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A modular X-ray scanning system was developed, to fill in the gap between portable instruments (with a limited analytical area) and mobile instruments (with large analytical areas, and sometimes bulky and difficult to transport). The scanner has been compared to a commercial tabletop instrument, by analysing a Portuguese tile (azulejo) from the 17th century. Complementary techniques were used to achieve a throughout characterisation of the sample in a complete non-destructive approach. The complexity of the acquired X-ray fluorescence (XRF) spectra, due to inherent sample stratigraphy, has been resolved using Monte Carlo simulations, and Raman spectroscopy, as the most suitable technique to complement the analysis of azulejos colours, yielding satisfactory results. The colouring agents were identified as cobalt blue and a Zn-modified Naples-yellow. The stratigraphy of the area under study was partially modelled with Monte Carlo simulations. The scanners performance has been compared by evaluating the images outputs and the global spectrum.

Nearly half of the world cereal production comes from soils low or marginal in plant available zinc, leading to unsustainable and poor quality grain production. Therefore, the effects of nitrogen (N) rate and application time on zinc (Zn) and iron (Fe) concentration in wheat grain were investigated. Wheat ( var. Krabat) was grown in a growth chamber with 8 and 16 h of day and night periods, respectively. The N rates were 29, 43, and 57 mg N kg soil, equivalent to 80, 120, and 160 kg N ha . Zinc and Fe were applied at 10 mg kg growth media. In one of the N treatments, additional Zn and Fe through foliar spray (6 mg of Zn or Fe in 10 ml water/pot) was applied. Micro-analytical localization of Zn and Fe within grain was performed using scanning macro-X-ray fluorescence (MA-XRF) and laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS). The following data were obtained: grain and straw yield pot , 1000 grains weight, number of grains pot , whole grain protein content, concentration of Zn and Fe in the grains. Grain yield increased from 80 to 120 kg N ha rates only and decreased at 160 kg N ha g. Relatively higher protein content and Zn and Fe concentration in the grain were recorded with the split N application of 160 kg N ha . Soil and foliar supply of Zn and Fe (Zn + Fe ), with a single application of 120 kg N ha N at sowing, increased the concentration of Zn by 46% and of Fe by 35%, as compared to their growth media application only. Line scans of freshly cut areas of sliced grains showed co-localization of Zn and Fe within germ, crease and aleurone. We thus conclude that split application of N at 160 kg ha at sowing and stem elongation, in combination with soil and foliar application of Zn and Fe, can be a good agricultural practice to enhance protein content and the Zn and Fe concentration in grain.

At present, macro X-ray fluorescence (MA-XRF) is one of the most essential analytical methods exploited by heritage science. By providing spatial distribution elemental maps, not only does it allow for material characterisation but also to understand, or at least to have a likely idea of, the production techniques of an analysed object. INFN-CHNet, the Cultural Heritage Network of the Italian National Institute of Nuclear Physics, designed and developed a MA-XRF scanner aiming to be a lightweight, easy to transport piece of equipment for use in in situ measurements. In this study, the INFN-CHNet MA-XRF scanner was employed for the analysis of a painting by the Flemish artist Rogier van der Weyden. The painting belongs to the collection of the Uffizi gallery in Florence and was analysed during conservation treatments at the Opificio delle Pietre Dure, one of the main conservation centres in Italy. The research aims were to characterise the materials employed by the artist and to possibly understand his painting technique. Although MA-XRF alone cannot provide a comprehensive characterisation, it nonetheless proved to be an invaluable tool for providing an initial overview or hypothesis of the painting materials and techniques used.

Analytical techniques play a fundamental role in heritage science. Among them, Particle Induced X-ray Emission (PIXE) and X-ray Fluorescence (XRF) techniques are widely used in many laboratories for elemental composition analysis. Although they are well-established, a strong effort is put on their upgrade, making them suitable for more and more applications. Over the years, at the INFN-LABEC (the laboratory of nuclear techniques for the environment and cultural heritage of the Italian National Institute of Nuclear Physics), the INFN-CHNet group, the network devoted to cultural heritage, has carried out many technological improvements to the PIXE and XRF set-ups for the analysis of works of art and archaeological finds. Among the many, we recall here the scanning external microbeam facility at the TANDEM accelerator and the MA-XRF scanner. The two instruments have shown complementary features: the former permits quantitative analysis of elements heavier than sodium, which is not possible with the latter in most of the case studies. On the contrary, the scanner has the undeniable advantage of portability, allowing it to work in situ. In this framework of technological developments in heritage science, INFN, CERN, and OPD are jointly carrying on the MACHINA (Movable Accelerator for Cultural Heritage In-situ Non-destructive Analysis) project for on-site Ion Beam Analysis (IBA) studies on cultural heritage.

As part of the 2018 Girl in the Spotlight project, reflectance and molecular fluorescence imaging spectroscopy (RIS, FIS), and macroscale X-ray fluorescence scanning (MA-XRF) were performed on Johannes Vermeer’s Girl with a Pearl Earring (c. 1665, Mauritshuis) with the goal of obtaining a comprehensive understanding of the distribution of pigments. Prior analysis of cross-sections in the 1990s, and their recent (re)-examination identified many of the pigments present in the painting. The results from all three imaging methods, along with site-specific fibre optic reflectance spectroscopy, confirmed Vermeer’s limited palette and determined how and where each pigment was used. RIS and MA-XRF found the blue region of the headscarf was painted with natural ultramarine and varying amounts of lead white. The yellow part of the headscarf was painted with yellow ochre and lead white, and the border of the headscarf additionally contained ultramarine and lead–tin yellow. The lit side of the jacket was painted with yellow ochre, lead white, and ultramarine, whereas the darker, ruddy blue-green areas that are in relative shadow contained yellow ochre with ultramarine. FIS also mapped a red lake in portions of the shadowed areas at the back of the jacket. The Girl’s skin was painted using earths (ochres), lead white, vermilion, and some red lake. Fluorescence emission from red lake was strongest in the lips, where vermilion was also found. The pearl earring was depicted using a scumble and highlight of lead white. In the dark background, the RIS data cube allowed the determination of the visible spectral shape even though the overall reflectance intensity was low (1 to 3%). A reflectance inflection point at ~ 700 nm indicated the presence of indigo, whereas lack of a reflectance peak at green wavelengths in most areas indicated degradation of the yellow pigment previously identified as weld. Some small green areas in the background (i.e. reflectance maximum at 525 nm) were found; these coincided with areas previously protected by old retouchings, and are thus better preserved. The combination of all three spectral imaging modalities provided a more complete understanding of how the colouration of the painting was achieved.

Even though X-ray fluorescence (XRF) is strictly an atomic method, this technique has been developed mostly at research centers for nuclear physics. One of its most valuable variations is the mapping mode that allows it to shift XRF from a punctual to an image technique. Macro X-ray Fluorescence (MA-XRF) is a widespread analytical technique applied in cultural heritage for characterizing the elemental composition of pigments with a non-destructive, rapid and green approach. When dealing with cultural heritage materials, the sustainability of the applied techniques is directly linked to the limited impact on the work of art. MA-XRF can reveal hidden sub-surface layers or restorations, but, nonetheless, it is hardly adopted for estimating the thickness of layers without resorting to complex Monte Carlo simulations or without combining information from other techniques. Exploiting the recurrent presence of lead white under pictorial layers in historical artworks, we perform a calibration on stand-alone layers produced ad hoc for the relative absorption of Pb L fluorescence lines, and then, their ratio is successfully used to estimate the thickness of azurite and ultramarine blue layers over lead white. The final result is rendered as a heatmap, easy to present to non-technical personnel frequently involved in the cultural heritage field. The new proposed procedure for calculating layer thickness extends the concept of non-invasive applications, paving the way to the possibility of performing stratigraphy without sampling.

Religious panel paintings (icons) play a pivotal role in the rituals of the Eastern Orthodox Christian Church. However, their continuous use often results in physical degradation, prompting remedial interventions. Quite commonly, alterations were treated by simply applying new paint layers directly over the decayed original, while in some cases, old icons were overpainted merely as a means to renovate and modernize them. Therefore, numerous overpainted icons are currently housed in churches, museums, and private collections across Greece. This study focuses on the investigation of a post-Byzantine icon of Christ Pantokrator, which displays extensive overpainting while retaining a few visible fragments of the original composition. The objective was to assess the extent and condition of preservation of the original artwork, to identify materials and techniques used both in the initial painting and in subsequent restoration phases, and to distinguish between those phases. To achieve these aims, a fully non-invasive diagnostic methodology was implemented, including visible light photography, ultraviolet radiation imaging (UVR/UVL), hyperspectral imaging (MuSIS HS), infrared reflectography (IRRef), X-ray radiography, and macroscopic X-ray fluorescence scanning (MA-XRF). The findings confirm that the original painting remains substantially preserved and is of high artistic quality. Moreover, analysis revealed at least two distinct phases of overpainting, likely dating from the 20th century, while the results suggest that the original artwork probably dates to the first half of the 18th century. The study highlights the need to use complementary techniques in order to non-invasively assess complex artifacts like overpainted icons and offers valuable insights into historical restoration practices providing foundation for future conservation planning.

X-ray fluorescence (XRF) spectrometry has proven to be a core, non-destructive, analytical technique in cultural heritage studies mainly because of its non-invasive character and ability to rapidly reveal the elemental composition of the analyzed artifacts. Being able to penetrate deeper into matter than the visible light, X-rays allow further analysis that may eventually lead to the extraction of information that pertains to the substrate(s) of an artifact. The recently developed scanning macroscopic X-ray fluorescence method (MA-XRF) allows for the extraction of elemental distribution images. The present work aimed at comparing two different analysis methods for interpreting the large number of XRF spectra collected in the framework of MA-XRF analysis. The measured spectra were analyzed in two ways: a merely spectroscopic approach and an exploratory data analysis approach. The potentialities of the applied methods are showcased on a notable 18th-century Greek religious panel painting. The spectroscopic approach separately analyses each one of the measured spectra and leads to the construction of single-element spatial distribution images (element maps). The statistical data analysis approach leads to the grouping of all spectra into distinct clusters with common features, while afterward dimensionality reduction algorithms help reduce thousands of channels of XRF spectra in an easily perceived dataset of two-dimensional images. The two analytical approaches allow extracting detailed information about the pigments used and paint layer stratigraphy (i.e., painting technique) as well as restoration interventions/state of preservation.

In 1540, in Ingolstadt, Germany, the influential astronomer and printer Peter Apian produced the Astronomicum Caesareum: a printed and hand-coloured astronomical book visualising the Ptolemaic universe through the use of diagrams and wheelcharts, worthy of his imperial patron, Charles V. About 130 copies have survived to this day, with varying degrees of paper quality and level of decoration, and only eleven volumes are considered deluxe copies. We thoroughly analysed one deluxe volume held at the Fitzwilliam Museum, Cambridge, and compared the results with four (one deluxe and three standard) other copies from institutions in the UK. A non-invasive analytical protocol was applied, including extensive microscopy, fibre-optic reflectance spectroscopy (FORS), X-ray spectroscopy (XRF), macroscale XRF (MA-XRF) and Raman spectroscopy. The most interesting pages were chosen based on art-historical evidence and the variety of the colour palette, including on volvelles (wheelcharts) and coats of arms. Following a systematic approach, we analysed the same pages in each volume, gathering information on the colour palette in all the volumes. The type of paper and the presence of watermarks were also documented. A wide range of materials was identified in the five copies, including red, purple and yellow organic dyes, lead white, verdigris, vermilion, azurite, indigo, smalt, and lead–tin yellow. Mosaic gold was used to embellish certain paint passages in the deluxe volumes and metals (gold and silver) were applied on some pages. The comprehensive findings were essential to identify specific traits related to Apian’s workshop, to differentiate deluxe from standard copies, to suggest an order of production of the copies, and to provide new information on this landmark book and more generally in an under-researched field of study.