique for direct phase analysis of samples smaller than 1 mm containing crystal constituents. It compliments optical and electron microscopy with elemental micro-analysis, especially in cases of complicated mixtures containing phases with similar chemical composition. However, modification of X-ray diffraction to the micro-scale together with its application for very heterogeneous real samples leads to deviations from the standard procedure. Knowledge of both the limits and the phenomena which can arise during the analysis is crucial for the meaningful and proper application of the method. We evaluated basic limits of micro-XRD equipped with a mono-capillary with an exit diameter of 0.1 mm, for example the size of irradiated area, appropriate grain size, and detection limits allowing identification of given phases. We tested the reliability and accuracy of quantitative phase analysis based on micro-XRD data in comparison with conventional XRD (reflection and transmission), carrying out experiments with two-phase model mixtures simulating historic colour layers. Furthermore, we demonstrate the wide use of micro-XRD for investigation of various types of micro-samples (contact traces, powder traps, colour layers) and we show how to enhance data quality by proper choice of experiment geometry and conditions. [ABSTRACT FROM AUTHOR]

A complete study of several English polychromed alabaster sculptures is presented. The support, pigment, and binders were characterised by combining μEDXRF, μRaman, and FTIR spectroscopies. Among the pigments, minium, vermilion, lead white, carbon black, red iron oxide, and a degraded green copper pigment were determined, together with gold leaf. The presence of the rare mineral moolooite (copper oxalate) was also found as a degradation product in the green areas, where weddellite (calcium oxalate dihydrate) was also determined. These facts, together with degradation of the green copper pigment, suggest microbiological degradation of the original materials. Remains of glue and a varnish were also determined by FTIR spectroscopy and principal-components analysis (PCA) of the spectra. Finally, PCA analysis was carried out to confirm whether the pieces came from the same quarry. [ABSTRACT FROM AUTHOR]

Non-destructive and non-invasive micro-Raman fibre optic and micro-XRF analyses were performed to study a wallpaper from the beginning of the 19th century. The complementarity of these two non-destructive techniques is shown in this work. The analysed artwork is considered one of the most beautiful wallpapers ever manufactured according to the catalogues and books; it is known as Chasse de Compiègne, manufactured by Jacquemart, Paris, in 1812. During the analysis, an unexpected pigment was detected by both analytical techniques: lead-tin yellow type II. This pigment was used until ca. 1750, when other yellow pigments replaced it, thus it is very difficult to find it in paintings afterwards. Together with this pigment, red lead, Prussian blue, brochantite, yellow iron oxide, calcium carbonate, vermilion, carbon black of animal origin (bone black), lead white, and raw and burnt sienna were also determined by combining the analytical information provided by both techniques. A possible degradation of brochantite to antlerite is also discussed. [ABSTRACT FROM AUTHOR]