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“Reproduction of 16-17th centuries enamels for stained glass after orignal compositions and recipes”. Caen J, Schalm O, Pires De Matos A, Ruivo A, Ferreira M, Janssens K, (2008)
Keywords: P3 Proceeding; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“Caractérisation historique et chimique des peintures en grisaille et du verre de vitrail dans l'oeuvre de J.-B. Capronnier (1814 –, 1891) et J.-B. Bethune (1821 –, 1894)”. Caen J, Schalm O, Janssens K, (2000)
Keywords: P3 Proceeding; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“Casting light on the darkening of colors in historical paintings”. da Pieve F, Hogan C, Lamoen D, Verbeeck J, Vanmeert F, Radepont M, Cotte M, Janssens K, Gonze X, Van Tendeloo G, Physical review letters 111, 208302 (2013). http://doi.org/10.1103/PhysRevLett.111.208302
Abstract: The degradation of colors in historical paintings affects our cultural heritage in both museums and archeological sites. Despite intensive experimental studies, the origin of darkening of one of the most ancient pigments known to humankind, vermilion (α-HgS), remains unexplained. Here, by combining many-body theoretical spectroscopy and high-resolution microscopic x-ray diffraction, we clarify the composition of the damaged paint work and demonstrate possible physicochemical processes, induced by illumination and exposure to humidity and air, that cause photoactivation of the original pigment and the degradation of the secondary minerals. The results suggest a new path for the darkening process which was never considered by previous studies and prompt a critical examination of their findings.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT); AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 8.462
Times cited: 30
DOI: 10.1103/PhysRevLett.111.208302
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“High resolution micro-XRF maps of iron oxides inside sensory dendrites of putative avian magnetoreceptors”. Falkenberg G, Fleissner GE, Fleissner GUE, Schuchardt K, Kühbacher M, Chalmin E, Janssens K, Journal of physics : conference series 186, 012084 (2009). http://doi.org/10.1088/1742-6596/186/1/012084
Abstract: Iron mineral containing sensory dendrites in the inner lining of the upper beak of homing pigeons [1] and various bird species [2] are the first candidate structures for an avian magnetic field receptor. A new concept of magnetoreception [3, 4] is based on detailed ultra-structural optical and electron microscopy analyses in combination with synchrotron radiation microscopic X-ray fluorescence analysis (micro-XRF) and microscopic X-ray absorption near edge structures (micro-XANES). Several behavioral experiments [5, 6] and first mathematical simulations [6] affirm our avian magnetoreceptor model. The iron minerals inside the dendrites are housed in three different subcellular compartments (bullets, platelets, vesicles), which could be clearly resolved and identified by electron microscopy on ultrathin sections [1, 3]. Micro-XRF and micro-XANES data obtained at HASYLAB beamline L added information about the elemental distribution and Fe speciation [3], but are averaged over the complete dendrite due to limited spatial resolution. Here we present recently performed micro-XRF maps with sub-micrometer resolution (ESRF ID21), which reveal for the first time subcellular structural information from almost bulk-like dendrite sample material. Due to the thickness of 30 μm the microarchitecture of the dendrites can be considered as undisturbed and artefacts introduced by sectioning might be widely reduced.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 2
DOI: 10.1088/1742-6596/186/1/012084
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“The identification of chromophores in ancient glass by the use of UV-VIS-NIR spectroscopy”. Meulebroeck W, Baert K, Wouters H, Cosyns P, Ceglia A, Cagno S, Janssens K, Nys K, Terryn H, Thienpont H, Proceedings of the Society of Photo-optical Instrumentation Engineers 7726, 77260d (2010). http://doi.org/10.1117/12.853666
Abstract: In this publication optical spectroscopy is considered to be a supplementary technique to study ancient colored glass. It results from a systematic study of the UV-VIS-NIR transmission spectra of intentionally colored glass fragments from various archaeological and historical sites and dated from the Roman period to the 21th century AD. The main goal consists of defining optical sensing parameters for this type of material. The considered colorants are iron, cobalt, manganese, copper and chromium. It is proved that many cases exist where optical spectroscopy can be seen as a straightforward, non-destructive, low-cost and in-situ applicable technique in identifying authentic material or to obtain information about the origin of the material. Possible sensing parameters are defined as the absence/presence of absorption bands characteristic for a specific coloring metal oxide and the spectral position of these bands. These parameters could reveal information about the applied furnace conditions and/or to the composition of the glass matrix. It is shown that the cobalt absorption band situated around 535 nm for soda rich glasses (Roman and industrial times) is shifted towards 526 nm for potash rich glasses (medieval and post-medieval times).
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 10
DOI: 10.1117/12.853666
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“The use of synchrotron radiation for the characterization of artists' pigments and paintings”. Janssens K, Alfeld M, van der Snickt G, de Nolf W, Vanmeert F, Radepont M, Monico L, et al, Annual review of analytical chemistry 6, 399 (2013). http://doi.org/10.1146/ANNUREV-ANCHEM-062012-092702
Abstract: We review methods and recent studies in which macroscopic to (sub)microscopic X-ray beams were used for nondestructive analysis and characterization of pigments, paint microsamples, and/or entire paintings. We discuss the use of portable laboratory- and synchrotron-based instrumentation and describe several variants of X-ray fluorescence (XRF) analysis used for elemental analysis and imaging and combined with X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS). Macroscopic and microscopic (μ-)XRF variants of this method are suitable for visualizing the elemental distribution of key elements in paint multilayers. Technical innovations such as multielement, large-area XRF detectors have enabled such developments. The use of methods limited to elemental analysis or imaging usually is not sufficient to elucidate the chemical transformations that take place during natural pigment alteration processes. However, synchrotron-based combinations of μ-XRF, μ-XAS, and μ-XRD are suitable for such studies.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 7.435
Times cited: 46
DOI: 10.1146/ANNUREV-ANCHEM-062012-092702
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“Formation of metallic mercury during photodegradation/photodarkening of \alpha-HgS : electrochemical evidence”. Anaf W, Janssens K, De Wael K, Angewandte Chemie: international edition in English 52, 12568 (2013). http://doi.org/10.1002/ANIE.201303977
Abstract: Das rote Pigment α-HgS neigt in Gegenwart von Licht und Chloridionen zur Schwärzung. Als Grund für die Zersetzung und Entfärbung werden die Bildung von (schwarzem) β-HgS oder Quecksilbermetall vermutet, doch diese Substanzen wurden noch nicht auf natürlich oder künstlich zersetzter HgS-Farbe nachgewiesen. Elektrochemische Experimente belegen nun die Bildung von Quecksilbermetall in Gegenwart von Licht und Chloridionen.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 11.994
Times cited: 19
DOI: 10.1002/ANIE.201303977
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“Nanoscale investigation of the degradation mechanism of a historical chrome yellow paint by quantitative electron energy loss spectroscopy mapping of chromium species”. Tan H, Tian H, Verbeeck J, Janssens K, Van Tendeloo G, Angewandte Chemie: international edition in English 52, 11360 (2013). http://doi.org/10.1002/anie.201305753
Abstract: Getting the picture: The investigation of 100 year old chrome yellow paint by transmission electron microscopy and spectroscopy has led to the identification of four types of coreshell particles. This nanoscale investigation has allowed a mechanism to be proposed for the darkening of some bright yellow colors in Van Gogh's paintings (e.g. in Falling leaves (Les Alyscamps), 1888).
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT); AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 11.994
Times cited: 29
DOI: 10.1002/anie.201305753
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Janssens K, Degryse P, Cosyns P, Caen J, Van 't dack L (2009) Annales of the 17th Congress of the International Association for the History of Glass (Antwerp, Belgium, 2006). 704 p
Keywords: ME2 Book as editor or co-editor; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“Composition and state of alteration of 18th century glass from the Cistercian nunnery of Clairefontaine (Belgium)”. Herremans D, Cagno S, Vincke A, de Clercq W, Janssens K, Proceedings of the Society of Photo-optical Instrumentation Engineers
T2 –, Conference on Integrated Approaches to the Study of Historical Glass, (IASHG), APR 16-17, 2012, Brussels, BELGIUM , 842206 (2012). http://doi.org/10.1117/12.975247
Abstract: An extended set of 18th century glass vessels was analyzed by means of SEM-EDX (major and minor element composition) The fragmented archaeological objects were recovered from a latrine belonging to the early 18th century building phase of the nunnery of Clairefontaine, near Arlon (B). On the basis of typology and decoration, the major part of the vessels could be dated around the middle of the 18th century. Variety in color and weathering of the glass suggest differences in glassmaking recipes and in the composition and origin of raw materials. The results of the analysis show how two main compositional groups constitute about 90% of the analyzed glass set, and these are constituted by potash glass (transparent beakers) and high lime low alkali glass (green bottles). Next to these, a few potash-lime and soda glasses are also found. The type of alteration has also a clear relation with the original glass composition.
Keywords: P1 Proceeding; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1117/12.975247
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“Degradation process of lead chromate in paintings by Vincent van Gogh studied by means of spectromicroscopic methods : 4 : artificial aging of model samples of co-precipitates of lead chromate and lead sulfate”. Monico L, Janssens K, Miliani C, van der Snickt G, Brunetti BG, Guidi MC, Radepont M, Cotte M, Analytical chemistry 85, 860 (2013). http://doi.org/10.1021/AC3021592
Abstract: Previous investigations about the darkening of chrome yellow pigments revealed that this form of alteration is attributable to a reduction of the original Cr(VI) to Cr(III), and that the presence of sulfur-containing compounds, most often sulfates, plays a key role during this process. We recently demonstrated that different crystal forms of chrome yellow pigments (PbCrO4 and PbCr1xSxO4) are present in paintings by Vincent van Gogh. In the present work, we show how both the chemical composition and the crystalline structure of lead chromate-based pigments influence their stability. For this purpose, oil model samples made with in-house synthesized powders of PbCrO4 and PbCr1xSxO4 were artificially aged and characterized. We observed a profound darkening only for those paint models made with PbCr1xSxO4, rich in SO42 (x ≥ 0.4), and orthorhombic phases (>30 wt %). Cr and S K-edge micro X-ray absorption near edge structure investigations revealed in an unequivocal manner the formation of up to about 60% of Cr(III)-species in the outer layer of the most altered samples; conversely, independent of the paint models chemical composition, no change in the S-oxidation state was observed. Analyses employing UVvisible diffuse reflectance and Fourier transform infrared spectroscopy were performed on unaged and aged model samples in order to obtain additional information on the physicochemical changes induced by the aging treatment.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 6.32
Times cited: 49
DOI: 10.1021/AC3021592
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“Composition of Facon de Venise glass from early 17th century London in comparison with luxury glass of the same age”. Cagno S, de Raedt I, Jeffries T, Janssens K, Proceedings of the Society of Photo-optical Instrumentation Engineers
T2 –, Conference on Integrated Approaches to the Study of Historical Glass, (IASHG), APR 16-17, 2012, Brussels, BELGIUM , 842205 (2012). http://doi.org/10.1117/12.975212
Abstract: SEM-EDX and LA-ICP-MS analyses were performed on a set of early 17th century London glass fragments. The samples originate from two archaeological sites (Aldgate and Old Broad Street) where glass workshops were active in this period. The great majority of the samples are made of soda glass. Two distinct compositional groups are observed, each typical of one site of provenance. The samples originating from the Old Broad Street excavation feature a silica-soda-lime composition, with a moderate amount of potash. The samples from Aldgate are richer in potassium and feature higher amounts of trace elements such as Rb, Zr and Cu. The distinction between the two groups stems from different flux and silica sources used for glassmaking. A comparison with different European glass compositions of that time reveals no resemblance with genuine Venetian production, yet the composition of the Old Broad Street glass shows a close similarity to that of fragments produced 'a la facon de Venise' in Antwerp at the end of the 16th century. This coincides with historical sources attesting the arrival of glassworkers from the Low Countries in England and suggests that a transfer of technology took place near the turn of the century.
Keywords: P1 Proceeding; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 1
DOI: 10.1117/12.975212
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“A chemical investigation of altered jade art objects”. Aerts A, Janssens K, Adams F, Orientations , 79 (1995)
Keywords: A3 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“Study of the early stages of Mn intrusion in corroded glass by means of combined SR FTIR/\muXRF imaging and XANES spectroscopy”. Nuyts G, Cagno S, Hellemans K, Veronesi G, Cotte M, Janssens K, Procedia Chemistry
T2 –, Youth in Conservation of Cultural Heritage Conference (YOCOCU), June 18-20, 2012, University of Antwerp, Antwerp, Belgium , 239 (2013). http://doi.org/10.1016/J.PROCHE.2013.03.030
Abstract: Historical glass, especially medieval glass, can undergo weathering under the influence of time and environmental conditions. The aim of this investigation was to better understand the processes involved in this natural degradation process by studying artificially altered glass samples prepared for the use of evaluation of conservation methods. Non-durable glass sensors produced by the Fraunhofer Institute (type M1.0) were used as a starting material for artificial alteration. These were immersed in acidic (pH = 0, 2, 4) and neutral solutions (1 h – 8 h). In a second stage the glass samples were immersed in a 0.5 M MnCl2 solution (24 h, 48 h and 72 h), allowing intrusion of Mn from the solution into the gel layer. The samples were characterized at different stages with reflectance FTIR spectroscopy, mu XRF mapping and mu XANES. All measurements were carried out at ESRF, beamline ID21. Reflectance FTIR spectroscopy measurements were performed in the 800 4000 cm(-1) range. Cluster analysis of the resulting maps evidenced the rapid growth of the gel layer in strong acidic conditions. The average spectra for each cluster feature show for the original glass a strong Si-O- stretching band between 900 and 1000 cm(-1), whereas the gel layer could be identified by the increasing Si-O-Si bands around 1100 and 1250 cm(-1). mu XRF maps were recorded at different stages of the experiment at energies around the Mn-K edge (6.539 keV) and with a step size of 2 by 2 m. These confirm the leaching of K+ and Ca+2 from the glass and the intrusion of Mn from the solution. Mn was found throughout the entire gel layer, but with a concentration gradient peaking at the surface. XANES point measurements were recorded at various points where Mn was present. No spatial variation was found, but linear combination fitting of the spectra with various Mn reference compounds indicated that Mn2+Mn23+O4 is the main Mn compound in the gel layer, as was hypothesised by Watkinson et al. The standard corroded glass samples studied here can be used for the evaluation of conservation treatments in follow-up experiments. (C) 2013 The Authors. Published by Elsevier B.V. Selection and peer-review under responsibility of the IA-CS (Italian Association of Conservation Scientists) and University of Antwerp
Keywords: P1 Proceeding; Engineering sciences. Technology; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 4
DOI: 10.1016/J.PROCHE.2013.03.030
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“Chemical analysis of the powder deposit on Chinese jade objects”. Aerts A, Janssens K, Adams F page 12 (1995).
Keywords: H3 Book chapter; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“Semi-quantitative analysis of the formation of a calcium oxalate protective layer for monumental limestone using combined micro-XRF and micro-XRPD”. Vanmeert F, Mudronja D, Fazinic S, Janssens K, Tibljas D, X-ray spectrometry 42, 256 (2013). http://doi.org/10.1002/XRS.2486
Abstract: A current method for the protection of cretaceous limestone present in various monuments consists of performing a passivating treatment with ammonium oxalate (AmOx). A calcium oxalate protective layer is formed on the surface and enhances the acid resistance of the stone. The in-depth formation of the calcium oxalate layer was investigated on cross sections by using combined micro X-ray fluorescence and micro X-ray powder diffraction (mu XRF/mu XRPD). XRPD showed the presence of both whewellite and weddellite in the calcite stone matrix. A correction was made for sample misalignment, which was visible in both the fluorescence and the diffraction line measurements. A semi-quantitative analysis was performed on the basis of Klug's equation for a two-phase mixture (the presence of weddellite was neglected) without the need for a known reference sample. By assuming two extreme compositions for a reference weight fraction (1 and 99wt%), it was possible to obtain whewellite concentration profiles, which can be used for comparing the effectiveness of different methods for the application of AmOx to the stone surface and the effect of treatment time and AmOx concentration used. It is shown that for the relative amounts of whewellite formed, the differences due to the assumed weight fractions are smaller than the errors due to sample heterogeneity and preferred orientation. Copyright (c) 2013 John Wiley & Sons, Ltd.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 1.298
Times cited: 5
DOI: 10.1002/XRS.2486
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“Micro-analytical characterisation of radioactive heterogeneities in samples from Central Asian TENORM sites”. Lind OC, de Nolf W, Janssens K, Salbu B, Journal of environmental radioactivity 123, 63 (2013). http://doi.org/10.1016/J.JENVRAD.2012.02.012
Abstract: The present work focuses on the use of micro-analytical techniques to demonstrate the heterogeneous distribution of radionuclides and metals in soils collected at Former Soviet Union mining sites in Central Asia. Based on digital autoradiography, radionuclides were heterogeneously distributed in soil samples collected at the abandoned uranium mining sites Kurday, Kazakhstan, Kadji Sai, Kyrgyzstan and Taboshar, Tajikistan. Using electron microscopy interfaced with X-ray microanalysis submicron – mm-sized radioactive particles and rock fragments with U, As, Se and toxic metals on the surfaces were identified in Kurday and Kadji Sai samples. Employing scanning and tomographic (3D) synchrotron radiation based micro-X-ray fluorescence (mu-SRXRF) and synchrotron radiation based micro-X-ray diffraction (mu-SRXRD) allowed us to observe the inner structure of the particles without physical sectioning. The distribution of elements in virtual crosssections demonstrated that U and a series of toxic elements were rather heterogeneously distributed also within individual radioactive TENORM particles. Compared to archived data, U in Kadji Sai particles was present as uraninite (U4O9+y or UO2+x) or Na-zippeite aNa(4)(UO2)(6)[(OH)(10)(SO4)(3)]center dot 4H(2)O), i.e. U minerals with very low solubility. The results suggested that TENORM particles can carry substantial amount of radioactivity, which can be subject to re-suspension, atmospheric transport and water transport. Thus, the potential radioecological and radioanalytical impact of radioactive particles at NORM and TENORM sites worldwide should be taken into account. The present work also demonstrates that radioecological studies should benefit from the use of advanced methods such as synchrotron radiation based techniques. (C) 2012 Elsevier Ltd. All rights reserved.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 2.31
Times cited: 16
DOI: 10.1016/J.JENVRAD.2012.02.012
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“Degradation process of lead chromate in paintings by Vincent van Gogh studied by means of spectromicroscopic methods : 3 : synthesis, characterization, and detection of different crystal forms of the chrome yellow pigment”. Monico L, Janssens K, Miliani C, Brunetti BG, Vagnini M, Vanmeert F, Falkenberg G, Abakumov A, Lu Y, Tian H, Verbeeck J, Radepont M, Cotte M, Hendriks E, Geldof M, van der Loeff L, Salvant J, Menu M;, Analytical chemistry 85, 860 (2013). http://doi.org/10.1021/ac302158b
Abstract: The painter, Vincent van Gogh, and some of his contemporaries frequently made use of the pigment chrome yellow that is known to show a tendency toward darkening. This pigment may correspond to various chemical compounds such as PbCrO4 and PbCr1-xSxO4, that may each be present in various crystallographic forms with different tendencies toward degradation. Investigations by X-ray diffraction (XRD), mid-Fourier Transform infrared (FTIR), and Raman instruments (benchtop and portable) and synchrotron radiation-based micro-XRD and X-ray absorption near edge structure spectroscopy performed on oil-paint models, prepared with in-house synthesized PbCrO4 and PbCr1-xSxO4, permitted us to characterize the spectroscopic features of the various forms. On the basis of these results, an extended study has been carried out on historic paint tubes and on embedded paint microsamples taken from yellow-orange/pale yellow areas of 12 Van Gogh paintings, demonstrating that Van Gogh effectively made use of different chrome yellow types. This conclusion was also confirmed by in situ mid-FTIR investigations on Van Goghs Portrait of Gauguin (Van Gogh Museum, Amsterdam).
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT); AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 6.32
Times cited: 79
DOI: 10.1021/ac302158b
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“A mobile instrument for in situ scanning macro-XRF investigation of historical paintings”. Alfeld M, Pedroso JV, van Hommes ME, van der Snickt G, Tauber G, Blaas J, Haschke M, Erler K, Dik J, Janssens K, Journal of analytical atomic spectrometry 28, 760 (2013). http://doi.org/10.1039/C3JA30341A
Abstract: Scanning macro-X-ray fluorescence analysis (MA-XRF) is rapidly being established as a technique for the investigation of historical paintings. The elemental distribution images acquired by this method allow for the visualization of hidden paint layers and thus provide insight into the artist's creative process and the painting's conservation history. Due to the lack of a dedicated, commercially available instrument the application of the technique was limited to a few groups that constructed their own instruments. We present the first commercially available XRF scanner for paintings, consisting of an X-ray tube mounted with a Silicon-Drift (SD) detector on a motorized stage to be moved in front of a painting. The scanner is capable of imaging the distribution of the main constituents of surface and sub-surface paint layers in an area of 80 by 60 square centimeters with dwell times below 10 ms and a lateral resolution below 100 mu m. The scanner features for a broad range of elements between Ti (Z = 22) and Mo (Z = 42) a count rate of more than 1000 counts per second (cps)?mass percent and detection limits of 100 ppm for measurements of 1 s duration. Next to a presentation of spectrometric figures of merit, the value of the technique is illustrated through a case study of a painting by Rembrandt's student Govert Flinck (1615-1660).
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.379
Times cited: 106
DOI: 10.1039/C3JA30341A
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“Scanning XRF investigation of a Flower Still Life and its underlying composition from the collection of the Kröller-Muller Museum”. Alfeld M, van der Snickt G, Vanmeert F, Janssens K, Dik J, Appel K, van der Loeff L, Chavannes M, Meedendorp T, Hendriks E, Applied physics A : materials science &, processing 111, 165 (2013). http://doi.org/10.1007/S00339-012-7526-X
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 1.455
Times cited: 35
DOI: 10.1007/S00339-012-7526-X
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“Visualizing the 17th century underpainting in Portrait of an Old Man by Rembrandt van Rijn using synchrotron-based scanning macro-XRF”. Alfeld M, Siddons DP, Janssens K, Dik J, Woll A, Kirkham R, van de Wetering E, Applied physics A : materials science &, processing 111, 157 (2013). http://doi.org/10.1007/S00339-012-7490-5
Abstract: In 17th century Old Master Paintings, the underpainting generally refers to the first sketch of a composition. The underpainting is applied to a prepared ground using a monochrome, brown oil paint to roughly indicate light, shade and contours. So far, methods to visualize the underpainting-other than in localized cross-sections-have been very limited. Neither infrared reflectography nor neutron induced autoradiography have proven to be practical, adequate visualization tools. Thus, although of fundamental interest in the understanding of a painting's genesis, the underpainting has virtually escaped all imaging efforts. In this contribution we will show that 17th century underpainting may consist of a highly heterogeneous mixture of pigments, including copper pigments. We suggest that this brown pigment mixture is actually the recycled left-over of a palette scraping. With copper as the heaviest exclusive elemental component, we will hence show in a case study on a Portrait of an Old Man attributed to Rembrandt van Rijn how scanning macro-XRF can be used to efficiently visualize the underpainting below the surface painting and how this information can contribute to the discussion of the painting's authenticity.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 1.455
Times cited: 26
DOI: 10.1007/S00339-012-7490-5
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“Efficiency of applying ammonium oxalate for protection of monumental limestone by poultice, immersion and brushing methods”. Mudronja D, Vanmeert F, Hellemans K, Fazinic S, Janssens K, Tibljas D, Rogosic M, Jakovljevic S, Applied physics A : materials science &, processing 111, 109 (2013). http://doi.org/10.1007/S00339-012-7365-9
Abstract: Samples of cretaceous limestone have been treated with three application methods (poultice, immersion and brushing) using different concentrations of ammonium oxalate solution (AmOx) and varying treatment time in order to test the efficiency of surface and in-depth formation of a protective layer of calcium oxalate (CaOx). Synchrotron-based microanalytical techniques (SR-mu XRD with 12.5 mu mx7.5 mu m (HxV) probe size, SR-mu FTIR with 10 mu mx10 mu m and 8 mu mx20 mu m probe sizes) and laboratory mu FTIR, XRD and SEM have been employed for analysis of the treated samples. Synchrotron-based techniques showed variations in the CaOx distribution along the surface on a micrometer scale. All treatments resulted in the development of a CaOx layer with a maximum thickness of approximately 40 mu m. Application by the brushing method with 10 1-min applications with 5-min breaks during one hour showed a development of the calcium oxalate layer equivalent to the poultice treatment taking 10 h. This treatment could be preferred for large marble or limestone surfaces where poultice usage is economically not feasible.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 1.455
Times cited: 13
DOI: 10.1007/S00339-012-7365-9
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“Spatially resolved (semi)quantitative determination of iron (Fe) in plants by means of synchrotron micro X-ray fluorescence”. Terzano R, Alfeld M, Janssens K, Vekemans B, Schoonjans T, Vincze L, Tomasi N, Pinton R, Cesco S, Analytical and bioanalytical chemistry 405, 3341 (2013). http://doi.org/10.1007/S00216-013-6768-6
Abstract: Iron (Fe) is an essential element for plant growth and development; hence determining Fe distribution and concentration inside plant organs at the microscopic level is of great relevance to better understand its metabolism and bioavailability through the food chain. Among the available microanalytical techniques, synchrotron mu-XRF methods can provide a powerful and versatile array of analytical tools to study Fe distribution within plant samples. In the last years, the implementation of new algorithms and detection technologies has opened the way to more accurate (semi)quantitative analyses of complex matrices like plant materials. In this paper, for the first time the distribution of Fe within tomato roots has been imaged and quantified by means of confocal mu-XRF and exploiting a recently developed fundamental parameter-based algorithm. With this approach, Fe concentrations ranging from few hundreds of ppb to several hundreds of ppm can be determined at the microscopic level without cutting sections. Furthermore, Fe (semi)quantitative distribution maps were obtained for the first time by using two opposing detectors to collect simultaneously the XRF radiation emerging from both sides of an intact cucumber leaf.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.431
Times cited: 27
DOI: 10.1007/S00216-013-6768-6
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“Revealing hidden paint layers in oil paintings by means of scanning macro-XRF : a mock-up study based on Rembrandt's “An old man in military costume””. Alfeld M, de Nolf W, Cagno S, Janssens K, et al, Journal of analytical atomic spectrometry 28, 40 (2013). http://doi.org/10.1039/C2JA30119A
Abstract: Over the past several decades the oeuvre of Rembrandt has been the subject of extensive art historical and scientific investigations. One of the most striking features to emerge is his frequent re-use of canvases and panels. The painting An Old Man in Military Costume (78.PB.246), in the collection of the J. Paul Getty Museum, is an example of such a re-used panel. Conventional imaging techniques revealed the presence of a second portrait under the surface portrait, but the details of this hidden portrait have not yet been revealed. Vermilion (HgS) has been identified to have been used nearly exclusively in the flesh tones of the lower painting, suggesting that element-specific XRF imaging might successfully image the hidden portrait. To test this hypothesis, a full-scale mock-up of the painting was created, including a “free impression” of the hidden portrait, reproducing as closely as possible the pigments and paint stratigraphy of the original painting. XRF imaging of the mock-up painting was conducted using three different XRF imaging systems: a mobile X-ray tube based system and two synchrotron-based setups (one equipped with multiple SDDs and one equipped with a Maia detector). The sensitivity, limits of detection and imaging capabilities of each system under the chosen experimental conditions are evaluated and compared. The results indicate that an investigation of the original painting by this method would have an excellent chance of success.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.379
DOI: 10.1039/C2JA30119A
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“Combined use of synchrotron radiation based micro-X-ray fluorescence, micro-X-ray diffraction, micro-X-ray absorption near-edge, and micro-fourier transform infrared spectroscopies for revealing an alternative degradation pathway of the pigment cadmium yellow in a painting by Van Gogh”. van der Snickt G, Janssens K, Dik J, de Nolf W, Vanmeert F, Jaroszewicz J, Cotte M, Falkenberg G, Van der Loeff L, Analytical chemistry 84, 10221 (2012). http://doi.org/10.1021/AC3015627
Abstract: Over the past years a number of studies have described the instability of the pigment cadmium yellow (CdS). In a previous paper we have shown how cadmium sulfide on paintings by James Ensor oxidizes to CdSO4 center dot H2O. The degradation process gives rise to the fading of the bright yellow color and the formation of disfiguring white crystals that are present on the paint surface in approximately 50 mu m sized globular agglomerations. Here, we study cadmium yellow in the painting “Flowers in a blue vase” by Vincent van Gogh. This painting differs from the Ensor case in the fact that (a) a varnish was superimposed onto the degraded paint surface and (b) the CdS paint area is entirely covered with an opaque crust. The latter obscures the yellow color completely and thus presents a seemingly more advanced state of degradation. Analysis of a cross-sectioned and a crushed sample by combining scanning microscopic X-ray diffraction (mu-XRD), microscopic X-ray absorption near-edge spectroscopy (mu-XANES), microscopic X-ray fluorescence (mu-XRF) based chemical state mapping and scanning microscopic Fourier transform infrared (mu-FT-IR) spectrometry allowed unravelling the complex alteration pathway. Although no crystalline CdSO4 compounds were identified on the Van Gogh paint samples, we conclude that the observed degradation was initially caused by oxidation of the original CdS pigment, similar as for the previous Ensor case. However, due to the presence of an overlying varnish containing lead-based driers and oxalate ions, secondary reactions took place. In particular, it appears that upon the photoinduced oxidation of its sulfidic counterion, the Cd2+ ions reprecipitated at the paint/varnish interface after having formed a complex with oxalate ions that themselves are considered to be degradation products of the resin and/or oil in the varnish. The SO42- anions, for their part, found a suitable reaction partner in Pb2+ ions stemming from a dissolved lead-based siccative that was added to the varnish to promote its drying. The resulting opaque anglesite compound in the varnish, in combination with the underlying CdC2O4 layer at the paint/varnish interface, account for the orange-gray crust that is disfiguring the painting on a macroscopic level. In this way, the results presented in this paper demonstrate how, through a judicious combined use of several microanalytical methods with speciation capabilities, many new insights can be obtained from two minute, but highly complex and heterogeneous paint samples.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 6.32
Times cited: 59
DOI: 10.1021/AC3015627
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“Restoration of X-ray fluorescence images of hidden paintings”. Anitha A, Brasoveanu A, Duarte M, Hughes S, Daubechies I, Dik J, Janssens K, Alfeld M, Signal processing 93, 592 (2013). http://doi.org/10.1016/J.SIGPRO.2012.09.027
Abstract: This paper describes our methods for repairing and restoring images of hidden paintings (paintings that have been painted over and are now covered by a new surface painting) that have been obtained via noninvasive X-ray fluorescence imaging of their canvases. This recently developed imaging technique measures the concentrations of various chemical elements at each two-dimensional spatial location across the canvas. These concentrations in turn result from pigments present both in the surface painting and in the hidden painting beneath. These X-ray fluorescence images provide the best available data from which to noninvasively study a hidden painting. However, they are typically marred by artifacts of the imaging process, features of the surface painting, and areas of information loss. Repairing and restoring these images thus consists of three stages: (1) repairing acquisition artifacts in the dataset, (2) removal of features in the images that result from the surface painting rather than the hidden painting, and (3) identification and repair of areas of information loss. We describe methods we have developed to address each of these stages: a total-variation minimization approach to artifact correction, a novel method for underdetermined blind source separation with multimodal side information to address surface feature removal, and two application-specific new methods for automatically identifying particularly thick or X-ray absorbent surface features in the painting. Finally, we demonstrate the results of our methods on a hidden painting by the artist Vincent van Gogh. (C) 2012 Elsevier B.V. All rights reserved.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.11
Times cited: 13
DOI: 10.1016/J.SIGPRO.2012.09.027
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“X-ray optics for synchrotron-radiation-induced X-ray micro fluorescence at the european synchrotron-radiation facility, Grenoble”. Vincze L, Janssens K, Adams F, Institute of physics conference series , 613 (1993)
Abstract: Different optical designs for generating synchrotron x-ray micro beams suitable for use in an X-ray fluorescence microscope using an ESRF bending magnet X-ray source are compared. Attention is devoted to the spatial and energy distribution of the photons in the micro beam and to the minimum detection limits that are achievable with each alternative optical system.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“Quantitative mu-XRF analysis of heterogeneous samples”. Vincze L, Janssens K, Adams F, Jones K, Microbeam Analysis 1995: Proceedings Of The 29th Annual Conference Of The Microbeam Analysis Society , 175 (1995)
Keywords: P1 Proceeding; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“Parameters influencing focussing capabilities of capillary optics”. Vincze L, Janssens K, Adams F, Larsson S, Rindby A, Engstrom P, Microbeam Analysis 1995: Proceedings Of The 29th Annual Conference Of The Microbeam Analysis Society , 161 (1995)
Keywords: P1 Proceeding; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“A laboratory mu-XRF spectrometer employing capillary optics”. Janssens K, Vekemans B, Rindby A, Vincze L, Adams F, , 159 (1995)
Keywords: P1 Proceeding; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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