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“Development of a multi-method analytical approach based on the combination of synchrotron radiation X-ray micro-analytical techniques and vibrational micro-spectroscopy methods to unveil the causes and mechanism of darkening of “fake-gilded&rdquo, decorations in a Cimabue painting”. Monico L, Prati S, Sciutto G, Catelli E, Romani A, Balbas DQ, Li Z, De Meyer S, Nuyts G, Janssens K, Cotte M, Garrevoet J, Falkenberg G, Tardillo Suarez VI, Tucoulou R, Mazzeo R, Journal of analytical atomic spectrometry 37, 114 (2022). http://doi.org/10.1039/D1JA00271F
Abstract: Redox processes activated by environmental factors have been identified as the main cause of the chromatic alterations of a number of artists' pigments, including the yellow pigment orpiment (As2S3). Although a general comprehension of the mechanisms has been provided through characterization of degradation compounds of As2S3, experimental evidences to prove how other paint components and how different environmental agents influence the formation pathways of specific secondary compounds are still lacking. Thus, it becomes fundamental to develop a methodological strategy which enable achieving a discrimination among the causes affecting the chemical stability of more heterogenous As2S3-based paints and defining the mechanism through which the alteration establishes and evolves, with the ultimate goal of optimizing the preventive conservation measures of unique masterpieces. In this paper, we propose a comprehensive multi-material and multi-method approach based on the combination of synchrotron radiation X-ray micro-analytical techniques (i.e., X-ray diffraction, X-ray fluorescence and X-ray absorption near edge structure spectroscopy at S K-/Ag L-3-/As K-edges) and vibrational micro-spectroscopy methods to unveil the causes and mechanism of darkening of “fake-gilded” decorations in tempera paintings, originally consisting of an unusual mixture of As2S3 and metallic silver (Ag-0). Such degradation process is a not yet understood phenomenon threatening a series of Old Master paintings, including those by the Italian painters Cimabue and Pietro Lorenzetti. The high specificity, sensitivity and lateral resolution of the employed analytical methods allowed providing first-time evidence for the presence of black acanthite (alpha-Ag2S), mimetite [Pb-5(AsO4)(3)Cl] and syngenite [K2Ca(SO4)(2)center dot H2O] as degradation products of the “fake-gilded” decorations in the Maesta by Cimabue (Church of Santa Maria dei Servi, Bologna, Italy). Furthermore, the study of the painting combined with that of tempera paint mock-ups permitted to explore and define the environmental agents and internal factors causing the darkening, by proving that: (i) Ag-0 and moisture are key-factors for triggering the transformation of As2S3 to alpha-Ag2S and As-oxides; (ii) S2--ions arising from the degradation of As2S3 are the main responsible for the formation of alpha-Ag2S; (iii) light exposure strengthens the tendency of the paint components towards alteration. Based on our findings, we finally propose a degradation mechanism of As2S3/Ag-0-based tempera paints.
Keywords: A1 Journal article; Antwerp X-ray Imaging and Spectroscopy (AXIS)
Impact Factor: 3.4
DOI: 10.1039/D1JA00271F
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“SEM-EDX hyperspectral data analysis for the study of soil aggregates”. Allegretta I, Legrand S, Alfeld M, Gattullo CE, Porfido C, Spagnuolo M, Janssens K, Terzano R, Geoderma: an international journal of soil science 406 (2022). http://doi.org/10.1016/J.GEODERMA.2021.115540
Abstract: Scanning electron microscopy coupled with microanalysis (SEM-EDX) is an important analytical tool for the morphological and chemical characterization of different types of materials. In many applications, SEM-EDX elemental maps are usually used and processed as images, thus flattening and reducing the spectroscopic information contained in EDX hyperspectral data cubes. The exploitation of the full hyperspectral dataset could be indeed very useful for the study of complex matrices like soil. In order to maximize the information attainable by SEM-EDX data cubes analysis, the software package “Datamuncher Gamma” was implemented and applied to study soil aggregates. By using this approach, different phases (silicates, aluminosilicates, Ca-carbonates, Ca-phosphates, organic matter, iron oxides) inside soil aggregates were successfully identified and segmented. The advantages of this method over the common ROI imaging approach are presented. Finally, this method was used to compare different aggregates in a Cr-polluted soil and understand their possible pedological history. The present method can be used for the analysis of every type of SEM-EDX data cubes, allowing its application to different types of samples and fields of study.
Keywords: A1 Journal article; Antwerp X-ray Imaging and Spectroscopy (AXIS)
Impact Factor: 6.1
DOI: 10.1016/J.GEODERMA.2021.115540
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“Synchrotron XRF analysis identifies cerium accumulation colocalized with pharyngeal deformities in CeO₂, NP-exposed caenorhabditis elegans”. Rossbach LM, Brede DA, Nuyts G, Cagno S, Olsson RMS, Oughton DH, Falkenberg G, Janssens K, Lind OC, Environmental science and technology 56, 5081 (2022). http://doi.org/10.1021/ACS.EST.1C08509
Abstract: A combination of synchrotron radiation-based elementalimaging, in vivo redox status analysis, histology, and toxic responses was usedto investigate the uptake, biodistribution, and adverse effects of Cenanoparticles (CeO2NP; 10 nm; 0.5-34.96 mg Ce L-1) or Ce(NO3)3(2.3-26 mg Ce L-1)inCaenorhabditis elegans. Elemental mapping of theexposed nematodes revealed Ce uptake in the alimentary canal prior todepuration. Retention of CeO2NPs was low compared to that of Ce(NO3)3in depurated individuals. X-rayfluorescence (XRF) mapping showed that Cetranslocation was confined to the pharyngeal valve and foregut. Ce(NO3)3exposure significantly decreased growth, fertility, and reproduction, causedslightly reduced fecundity. XRF mapping and histological analysis revealedsevere tissue deformities colocalized with retained Ce surrounding thepharyngeal valve. Both forms of Ce activated the sod-1 antioxidant defense,particularly in the pharynx, whereas no significant effects on the cellular redox balance were identified. The CeO2NP-induceddeformities did not appear to impair the pharyngeal function or feeding ability as growth effects were restricted to Ce(NO3)3exposure. The results demonstrate the utility of integrated submicron-resolution SR-based XRF elemental mapping of tissue-specificdistribution and adverse effect analysis to obtain robust toxicological evaluations of metal-containing contaminants.
Keywords: A1 Journal article; Antwerp X-ray Imaging and Spectroscopy (AXIS)
Impact Factor: 11.4
DOI: 10.1021/ACS.EST.1C08509
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“The “Historical Materials BAG&rdquo, : a new facilitated access to synchrotron X-ray diffraction analyses for cultural heritage materials at the European Synchrotron Radiation Facility”. Cotte M, Gonzalez V, Vanmeert F, Monico L, Dejoie C, Burghammer M, Huder L, de Nolf W, Fisher S, Fazlic I, Chauffeton C, Wallez G, Jimenez N, Albert-Tortosa F, Salvado N, Possenti E, Colombo C, Ghirardello M, Comelli D, Avranovich Clerici E, Vivani R, Romani A, Costantino C, Janssens K, Taniguchi Y, McCarthy J, Reichert H, Susini J, Molecules: a journal of synthetic chemistry and natural product chemistry 27, 1997 (2022). http://doi.org/10.3390/MOLECULES27061997
Abstract: The European Synchrotron Radiation Facility (ESRF) has recently commissioned the new Extremely Brilliant Source (EBS). The gain in brightness as well as the continuous development of beamline instruments boosts the beamline performances, in particular in terms of accelerated data acquisition. This has motivated the development of new access modes as an alternative to standard proposals for access to beamtime, in particular via the “block allocation group” (BAG) mode. Here, we present the recently implemented “historical materials BAG”: a community proposal giving to 10 European institutes the opportunity for guaranteed beamtime at two X-ray powder diffraction (XRPD) beamlines-ID13, for 2D high lateral resolution XRPD mapping, and ID22 for high angular resolution XRPD bulk analyses-with a particular focus on applications to cultural heritage. The capabilities offered by these instruments, the specific hardware and software developments to facilitate and speed-up data acquisition and data processing are detailed, and the first results from this new access are illustrated with recent applications to pigments, paintings, ceramics and wood.
Keywords: A1 Journal article; Antwerp X-ray Imaging and Spectroscopy (AXIS)
Impact Factor: 4.6
DOI: 10.3390/MOLECULES27061997
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“Synchrotron XRF and histological analyses identify damage to digestive tract of uranium NP-exposed Daphnia magna”. Byrnes I, Rossbach LM, Jaroszewicz J, Grolimund D, Sanchez DF, Gomez-Gonzalez MA, Nuyts G, Reinoso-Maset E, Janssens K, Salbu B, Brede DA, Lind OC, Environmental science and technology 57, 1071 (2023). http://doi.org/10.1021/ACS.EST.2C07174
Abstract: Micro-and nanoscopic X-ray techniques were used to investigate the relationship between uranium (U) tissue distributions and adverse effects to the digestive tract of aquatic model organism Daphnia magna following uranium nanoparticle (UNP) exposure. X-ray absorption computed tomography measure-ments of intact daphnids exposed to sublethal concentrations of UNPs or a U reference solution (URef) showed adverse morphological changes to the midgut and the hepatic ceca. Histological analyses of exposed organisms revealed a high proportion of abnormal and irregularly shaped intestinal epithelial cells. Disruption of the hepatic ceca and midgut epithelial tissues implied digestive functions and intestinal barriers were compro-mised. Synchrotron-based micro X-ray fluorescence (XRF) elemental mapping identified U co-localized with morphological changes, with substantial accumulation of U in the lumen as well as in the epithelial tissues. Utilizing high-resolution nano-XRF, 400-1000 nm sized U particulates could be identified throughout the midgut and within hepatic ceca cells, coinciding with tissue damages. The results highlight disruption of intestinal function as an important mode of action of acute U toxicity in D. magna and that midgut epithelial cells as well as the hepatic ceca are key target organs.
Keywords: A1 Journal article; Antwerp X-ray Imaging and Spectroscopy (AXIS)
Impact Factor: 11.4
DOI: 10.1021/ACS.EST.2C07174
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“Multi-scale X-ray imaging of the pigment discoloration processes triggered by chlorine compounds in the Upper Basilica of Saint Francis of Assisi”. Avranovich Clerici E, De Meyer S, Vanmeert F, Legrand S, Monico L, Miliani C, Janssens K, Molecules: a journal of synthetic chemistry and natural product chemistry 28, 6106 (2023). http://doi.org/10.3390/MOLECULES28166106
Abstract: In this paper, the chromatic alteration of various types of paints, present on mural painting fragments derived from the vaults of The Upper Basilica of Saint Francis of Assisi in Italy (12th-13th century), is studied using synchrotron radiation. Six painted mural fragments, several square centimeters in size, were available for analysis, originating from the ceiling paintings attributed to Cimabue and Giotto; they correspond to originally white, blue/green, and brown/yellow/orange areas showing discoloration. As well as collecting macroscopic X-ray fluorescence and diffraction maps from the entire fragments in the laboratory and at the SOLEIL synchrotron, corresponding paint cross-sections were also analyzed using microscopic X-ray fluorescence and powder diffraction mapping at the PETRA-III synchrotron. Numerous secondary products were observed on the painted surfaces, such as (a) copper tri-hydroxychloride in green/blue areas; (b) corderoite and calomel in vermillion red/cinnabar-rich paints; (c) plattnerite and/or scrutinyite assumed to be oxidation products of (hydro)cerussite (2PbCO(3)center dot Pb(OH)(2)) in the white areas, and (d) the calcium oxalates whewellite and weddellite. An extensive presence of chlorinated metal salts points to the central role of chlorine-containing compounds during the degradation of the 800-year-old paint, leading to, among other things, the formation of the rare mineral cumengeite (21PbCl(2)center dot 20Cu(OH) (2) center dot 6H(2)O).
Keywords: A1 Journal article; Antwerp X-ray Imaging and Spectroscopy (AXIS)
Impact Factor: 4.6
DOI: 10.3390/MOLECULES28166106
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“Two pathways for the degradation of orpiment pigment (As₂S₃) found in paintings”. Broers FTH, Janssens K, Weker JN, Webb SM, Mehta A, Meirer F, Keune K, Journal of the American Chemical Society 145, 8847 (2023). http://doi.org/10.1021/JACS.2C12271
Abstract: Paintings are complex objects containing many different chemical compounds that can react over time. The degradation of arsenic sulfide pigments causes optical changes in paintings. The main degradation product was thought to be white arsenolite (As2O3), but previous research also showed the abundant presence of As(V) species. In this study, we investigate the influence of the presence of a medium on the degradation mechanism of orpiment (As2S3) using synchrotron radiation (SR)-based tomographic transmission X-ray microscopy, SR-based micro-X-ray fluorescence, and Xray absorption near edge structure spectroscopy. Upon direct illumination of dry orpiment powder using UV-visible light, only the formation of As2O3 was observed. When As2S3 was surrounded by a medium and illuminated, As2O3 was only observed in the area directly exposed to light, while As(V) degradation species were found elsewhere in the medium. Without accelerated artificial light aging, As(V)(aq) species are formed and migrate throughout the medium within weeks after preparation. In both scenarios, the As(V) species form via intermediate As(III)(aq) species and the presence of a medium is necessary. As(V)(aq) species can react with available cations to form insoluble metal arsenates, which induces stress within the paint layers (leading to, e.g., cracks and delamination) or can lead to a visual change of the image of the painting.
Keywords: A1 Journal article; Antwerp X-ray Imaging and Spectroscopy (AXIS)
Impact Factor: 15
DOI: 10.1021/JACS.2C12271
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“Darkening of lead white in old master drawings and historic prints : a multi-analytical investigation”. Pastorelli G, Miranda ASO, Avranovich Clerici E, d'Imporzano P, Hansen BV, Janssens K, Davies GR, Borring N, Microchemical journal 199, 109912 (2024). http://doi.org/10.1016/J.MICROC.2024.109912
Abstract: Old master drawings and historic prints often feature white highlights, which are typically painted using lead white, one of the most widely used historical white pigments. However, it has been observed that many of these highlights discolour over time, becoming dark brown or black due to unclear degradation processes. This phenomenon not only misrepresents the original artefacts, threatening their suitability for public display, but also diminishes their longevity. To ensure their preservation, it is essential to determine why some lead white highlights in these museum objects retain their light tones while others are prone to darkening. The objective of this study was to identify the relationships between the composition, provenance, and production methods of lead white pigments, and their role in the discolouration observed on drawings, lithographs and early photographs. Selected samples and artefacts were examined using a range of analytical techniques, namely X-ray fluorescence spectroscopy (XRF), X-ray powder diffraction (XRPD), and lead isotope analysis. While XRF analyses confirmed the presence of lead as the primary element in the majority of the highlights, XRPD measurements identified a variety of lead compounds such as the carbonates cerussite and hydrocerussite alongside galena-a black crystalline sulfide-and lead sulfates. Additionally, isotope analyses classified the lead raw materials into five main groups. Through these measurements, the examined lead white pigments were categorised based on their compositional properties in relation to the raw materials used, as well as their geographical and temporal origin. A significant finding is that lead white pigments from different production periods, spanning from older to more modern, may be characterised by varying proneness to discolouration irrespective of their provenance.
Keywords: A1 Journal article; Antwerp X-ray Imaging and Spectroscopy (AXIS)
Impact Factor: 4.8
DOI: 10.1016/J.MICROC.2024.109912
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“Chemical mapping of the degradation of geranium lake in paint cross sections by MALDI-MSI”. Alvarez-Martin A, Quanico J, Scovacricchi T, Avranovich Clerici E, Baggerman G, Janssens K, Analytical chemistry 95, 18215 (2023). http://doi.org/10.1021/ACS.ANALCHEM.3C03992
Abstract: Matrix assisted laser desorption ionization-mass spectrometry imaging (MALDI-MSI) has become a powerful method to extract spatially resolved chemical information in complex materials. This study provides the first use of MALDI-MSI to define spatial–temporal changes in oil paints. Due to the highly heterogeneous nature of oil paints, the sample preparation had to be optimized to prevent molecules from delocalizing. Here, we present a new protocol for the layer-specific analysis of oil paint cross sections achieving a lateral resolution of 10 μm and without losing ionization efficiency due to topographic effects. The efficacy of this method was investigated in oil paint samples containing a mixture of two historic organic pigments, geranium lake and lead white, a mixture often employed in the work of painter Vincent Van Gogh. This methodology not only allows for spatial visualization of the molecules responsible for the pink hue of the paint but also helps to elucidate the chemical changes behind the discoloration of paintings with this composition. The results demonstrate that this approach provides valuable molecular compositional information about the degradation pathways of pigments in specific paint layers and their interaction with the binding medium and other paint components and with light over time. Since a spatial correlation between molecular species and the visual pattern of the discoloration pattern can be made, we expect that mass spectrometry imaging will become highly relevant in future degradation studies of many more historical pigments and paints.
Keywords: A1 Journal article; Antwerp X-ray Imaging and Spectroscopy (AXIS); Ecosphere
Impact Factor: 7.4
DOI: 10.1021/ACS.ANALCHEM.3C03992
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“The dark halo technique in the oeuvre of Michael Sweerts and other Flemish and Dutch baroque painters. A 17th c. empirical solution to mitigate the optical 'simultaneous contrast' effect?”.Derks K, van der Snickt G, Legrand S, van der Stighelen K, Janssens K, Heritage science 10, 5 (2022). http://doi.org/10.1186/S40494-021-00634-W
Abstract: Although the topic is rarely addressed in literature, a significant number of baroque paintings exhibit dark, halo-like shapes around the contours of the dramatis personae. Close examination of both finished and unfinished works suggests that this intriguing feature was a practical tool that helped the artist in the early painting stages. When applying the final brushwork, the halo lost its function, with some artists undertaking efforts to hide it. Although their visibility might not have been intended by the artists, today this dark paint beneath the surface is partially visible through the upper paint layers. Moreover, the disclosure of many halos using infrared photography (IRP), infrared reflectography (IRR) and macro X-ray fluorescence imaging (MA-XRF), additional to those that can be observed visually, suggests that this was a common and established element of 17th-century painting practice in Western Europe. Building on an existing hypothesis, we argue that halos can be considered as a solution to an optical problem that arose when baroque painters reversed the traditional, 15th- and 16th-century painting sequence of working from background to foreground. Instead, they started with the dominant parts of a composition, such as the face of a sitter. In that case, a temporary halo can provide the essential tonal reference to anticipate the chromatic impact of the final dark colored background on the adjacent delicate carnations. In particular, we attempt to clarify the prevalence of dark halos as a response to optical effects such as 'simultaneous contrast' and 'the crispening effect', described in literature only centuries later. As such, the recently termed 'ring condition' can be seen as the present-day equivalent of the 'halo solution' that was seemingly empirically or intuitively developed by 17th-century artists. Modern studies in visual perception proves that by laying a black ring around a target color, the optical impact of a surrounding color can be efficiently neutralized. Finally, by delving into works by Michael Sweerts, it becomes clear that resourceful artists might have adapted the halo technique and the underlying principles to their individual challenges, such as dealing with differently colored grounds.
Keywords: A1 Journal article; Art; Antwerp Cultural Heritage Sciences (ARCHES); Antwerp X-ray Imaging and Spectroscopy (AXIS)
Impact Factor: 2.5
DOI: 10.1186/S40494-021-00634-W
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“Combined macro X-ray fluorescence (MA-XRF) and pulse phase thermography (PPT) imaging for the technical study of panel paintings”. Deleu N, Hillen M, Steenackers G, Borms G, Janssens K, Van der Stighelen K, Van der Snickt G, Talanta : the international journal of pure and applied analytical chemistry 270, 125533 (2024). http://doi.org/10.1016/J.TALANTA.2023.125533
Abstract: Museum staff usually relies on a proven combination of X-ray radiography (XRR) and infrared reflectography (IRR) to study paintings in a non-destructive manner. In the last decades, however, the research toolbox of heritage scientists has expanded considerably, with a prime example being macro X-ray fluorescence (MA-XRF), producing element-specific images. The goal of this article is to illustrate the added value of augmenting MA-XRF with pulse phase thermography (PPT), a variant of active infrared thermographic imaging (IRT), which is an innovative diagnostic method that is able to reveal variations between or in materials, based on a different response to minor fluctuations in temperature when irradiated with optical radiation. By examining three 16thand 17th-century panel paintings we assess the extent in which combined MA-XRF and PPT contributes to a better understanding of two commonly encountered interventions to panel paintings: (a) Anstuckungen (enlargement of the panel) or (b) substitutions (replacement of part of the panel). Yielding information from different depths of the painting, these two techniques proved highly complementary with IRR and XRR, expanding the understanding of the build-up, genesis, and material history of the paintings. While MA-XRF documented the interventions to the wooden substrate indirectly by revealing variations in painting materials, paint handling and/ or layer sequence between the original part and the extended or replaced planks, PPT proved beneficial for the study of the wooden support itself, by providing a clear image of the wood structure quasi-free of distortion by the superimposed paint or cradling. XRR, on the other hand, revealed other features from the wood structure, not visible with PPT, and allowed looking through the wooden panels, revealing e.g. the dowels used for joining the planks. Additionally, IRR visualised dissimilarities in the underdrawings. In this way, the results indicate that PPT has the potential to become an acknowledged add-on to the expanding set of imaging methods for paintings, especially when used in combination with MA-XRF, IRR and XRR.
Keywords: A1 Journal article; Art; Antwerp Cultural Heritage Sciences (ARCHES); Antwerp X-ray Imaging and Spectroscopy (AXIS)
Impact Factor: 6.1
DOI: 10.1016/J.TALANTA.2023.125533
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“The synergistic influence of metal cations on the drying and viscosity of linseed oil assessed by means of model samples containing synthesised metal carboxylates”. Kirkpatrick S, Sanyova J, Janssens K, van der Snickt G, Heritage science 12, 209 (2024). http://doi.org/10.1186/S40494-024-01309-Y
Abstract: The recent multi-analytical study carried out on the Van Eyck's Ghent Altarpiece showed the simultaneous presence of several kinds of metal carboxylates in oil-rich glaze layers. This outcome raised the question whether these carboxylates had already formed during the preparation of the oil binder by the artists. In the case of early-stage formation, they may have had an impact on the drying rate of the resulting oil, as well as on its handling properties. This hypothesis was investigated using a model system of in-house-prepared linseed oil containing incremental concentrations (2-5-10 wt.%) of relevant metal carboxylates (i.e. Ca-, Zn-, Cu-, and Pb oleates and stearates). This paper describes the influence of these type of molecules on the drying rate of linseed oil and, to an extent, on its viscosity. The drying time of the linseed oil, to which one or more metal carboxylates were added, was measured with a drying recorder while the viscosity was assessed with a rheometer. When introduced together, some of these metal carboxylates act in synergy to shorten the drying time with respect to the situation when the same metal carboxylates were added separately to linseed oil. Mixtures of Ca- and Zn-oleates proved to have a larger effect than other binary combinations. Addition of two metal oleates (combination of Ca/Zn/Cu/Pb) reduced the drying time even more. On the other hand, specific combinations of three metal stearates and/or oleates also demonstrated a significant synergistic effect towards increasing the viscosity of the binder. Especially combinations of Ca/Zn/Cu and Ca/Zn/Pb stearates and oleates gave rise to the highest level of linseed oil viscosity increase, when compared to the situation in which the same metal carboxylates were added separately.
Keywords: A1 Journal article; Art; Antwerp Cultural Heritage Sciences (ARCHES); Antwerp X-ray Imaging and Spectroscopy (AXIS)
Impact Factor: 2.5
DOI: 10.1186/S40494-024-01309-Y
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“Lead(II) formate in Rembrandt's Night Watch : detection and distribution from the macro- to the micro-scale”. Gonzalez V, Fazlic I, Cotte M, Vanmeert F, Gestels A, De Meyer S, Broers F, Hermans J, van Loon A, Janssens K, Noble P, Keune K, Angewandte Chemie: international edition in English , 1 (2023). http://doi.org/10.1002/ANIE.202216478
Abstract: The Night Watch, painted in 1642 and on view in the Rijksmuseum in Amsterdam, is considered Rembrandt's most famous work. X-ray powder diffraction (XRPD) mapping at multiple length scales revealed the unusual presence of lead(II) formate, Pb(HCOO)(2), in several areas of the painting. Until now, this compound was never reported in historical oil paints. In order to get insights into this phenomenon, one possible chemical pathway was explored thanks to the preparation and micro-analysis of model oil paint media prepared by heating linseed oil and lead(II) oxide (PbO) drier as described in 17(th) century recipes. Synchrotron radiation based micro-XRPD (SR-mu-XRPD) and infrared microscopy were combined to identify and map at the micro-scale various neo-formed lead-based compounds in these model samples. Both lead(II) formate and lead(II) formate hydroxide Pb(HCOO)(OH) were detected and mapped, providing new clues regarding the reactivity of lead driers in oil matrices in historical paintings.
Keywords: A1 Journal article; Art; Antwerp X-ray Imaging and Spectroscopy (AXIS)
Impact Factor: 16.6
DOI: 10.1002/ANIE.202216478
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“Discovery of pararealgar and semi-amorphous pararealgar in Rembrandt's The Night Watch : analytical study and historical contextualization”. De Keyser N, Broers FTH, Vanmeert F, van Loon A, Gabrieli F, De Meyer S, Gestels A, Gonzalez V, Hermens E, Noble P, Meirer F, Janssens K, Keune K, Heritage science 12, 237 (2024). http://doi.org/10.1186/S40494-024-01350-X
Abstract: This article reports on the discovery of pararealgar and semi-amorphous pararealgar in Rembrandt's masterpiece The Night Watch. A large-scale research project named Operation Night Watch was started in 2019. A variety of non-invasive analytical imaging techniques, together with paint sample research, has provided new information about Rembrandt's pigments, materials, and techniques as well as the current condition of the painting. Macroscopic X-ray fluorescence, macroscopic X-ray powder diffraction and reflectance imaging spectroscopy identified the presence of arsenic sulfide pigments and degradation products of these pigments in the doublet sleeves and embroidered buff coat worn by Lieutenant Willem van Ruytenburch (central figure to the right of Captain Frans Banninck Cocq). Examination by light microscopy of two paint samples taken from this area shows a mixture of large sharp-edged tabular yellow and orange to red pigment particles, and scanning electron microscopy-energy dispersive X-ray analysis identified these particles as containing arsenic and sulfur. Using micro-Raman spectroscopy, the yellow particles were identified as pararealgar, and the orange to red particles as semi-amorphous pararealgar. Synchrotron-based X-ray diffraction allowed visualization of the presence of multiple degradation products associated with arsenic sulfides throughout the paint layer. The discovery of pararealgar and semi-amorphous pararealgar is a new addition to Rembrandt's pigment palette. To contextualize our findings and to hypothesize why, how, and where Rembrandt obtained the pigments, we studied related historical sources. A comprehensive review of historical sources gives insight into the types of artificial arsenic sulfides that were available and suggests that a broader range of arsenic pigments could have been available in Amsterdam in the seventeenth century than previously thought. This is supported by the use of a very similar mixture of pigments by Willem Kalf (1619-1693), a contemporary artist based in Amsterdam. Together with the condition of the particles in the paint cross sections, this brings us to the conclusion that Rembrandt intentionally used pararealgar and semi-amorphous pararealgar, together with lead-tin yellow and vermilion, to create an orange paint.
Keywords: A1 Journal article; Art; Antwerp X-ray Imaging and Spectroscopy (AXIS)
Impact Factor: 2.5
DOI: 10.1186/S40494-024-01350-X
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“Artificial orpiment, a new pigment in Rembrandt's palette”. van Loon A, Noble P, Krekeler A, van der Snickt G, Janssens K, Abe Y, Nakai I, Dik J, Heritage science 5, 26 (2017). http://doi.org/10.1186/S40494-017-0138-1
Abstract: This paper reports on how the application of macro X-ray fluorescence (MA-XRF) imaging, in combination with the re-examination of existing paint cross-sections, has led to the discovery of a new pigment in Rembrandt's palette: artificial orpiment. In the NWO Science4Arts 'ReVisRembrandt' project, novel chemical imaging techniques are being developed and applied to the study of Rembrandt's late paintings in order to help resolve outstanding questions and to gain a better understanding of his late enigmatic painting technique. One of the selected case studies is the Portrait of a Couple as Isaac and Rebecca, known as 'The Jewish Bride', dated c. 1665 and on view in the Rijksmuseum. During the re-installation of the Rijksmuseum in 2013, the picture was scanned using the Bruker M6 Jetstream MAXRF scanner. The resulting elemental distribution maps made it possible to distinguish many features in the painting, such as bone black remains of the original hat (P, Ca maps), and the now discolored smalt-rich background (Co, Ni, As, K maps). The arsenic (As) map also revealed areas of high-intensity in Isaac's sleeve and Rebecca's dress where it could be established that it was not related with the pigment smalt that also contains arsenic. This pointed to the presence of a yellow or orange arsenic-containing pigment, such as realgar or orpiment that is not associated with the artist's palette. Subsequent examination of existing paint cross-sections from these locations taken by Karin Groen in the 1990s identified isolated, almost perfectly round particles of arsenic sulfide. The round shape corresponds with published findings on a purified form of artificial orpiment glass obtained by dry processing, a sublimation reaction. In bright field, the particles characteristically exhibit a dark cross in the middle caused by internal light reflections. The results of additional non-invasive techniques (portable XRD and portable Raman) are discussed, as well as the implications of this finding and how it fits with Rembrandt's late experimental painting technique.
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 6
DOI: 10.1186/S40494-017-0138-1
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“Characterization of the main causes of deterioration of grisaille paint layers in 19th C. stained-glass windows by J.-B. Capronnier”. Schalm O, Janssens K, Caen J, Spectrochimica acta: part B : atomic spectroscopy 58, 589 (2003). http://doi.org/10.1016/S0584-8547(02)00282-3
Abstract: Twenty-seven glass fragments containing dark coloured grisaille paint layers of different qualities were collected from ten windows of the cathedral St. Michael & St. Gudule in Brussels (Belgium). The windows were made by J.-B. Capronnier (18141891) and cover the period between 1843 and 1878. The samples were cross-sectioned and examined in an electron microscope. Grisaille paint layers are not homogeneous and therefore, it is not meaningful to characterize them in terms of their average composition. Instead, parameters such as granularity, the number of residual gas bubbles per running millimetre of paint, the type of pigments, and the thickness of the paint layer were used to characterize them. The microscopic morphology allows a classification of the grisaille paint layers in four groups, every group associated with a quality level. Moreover, the main causes of the accelerated degradation of some of these paint layers could be explained. The classification made it possible to distinguish two periods in the work of Capronnier: (1) the early period (18431848) is characterized by the presence of either single granular paint layers or of double-layered systems consisting of a granular paint layer on top of a well-melted paint layer. The granular grisaille paint layers tend to pulverize; (2) the later period (18481878) is characterized by the presence of only well-vitrified paint layers. No sign of deterioration was found on the well-vitrified paint layers.
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.241
DOI: 10.1016/S0584-8547(02)00282-3
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“Identification of artificial orpiment in the interior decorations of the Japanese tower in Laeken, Brussels, Belgium”. Vermeulen M, Sanyova J, Janssens K, Heritage science 3, Unsp 9 (2015). http://doi.org/10.1186/S40494-015-0040-7
Abstract: In this paper, we used a multi-technique approach in order to identify the arsenic sulfide pigment used in the decorative panels of the Japanese tower in Laeken, Belgium. Our attention was drawn to this particular pigment because of its relatively good conservation state, despite its known tendency to fade over time when exposed to light. The pigment was used with different painting techniques, bound with oil and urushi in the lacquers and with an aqueous binder in the mat relief panels. In the latter case it is always applied as an underlayer mixed with ultramarine blue. This quite unusual pigment mixture also shows a good state of preservation. In this study, the orpiment used for the Japanese tower has been identified as an amorphous arsenic sulfide glass (AsxSx) with the aid of light microscopy, PLM, SEM-EDX and Raman microscopy. The pigment features different degrees of As4S4 monomer units in its structure, also known as realgar-like nano-phases. This most likely indicates different synthesis processes as the formation of these As4S4 monomers is dependent of the quenching temperature (Tq) to which the artificial pigment is exposed during the preparation phase.
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 17
DOI: 10.1186/S40494-015-0040-7
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“Integrated X-ray fluorescence and diffuse visible-to-near-infrared reflectance scanner for standoff elemental and molecular spectroscopic imaging of paints and works on paper”. Delaney JK, Conover DM, Dooley KA, Glinsman L, Janssens K, Loew M, Heritage science 6, 31 (2018). http://doi.org/10.1186/S40494-018-0197-Y
Abstract: Prior studies have shown the improved ability to identify artists' pigments by combining results from X-ray fluorescence (XRF), which provides elemental information, with reflectance spectroscopy in the visible to near infrared (400-1000 nm) that provides information on electronic transitions. Extending the spectral range of reflectance spectroscopy into the UV, 350-400 nm, allows identification of several white pigments since their electronic transitions occur in this region (e.g., zinc white and rutile and anatase forms of titanium white). Extending the range further into the infrared, out to 2500 nm, provides information on vibrational transitions of various functional groups, such as hydroxyl, carbonate, and methyl groups. This allows better identification of mineral-based pigments and some paint binders. The combination of elemental information with electronic and vibrational transitions provides a more robust method to identify artists' materials in situ. The collection of both sets of spectral information across works of art, such as paintings and works on paper, allows generating a more complete map of artists' materials. Here, we describe a 2-D scanner that simultaneously collects XRF spectra and reflectance spectra from 350 to 2500 nm across the surfaces of works of art. The scanner consists of a stationary, single pixel XRF spectrometer and fiber optic reflectance spectrometer along with a 2-D position-controlled easel that moves the artwork in front of the two detection systems. The dual-mode scanner has been tested on a variety of works of art from illuminated manuscripts (0.1 x 0.1 m(2)) to paintings as large as 1.7 x 1.9 m(2). The scanner is described and two sets of results are presented. The first is the XRF scanning of a large warped panel painting by Andrea del Sarto titled Charity. The second is a combined XRF and reflectance scan of Georges Seurat's painting titled Haymakers at Montfermeil. The XRF was collected at 1 mm spatial sampling and the reflectance spectral data at 3 mm. Combining the results from the data sets was found to enhance the identification of pigments as well as yield distribution maps, in spite of the relatively low reflectance spatial sampling. The elemental and reflectance maps allowed the identification and mapping of lead white, cobalt blue, viridian, ochres, and likely chrome yellow. The maps also provide information on the mixing of pigments. While the reflectance image cube has 10-20x larger spatial samples than desired, the elimination of having to use two hyperspectral cameras to cover the range from 400 to 2500 nm makes for a low cost dual modality scanner.
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 7
DOI: 10.1186/S40494-018-0197-Y
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“An intrusive portrait by Goya”. Bull D, Krekeler A, Alfeld M, Dik J, Janssens K, The Burlington magazine 153, 668 (2011)
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“Jan Davidsz. de Heem (1606-1684): a technical examination of fruit and flower still lifes combining MA-XRF scanning, cross-section analysis and technical historical sources”. De Keyser N, van der Snickt G, Van Loon A, Legrand S, Wallert A, Janssens K, Heritage science 5, 38 (2017). http://doi.org/10.1186/S40494-017-0151-4
Abstract: This article discusses the technical examination of five flower and fruit still life paintings by the seventeenth century artist Jan Davidsz. de Heem (1606-1684). The painter is known for his meticulously composed and finely detailed still life paintings and is a master in imitating the surface textures of various fruits, flowers, and objects. Macro X-ray fluorescence (MA-XRF) scanning experiments were supplemented with a study of paint cross-sections and contemporary art technical sources with the aim of reconstructing the complex build-up of the overall lay-in of the composition and individual subjects. MA-XRF provided information on the distribution of key chemical elements present in painting materials and made it possible to recapture evidence of the different phases in the artist's working methods: from the application of the ground layers, to De Heem's characteristic oval-shaped underpaintings, and finally, the superposition of multiple paint layers in the working up of the paintings. SEM-EDX analysis of a limited number of paint cross-sections complemented the chemical images with local and layer-specific information on the microscale, providing more accuracy on the layer sequence and enabling the study of elements with a low atomic number for which the non-invasive technique is less sensitive. The results from this technical examination were in addition compared with recipes and paint instructions, to obtain a better understanding of the relation between the general practice and actual painting technique of Jan Davidsz. de Heem. Ultimately, this combined approach uncovered new information on De Heem's artistic practice and demonstrated the complementarity of the methods.
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 5
DOI: 10.1186/S40494-017-0151-4
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“MA-XRF imaging on Rene Magritte's La condition humaine : insights into the artist's palette and technique and the discovery of a third quarter of La pose enchantee”. da Silva AT, Legrand S, van der Snickt G, Featherstone R, Janssens K, Bottinelli G, Heritage science 5, 37 (2017). http://doi.org/10.1186/S40494-017-0150-5
Abstract: Magritte's composition La condition humaine, 1935 was found to conceal under its paint layers an entire quarter of a lost composition by the artist, until recently only known from a small black/white catalogue illustration-La pose enchantee, 1927. This study is the latest contribution to the discovery of the artist's missing painting, now known to have been cut into four parts and re-used by Magritte as the support for new compositions. Non-destructive analytical and examination methods and specifically macroscopic X-ray fluorescence (MAXRF) scanning and conventional X-ray radiography (XRR) were the two non-destructive analytical and examination methods used to study both compositions and add to the existing knowledge on the artist's palette during both periods. The first method is capable of identifying the presence and the distribution of key chemical elements present in artists' materials. In some instances elemental mapping provided useful information on the hidden painting, but conventional X-ray radiography (XRR) enabled a better visualisation of the form and paint application of the underlying composition. Furthermore, the turnover edges of the canvas reveal after over 80 years the artist's palette directly to the viewer. Additional XRF scanning of this exposed paint has confirmed and added to the existing research published to date of this lost painting, including a proposed colour reconstruction, but at the same time highlighting the need for further analytical research involving both non-destructive point analysis and the use of paint samples.
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 7
DOI: 10.1186/S40494-017-0150-5
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“A methodology for the identification of glass panes of different origin in a single stained glass window: application on two 13th century windows”. Schalm O, de Raedt I, Caen J, Janssens K, Journal of cultural heritage 11, 487 (2010). http://doi.org/10.1016/J.CULHER.2010.05.004
Abstract: The chemical composition of 11 glass panes originating from two 13th century non-figurative windows were analyzed by means of Scanning Electron MicroscopyEnergy Dispersive X-ray system (SEM-EDX). The windows were discovered in the back-wall of the triforium during the restoration of the choir of the cathedral St. Michael and St. Gudule in Brussels (Belgium). In order to determine if these windows were fabricated with glass of different origin or not, the compositional difference between the panes were compared with the variation in composition as a result of the following causes: (1) compositional fluctuation between panes cut from the same sheet of glass, (2) compositional fluctuation caused when panes are cut from different sheets that were made with the same batch, (3) compositional fluctuation caused when the glass is made from different batches at the same production center, and (4) compositional fluctuation as a result of glass produced at different fabrication centers.
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 1.838
Times cited: 7
DOI: 10.1016/J.CULHER.2010.05.004
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“Rembrandt's An Old Man in Military Costume : combining hyperspectral and MA-XRF imaging to understand how two paintings were painted on a single panel”. MacLennan D, Trentelman K, Szafran Y, Woollett AT, Delaney JK, Janssens K, Dik J, Journal of the American Institute for Conservation 58, 54 (2019). http://doi.org/10.1080/01971360.2018.1540245
Abstract: Over the past several decades the painting An Old Man in Military Costume by Rembrandt Harmensz van Rijn (ca. 1630-31; J. Paul Getty Museum, 78.PB.246) has been the subject of a number of investigations carried out in order to better visualize a second painting beneath the surface figure. The underlying image – the head and shoulders of a man wearing a cloak – is oriented 180 degrees from the upper image and appears to be fairly complete. Scanning macro x-ray fluorescence (XRF) spectroscopy reveals the face is painted with lead white and a mercury-containing pigment (likely vermilion), and the cloak is painted with a copper-containing pigment. Following the revelation and digital color reconstruction of the underlying figure, a number of questions still remained. Here, through the use of infrared reflectance imaging spectroscopy (i.e., hyperspectral imaging) and macro-XRF imaging spectroscopy, together with cross-sections taken from targeted areas, the sequence of painting in both compositions was explored. Of particular interest was the discovery of evidence of multiple attempts to situate the lower figure, and the subsequent application of a blocking-out layer over the lower figure before the artist rotated the panel and executed the upper figure. In addition, examination of the placement of the two images on the panel adds to our understanding of the subtle complexities of Rembrandt's working process. RESUMEAu cours des dernieres decennies, la peinture Le vieil homme en costume militaire de Rembrandt Harmensz van Rijn (ca. 1630-31; J. Paul Getty Museum, 78.PB.246) a fait l'objet de nombreuses investigations menees dans le but de mieux visualiser une seconde peinture dissimulee sous la surface. L'image sous-jacente – la tete et les epaules d'un homme vetu d'une cape – est orientee a 180 degres de de l'image du vieil homme, et elle semble assez complete. La spectroscopie a macro-balayage de fluorescence X (MA-XRF) revele que le visage est peint avec du blanc de plomb et un pigment contenant du mercure (comme le vermillon), et que la cape est peinte avec un pigment a base de cuivre. Plusieurs questions restaient en suspens suite a cette decouverte et a la reconstruction numerique en couleur de l'image sous-jacente. Grace a l'emploi de techniques d'imagerie comme la spectroscopie proche infrarouge (ex., imagerie hyperspectrale) et l'imagerie MA-XRF, combinees a l'analyse de coupes stratigraphiques prelevees a des endroits cibles, on a pu explorer la sequence d'application des couches picturales de chacune des deux compositions. Une decouverte particulierement interessante est la preuve que l'artiste a fait plusieurs tentatives pour positionner la figure sous-jacente puis, a ensuite applique une couche pour la recouvrir completement avant de faire pivoter le panneau et peindre la figure du vieil homme. De plus, l'examen du positionnement des deux images sur le panneau ajoute a notre comprehension de la subtile complexite du processus de creation de Rembrandt. Traduit par Elisabeth Forest. RESUMONas ultimas decadas, a pintura Um Velho em Traje Militar, de Rembrandt Harmensz van Rijn (ca. 1630-31; J. Paul Getty Museum, 78.PB.246), foi objeto de uma serie de investigacoes realizadas para visualizar melhor uma segunda pintura abaixo da figura aparente. A imagem subjacente – a cabeca e os ombros de um homem usando uma capa – e orientada a 180 graus da imagem superior e parece estar bastante completa. O macro mapeamento de imagem por espectroscopia de fluorescencia de raios X (FRX) revela que a face e pintada com branco de chumbo e um pigmento contendo mercurio (provavelmente vermelhAo), e a capa e pintada com um pigmento contendo cobre. Apos a descoberta e reconstrucAo digital da cor da figura subjacente, uma serie de questoes ainda permanecem. EntAo, atraves da utilizacAo do mapeamento por imagem de espectroscopia de refletancia por infravermelhos (i.e. mapeamento hiperespectral) e macro mapeamento por imagem de FRX, juntamente com cortes estratigraficos de amostras retiradas de areas de interesse, a pintura em ambas as composicoes foi explorada. De particular interesse foi a descoberta de evidencias de multiplas tentativas de posicionar a figura subjacente, e a subsequente aplicacAo de uma camada intermediaria de separacAo sobre a figura inferior antes do artista girar o painel e executar a figura superior. Alem disso, o exame da colocacAo das duas imagens no painel aumenta nossa compreensAo das sutis complexidades do processo de trabalho de Rembrandt. Traduzido por Marcia Rozzi e Beatriz Haspo. RESUMENA lo largo de las ultimas decadas, la pintura Un anciano con traje militar de Rembrandt Harmensz van Rijn (ca. 1630-31; J. Paul Getty Museum, 78.PB.246) ha sido objeto de varias investigaciones realizadas con el fin de visualizar mejor una segunda pintura debajo de la figura de la superficie. La imagen subyacente, la cabeza y los hombros de un hombre que lleva una capa, esta orientada a 180 grados de la imagen superior y parece estar bastante completa. La espectroscopia de fluorescencia de rayos X (XRF) de barrido revela que la cara esta pintada con blanco de plomo y un pigmento que contiene mercurio (probablemente bermellon), y la capa esta pintada con un pigmento que contiene cobre. Tras la revelacion y la reconstruccion digital del color de la figura subyacente, aun quedaban algunas preguntas. Aqui, por medio del uso de la espectroscopia de imagenes de reflectancia infrarroja (es decir, imagenes hiperespectrales) e imagenes macro-XRF, junto con las secciones transversales tomadas de areas especificas, se exploro la secuencia de pintura en ambas composiciones. De particular interes fue el descubrimiento de evidencia de multiples intentos de situar la figura inferior, y la aplicacion posterior de una capa de bloqueo sobre la figura inferior antes de que el artista rotara el panel y ejecutara la figura superior. Ademas, el examen de la colocacion de las dos imagenes en el panel contribuye a nuestra comprension de las sutiles complejidades del proceso de trabajo de Rembrandt. Traduccion: Amparo Rueda.
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 2
DOI: 10.1080/01971360.2018.1540245
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“Separating two painting campaigns in Saul and David, attributed to Rembrandt, using macroscale reflectance and XRF imaging spectroscopies and microscale paint analysis”. Dooley KA, Gifford EM, van Loon A, Noble P, Zeibel JG, Conover DM, Alfeld M, van der Snickt G, Legrand S, Janssens K, Dik J, Delaney JK, Heritage science 6, 46 (2018). http://doi.org/10.1186/S40494-018-0212-3
Abstract: Late paintings of Rembrandt van Rijn (1606-1669) offer intriguing problems for both art historians and conservation scientists. In the research presented here, the key question addressed is whether observed stylistic differences in paint handling can be correlated with material differences. In Saul and David, in the collection of the Royal Picture Gallery Mauritshuis in The Hague, NL, the stylistic differences between the loose brushwork of Saul's cloak and the more detailed depiction of his turban and the figure of David have been associated with at least two painting stages since the late 1960s, but the attribution of each stage has been debated in the art historical literature. Stylistic evaluation of the paint handling in the two stages, based on magnified surface examination, is further described here. One of the research goals was to determine whether the stylistic differences could be further differentiated with macroscale and microscale methods of material analysis. To address this, selected areas of the painting having pronounced stylistic differences were investigated with two macroscopic chemical imaging methods, X-ray fluorescence and reflectance imaging spectroscopies. The pigments used were identified and their spatial distribution was mapped. The mapping results show that the passages rendered in more detail and associated stylistically with the first painting stage, such as the orange-red color of David's garment or the Greek key design in Saul's turban, were painted with predominately red ochre mixed with vermilion. The regions of loose, bold brushwork, such as the orange-red slashing strokes in the interior of Saul's cloak, associated with the second painting stage, were painted with predominately red ochre without vermilion. These macroscale imaging results were confirmed and extended with scanning electron microscopy with energy-dispersive X-ray spectroscopy (SEM-EDX) analysis of three cross-sections taken from regions of stylistic differences associated with the two painting stages, including one sample each from the right and left sleeve of David, and one from the interior of Saul's cloak. SEM-EDX also identified a trace component, barium sulfate, associated with the red ochre of the second stage revisions. Combining mapping information from two spectroscopic imaging methods with localized information from microscopic samples has clearly shown that the stylistic differences observed in the paint handling are affiliated with differences in the chemical composition of the paints.
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 3
DOI: 10.1186/S40494-018-0212-3
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“The hidden youth of Dirck Jacobsz leeuw : a portrait by Govert Flinck revealed”. Van Hommes ME, Lambour R, Du Mortier BM, De Winkel M, Tauber G, Alfeld M, Janssens K, Dik J, The Rijksmuseum bulletin 64, 4 (2016)
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“The rediscovered portrait of Prospero Farinacci by Caravaggio”. Cardinali M, De Ruggieri MB, Leone G, Prohaska W, Alfeld M, Janssens K, Artibus et historiae : an art anthology , 249 (2016)
Abstract: Caravaggio's early production as a portrait painter is still the subject of research and a fount of enigmas. Despite the numerous citations in documents, only rarely have these been linked unequivocally to paintings known to date. This is also the case with the `portrait of Farinaccio criminalist painted on a head-size canvas believed to be by Michelangelo from Caravaggio', that was listed in the 1638 inventory of the Marquis Giustiniani and with `the speaker wearing a robe, painted by Caravaggio' on a head-size canvas, owned in 1652 by Caterina Campani, Onorio Longhi's wife. The present multidisciplinary research examines the rediscovery of the portrait of Prospero Farinacci by Caravaggio. The painting, undisclosed until now, hides an underlying female portrait. The authors investigate both compositions from a technical, iconographical and critical point of view, supporting Caravaggio's attribution. The technical researches allow cross-validation in the brushwork and materials of the picture, compared to Caravaggio's early painting technique and style. The portrait of Maffeo Barberini, recently re-ascribed to Caravaggio, shows a significant similarity, while the underlying woman of the retrieved painting closely resembles the gipsy of the Louvre Fortune Teller. In addition, a newly introduced and advanced imaging technique (MaXRF) has detected on the male portrait the feature of the lawyer's robe, which supports the identification with Prospero Farinacci. The intriguing topic of physiognomic accuracy versus stylizing tendency in Caravaggio's portraiture is considered with the aid of Giulio Mancini's observations. Besides, the possible interpretation of the underlying figure as a religious subject sheds a light on the obscure activity of the young Caravaggio in Lorenzo Carli's workshop, recently brought to scholars' attention by new documents and hypotheses.
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“Van Gogh's Irises and Roses : the contribution of chemical analyses and imaging to the assessment of color changes in the red lake pigments”. Centeno SA, Hale C, Caro F, Cesaratto A, Shibayama N, Delaney J, Dooley K, van der Snickt G, Janssens K, Stein SA, Heritage science 5, 18 (2017). http://doi.org/10.1186/S40494-017-0131-8
Abstract: Vincent van Gogh's still lifes Irises and Roses were investigated to shed light onto the degree to which the paintings had changed, both individually and in relation to each other since they were painted, particularly in regard to the fading of the red lakes. Non-invasive techniques, including macroscopic X-ray fluorescence mapping, reflectance imaging spectroscopy, and X-radiography, were combined with microanalytical techniques in a select number of samples. The in-depth microchemical analysis was necessary to overcome the complications that arise when evaluating by non-invasive methods alone the compositions of passages with complex layering and mixing of paints. The results obtained by these two approaches were complemented by color measurements performed on paint cross-sections and on protected edges, and with historical information provided by the artist's own descriptions, early reviews and reproductions, and the data was used to carry out digital color simulations that provided, to a certain extent, a visualization of how the paintings may have originally appeared.
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 21
DOI: 10.1186/S40494-017-0131-8
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“Beauty is skin deep : the skin tones of Vermeer's Girl with a Pearl Earring”. van Loon A, Vandivere A, Delaney JK, Dooley KA, De Meyer S, Vanmeert F, Gonzalez V, Janssens K, Leonhardt E, Haswell R, de Groot S, D'Imporzano P, Davies GR, Heritage science 7, 102 (2019). http://doi.org/10.1186/S40494-019-0344-0
Abstract: The soft modelling of the skin tones in Vermeer's Girl with a Pearl Earring (Mauritshuis) has been remarked upon by art historians, and is their main argument to date this painting to c. 1665. This paper describes the materials and techniques Vermeer used to accomplish the smooth flesh tones and facial features of the Girl, which were investigated as part of the 2018 Girl in the Spotlight research project. It combines macroscopic X-ray fluorescence imaging (MA-XRF), reflectance imaging spectroscopy (RIS), and 3D digital microscopy. Vermeer built up the face, beginning with distinct areas of light and dark. He then smoothly blended the final layers to create almost seamless transitions. The combination of advanced imaging techniques highlighted that Vermeer built the soft contour around her face by leaving a 'gap' between the background and the skin. It also revealed details that were otherwise not visible with the naked eye, such as the eyelashes. Macroscopic imaging was complemented by the study of paint cross-sections using: light microscopy, SEM-EDX, FIB-STEM, synchrotron radiation mu-XRPD and FTIR-ATR. Vermeer intentionally used different qualities or grades of lead white in the flesh paints, showing different hydrocerussite/cerussite ratios and particle sizes. Lead isotope analysis showed that the geographic source of lead, from which the different types of lead white were manufactured, was the same: the region of Peak District of Derbyshire, UK. Finally, cross-section analysis identified the formation of new lead species in the paints: lead soaps and palmierite (K2Pb(SO4)(2)), associated with the red lake.
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1186/S40494-019-0344-0
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“Formation of zinc oxalate from zinc white in various oil binding media: the influence of atmospheric carbon dioxide by reaction with 13CO2”. Simonsen KP, Poulsen JN, Vanmeert F, Ryhl-Svendsen M, Bendix J, Sanyova J, Janssens K, Mederos-Henry F, Heritage science 8, 126 (2020). http://doi.org/10.1186/S40494-020-00467-Z
Abstract: The formation of metal oxalates in paintings has recently gained a great deal of interest within the field of heritage science as several types of oxalate compounds have been identified in oil paintings. The present work investigates the formation of metal oxalates in linseed oil in the presence of the artists' pigments zinc white, calcite, lead white, zinc yellow, chrome yellow, cadmium yellow, cobalt violet, and verdigris. The oil paint films were artificially photo-aged by exposure to UVA light at low and high relative humidity, and afterwards analysed by attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR). The results showed that, compared to the other pigments investigated, zinc white is especially prone to metal oxalate formation and that high humidity is a crucial factor in this process. Consequently, the reactivity and photo-aging of ZnO in various oil binding media was investigated further under simulated solar radiation and at high relative humidity levels. ATR-FTIR showed that zinc oxalate is formed in all oil binding media while X-ray powder diffraction (PXRD) revealed it was mainly present in an amorphous state. To examine whether atmospheric CO2(g) has any influence on the formation of zinc oxalate, experiments with isotopically enriched (CO2(g))-C-13 were performed. Based on ATR-FTIR measurements, neither (ZnC2O4)-C-13 nor (ZnCO3)-C-13 were formed which suggests that the carbon source for the oxalate formation is most likely the paint itself (and its oil component) and not the surrounding atmosphere.
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 2.5
DOI: 10.1186/S40494-020-00467-Z
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“Jackson Pollock's Number 1A, 1948 : a non-invasive study using macro-x-ray fluorescence mapping (MA-XRF) and multivariate curve resolution-alternating least squares (MCR-ALS) analysis”. Martins A, Coddington J, van der Snickt G, van Driel B, McGlinchey C, Dahlberg D, Janssens K, Dik J, Heritage science 4, 33 (2016). http://doi.org/10.1186/S40494-016-0105-2
Abstract: Jackson Pollock's Number 1A, 1948 painting was investigated using in situ scanning macro-x-ray fluorescence mapping (MA-XRF) to help characterize the artist's materials and his creative process. A multivariate curve resolution-alternating least squares (MCR-ALS) approach was used to examine the hyperspectral data and obtain distribution maps and signature spectra for the paints he used. The composition of the paints was elucidated based on the chemical elements identified in the signature spectra and a tentative list of pigments, fillers and other additives is proposed for eleven different paints and for the canvas. The paint distribution maps were used to virtually reconstruct the artist process and document the sequence and manner in which Pollock applied the different paints, using deliberate and specific gestures.
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1186/S40494-016-0105-2
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