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Author Vanmeert, F.; de Nolf, W.; De Meyer, S.; Dik, J.; Janssens, K. url  doi
openurl 
  Title Macroscopic X-ray powder diffraction scanning, a new method for highly selective chemical imaging of works of art : instrument optimization Type A1 Journal article
  Year 2018 Publication Analytical chemistry Abbreviated Journal Anal Chem  
  Volume 90 Issue 11 Pages 6436-6444  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract In the past decade macroscopic X-ray fluorescence imaging (MA-XRF) has become established as a method for the noninvasive investigation of flat painted surfaces, yielding large scale elemental maps. MA-XRF is limited by a lack of specificity, only allowing for indirect pigment identification based on the simultaneous presence of chemical elements. The high specificity of X-ray powder diffraction (XRPD) mapping is already being exploited at synchrotron facilities for investigations at the (sub)microscopic scale, but the technique has not yet been employed using lab sources. In this paper we present the development of a novel MA-XRPD/XRF instrument based on a laboratory X-ray source. Several combinations of X-ray sources and area detectors are evaluated in terms of their spatial and angular resolution and their sensitivity. The highly specific imaging capability of the combined MA-XRPD/XRF instrument is demonstrated on a 15th/16th century illuminated manuscript directly revealing the distribution of a large number of inorganic pigments, including the uncommon yellow pigment massicot (o-PbO). The case study illustrates the wealth of new mapping information that can be obtained in a noninvasive manner using the laboratory MA-XRPD/XRF instrument.  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000434893200019 Publication Date 2018-04-06  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0003-2700; 5206-882x ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 6.32 Times cited (up) 11 Open Access  
  Notes ; The authors thank the persons involved at Incoatec GmbH, imXPAD SAS and Dectris Ltd. for loaning us some of their products over the past years. We acknowledge financial support from BELSPO (Brussels) S2-ART, the NWO (The Hague) Science4Arts “ReVisRembrandt” Project and GOA Project Solarpaint (University of Antwerp Research Council). Photo Copyright Geert Van der Snickt, 2008 for the photograph of the illuminated manuscript in the TOC graphic. ; Approved Most recent IF: 6.32  
  Call Number UA @ admin @ c:irua:151993 Serial 5701  
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Author Benito, P.; de Nolf, W.; Nuyts, G.; Janssens, K.; et al. pdf  url
doi  openurl
  Title Role of coating-metallic support interaction in the properties of electrosynthesized Rh-based structured catalysts Type A1 Journal article
  Year 2014 Publication ACS catalysis Abbreviated Journal Acs Catal  
  Volume 4 Issue 10 Pages 3779-3790  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract Rh-structured catalysts for the catalytic partial oxidation of CH4 to syngas were prepared by electrosynthesis of Rh-containing hydrotalcite-type (HT) compounds on FeCrAlloy foams followed by calcination at 900 degrees C. During the calcination the simultaneous decomposition of the layered HT structure and formation of the protective FeCrAlloy outer shell in alumina occurred. Here, we studied the role of the coating-metallic support interaction in the properties of the catalysts after calcination, H-2 reduction, and catalytic tests, by a combination of electron (FEG-SEM/EDS) and synchrotron X-ray (XRF/XRPD and XRF/XANES) microscopic techniques. The characterization of crystalline phases in the metallic support and coating and distribution of Rh active species was carried out on several samples prepared by modifying the Rh content in the electrolytic solution (Rh/Mg/Al = 11.0/70.0/19.0, 5.0/70.0/25.0, 0/70.0/30.0 atomic ratio). A sample was also prepared with no aluminum in the electrolytic solution (Rh/Mg/Al = 13.6/86.4/0.0 atomic ratio) and calcined at 550 and 900 degrees C. The interaction between the elements of the metallic support and the catalytic coating increased the film adhesion during the thermal treatment and catalytic tests and modified the catalyst crystalline phases. A chemical reaction between Al corning from the foam and Mg in the coating occurred during calcination at high temperature leading to the formation of spinel phases in which rhodium is solved, together with some Rh2O3 and Rh. The metallic support was oxidized forming the corundum scale and chromium oxides, moreover t-Al2O3 was identified. For the Rh11.0Mg70.0Al19.0 catalyst the inclusion of Rh in the spinel phase decreased its reducibility in the H-2 pretreatment. The reduction continued during catalytic tests by feeding diluted CH4/O-2/He gas mixtures, evidenced by the catalyst activation. While under concentrated gas mixtures the deactivation occurred, probably by oxidation.  
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  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000345735200053 Publication Date 2014-09-24  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 2155-5435 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 10.614 Times cited (up) 13 Open Access  
  Notes ; The authors thank the scientists who assisted during the conducted experiments: D. Grolimund and C. N. Borca for the mu XRF/XRPD experiments performed at MicroXAS Beamline of SLS, M. Janousch for the mu XRF/XANES experiments at Phoenix Beamline of the SLS, M. Salome for the mu XRE/XANES experiments at ID21 Beamline of the ESRF, and I. Guerra for the FEG-SEM/EDS experiments at Granada University. Thanks must go to Porvair for supplying FeCrAlloy foams. The financial support from the Ministero per l'Istruzione, l'Universita e la Ricerca (MIUR, Roma, I) is gratefully acknowledged. ; Approved Most recent IF: 10.614; 2014 IF: 9.312  
  Call Number UA @ admin @ c:irua:122215 Serial 5820  
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Author Benito, P.; Monti, M.; de Nolf, W.; Nuyts, G.; Janssens, K.; et al. pdf  doi
openurl 
  Title Improvement in the coating homogeneity in electrosynthesized Rh structured catalysts for the partial oxidation of methane Type A1 Journal article
  Year 2015 Publication Catalysis today Abbreviated Journal Catal Today  
  Volume 246 Issue Pages 154-164  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract The precipitation of Rh/Mg/Al and Rh/Al hydroxides on the surface of FeCrAlloy foams by a base electrogeneration method was investigated to improve the properties of the deposited film (homogeneity and composition) and therefore the performances of the structured catalysts, obtained by calcination, in the Catalytic Partial Oxidation of CH4 to syngas. The work focussed on decreasing current gradients within open-cell foam cylinders by increasing the number of electrical contacts from 1 to 3 points to promote a more homogeneous precipitation of the hydroxides. Electrochemical and catalytic tests as well as SEM/EDS and mu-XRFIXRD analyses allowed to correlate the effect of the number of electrical contact points with materials properties. Lastly, syntheses were performed on Pt plates to study the effect of the electrical behaviour and shape of the support on the composition of the film. A more homogeneous coating of the foam surface was achieved by adopting a configuration with 3 contact points since the reduction of nitrates and water molecules that generates the basic media in the vicinity of the support was enhanced. Layer thicknesses up to 5-15 mu m were deposited; however, the sequential precipitation of a film with composition closer to the expected one and a layer enriched in Al and Rh (outer layer) was not avoided. The improvement in the coating gave rise to enhanced performances for a sample prepared at -1.1 V for 3000 s. Contrarily, the low adherence of the outer layer in a sample prepared at -1.2 V for 2000 s during both calcination and catalytic tests may be responsible of the unexpected decrease in catalytic performances. The same sequential precipitation was observed by performing the syntheses on Pt plates, showing that the electrical nature the support did not play a key role on this phenomenon. (C) 2014 Elsevier B.V. All rights reserved.  
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  Corporate Author Thesis  
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  Language Wos 000349998300020 Publication Date 2014-10-31  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0920-5861 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 4.636 Times cited (up) 14 Open Access  
  Notes ; The financial support from the Ministero per l'Istruzione, l'Universita e la Ricerca (MIUR, Roma, I) is gratefully acknowledged. The authors thank D. Grolimund and C.N. Borca for assisting the mu XRF/XRD conducted experiments at MicroXAS Beamline of SLS Thanks are due to Porvair for supplying FeCrAlloy foams. ; Approved Most recent IF: 4.636; 2015 IF: 3.893  
  Call Number UA @ admin @ c:irua:124616 Serial 5656  
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Author Benito, P.; Nuyts, G.; Monti, M.; de Nolf, W.; Fornasari, G.; Janssens, K.; Scavetta, E.; Vaccari, A. pdf  doi
openurl 
  Title Stable Rh particles in hydrotalcite-derived catalysts coated on FeCrAlloy foams by electrosynthesis Type A1 Journal article
  Year 2015 Publication Applied catalysis : B : environmental Abbreviated Journal Appl Catal B-Environ  
  Volume 179 Issue Pages 321-332  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract Rh-based structured catalysts for the Catalytic Partial Oxidation of CH4 to syngas were prepared by electrosynthesis of Rh/Mg/Al hydrotalcite-type compounds on FeCrAlloy foams and calcination. The effects of Rh content, total metal concentration, and partial replacement of Mg2+ by Ni2+ in the electrolytic solution on coating thickness, Rh speciation, metallic particle size, and catalytic activity were investigated by SEM/EDS, mu-XRF/XANES and tests under diluted and concentrated reaction conditions. The amount of Rh species, present as Mg (RhxAl1-x)(2)O-4, depended on the thickness of the electrosynthesised layer as well as the Rh particle size and dispersion. Smaller and more dispersed particles were obtained by decreasing the Rh concentration in the electrolytic solution from Rh/Mg/Al=11/70/19 to 5/70/25 and 2/70/28 atomic ratio% (a.r.%) and in thinner rather than thicker layers. Despite the improvement in metallic particles features, the CH4 conversion was negatively affected by the low amount of active sites in the coating, the high metal support interaction and possibly the oxidation of metallic particles and carbon formation. A larger amount of solid containing well dispersed Rh particles was deposited by increasing the total metal concentration from 0.03 M to 0.06 M with the Rh/Mg/Al=5/70/25 a.r.%, and the catalytic performances were enhanced. The partial replacement of Mg2+ by Ni2+ gave rise to a very active bimetallic Rh/Ni catalyst, CH4 conversion and selectivity to syngas were above 90%, however, it slightly deactivated with time-on-stream. (C) 2015 Elsevier B.V. All rights reserved.  
  Address  
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  Publisher Place of Publication Editor  
  Language Wos 000359873800036 Publication Date 2015-05-19  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0926-3373 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 9.446 Times cited (up) 14 Open Access  
  Notes ; The Authors acknowledge M. Salome for helping during the mu XRF/XANES experiments at ID21 Beamline of the ESRF, the Department of Structural Characterisation of CNR-IMM of Bologna for the access to the FEG-SEM facility and Dr F. Ospitali for the scientific support. Thanks are due to Farrel Lytle database for providing the necessary Rh metal spectrum (rhfoil.a99 in http:// ixs.iit.edu/data/FarrelLytledata/). The financial support from the Ministero per l'Istruzione, l'Universita e la Ricerca (MIUR, Roma, Italy) and the University of Bologna (FARB program) is gratefully acknowledged. ; Approved Most recent IF: 9.446; 2015 IF: 7.435  
  Call Number UA @ admin @ c:irua:127777 Serial 5846  
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Author Lind, O.C.; de Nolf, W.; Janssens, K.; Salbu, B. pdf  doi
openurl 
  Title Micro-analytical characterisation of radioactive heterogeneities in samples from Central Asian TENORM sites Type A1 Journal article
  Year 2013 Publication Journal of environmental radioactivity Abbreviated Journal J Environ Radioactiv  
  Volume 123 Issue Pages 63-70  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  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.  
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  Publisher Place of Publication Editor  
  Language Wos 000321177200007 Publication Date 2012-03-16  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0265-931x ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 2.31 Times cited (up) 16 Open Access  
  Notes ; We gratefully acknowledge the support provided by the Norwegian Ministry of Foreign Affairs and the European Commission (HASYLAB proposal I-20070051 EC and II-20090184 EC). The authors are indebted to Dr. Karen Appel and Dr. Manuela Borchert, Hasylab for beamline assistance. ; Approved Most recent IF: 2.31; 2013 IF: 3.571  
  Call Number UA @ admin @ c:irua:109558 Serial 5710  
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Author Denecke, M.A.; Brendebach, B.; de Nolf, W.; Falkenberg, G.; Janssens, K.; Simon, R. doi  openurl
  Title Spatially resolved micro-X-ray fluorescence and micro-X-ray absorption fine structure study of a fractured granite bore core following a radiotracer experiment Type A1 Journal article
  Year 2009 Publication Spectrochimica acta: part B : atomic spectroscopy Abbreviated Journal Spectrochim Acta B  
  Volume 64 Issue 8 Pages 791-795  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract Spatially resolved X-ray absorption and fluorescence investigation with a micrometer-scale resolution on actinide-containing samples provide information necessary for safety assessment of nuclear waste disposal. In this paper one example of such an experiment is presented. This example entails neptunium speciation in a fractured granite bore core from the Swedish Äspö Hard Rock Laboratory following a radiotracer experiment using µ-XAFS and µ-XRF. In order to probe micro-volumes below the surface in the granite samples and thereby avoid potential changes in the Np speciation during cutting of the bore core, a confocal irradiationdetection geometry is employed. µ-XAFS results for a selected granite bore core cross section with ~ 3 nmol Np/g reveal that Np, originally introduced as Np(V) in the tracer cocktail, is present in the granite in its reduced Np(IV) form. The Np(IV) is often present as particles, tens of µm in size. Elemental distribution maps show the tracer Np to be located in fissures and permeable channels not larger than 100 µm. The Np distribution appears often correlated with Zn also present in some fissures. We observe small granite fissures containing Fe (presumably Fe(II)), where we do not detect any Np. It is feasible that inflowing Np(V) has a shorter residence time in large fractures, while in the smaller fissures migration is slower, leading to longer residence times, i.e., reaction times, where it is reduced to less soluble Np(IV) and becomes thereby immobilized.  
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  Corporate Author Thesis  
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  Language Wos 000269995300013 Publication Date 2009-06-10  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0584-8547; 0038-6987 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 3.241 Times cited (up) 21 Open Access  
  Notes Approved Most recent IF: 3.241; 2009 IF: 2.719  
  Call Number UA @ admin @ c:irua:79740 Serial 5837  
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Author Basile, F.; Benito, P.; Bugani, S.; de Nolf, W.; Fornasari, G.; Janssens, K.; Morselli, L.; Scavetta, E.; Tonelli, D.; Vaccari, A. doi  openurl
  Title Combined use of synchrotron-radiation-based imaging techniques for the characterization of structured catalysts Type A1 Journal article
  Year 2010 Publication Advanced functional materials Abbreviated Journal Adv Funct Mater  
  Volume 20 Issue 23 Pages 4117-4126  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract Active-phase-coated metallic supports as structured catalysts are gaining attention in endothermic and exothermic processes because they improve heat transfer. The deposition of a well-adhered and stable catalyst layer on the metallic support constitutes an important feature for the successful application of the final material. In this work, coating of FeCrAlY foams is performed by a one-step electrosynthesis-deposition of hydrotalcite-type compounds, precursors of catalysts active in endothermic steam methane reforming. The catalysts are studied at different length scales by using, for the first time, a combination of several techniques: SEM/EDS and X-ray fluorescence, X-ray powder diffraction and absorption-tomography experiments on the micro- and nanoscales at a synchrotron facility. The results show that the morphology of the coating depends on the synthesis conditions and that the catalyst may be described as Ni metal crystallites dispersed on γ-Al2O3, homogeneously coating the FeCrAlY foam.  
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  Language Wos 000285392900010 Publication Date 2010-09-23  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 1616-301x ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 12.124 Times cited (up) 24 Open Access  
  Notes ; The authors give thanks to Dr. Cloetens, for helping during the absorption tomography experiments, performed at ID19 of the ESRF; and P. Blauet and R. Toucolou, for helping during the mu-XRF/XRPD and nano-XRF experiments at ID22 and ID22-NI of the ESRF. The financial support from the Ministero per l'Istruzione, l'Universita e la Ricerca (MIUR, Roma, Italy) is gratefully acknowledged. ; Approved Most recent IF: 12.124; 2010 IF: 8.508  
  Call Number UA @ admin @ c:irua:85834 Serial 5525  
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Author Legrand, S.; Alfeld, M.; Vanmeert, F.; de Nolf, W.; Janssens, K. pdf  doi
openurl 
  Title Macroscopic Fourier transform infrared scanning in reflection mode (MA-rFTIR), a new tool for chemical imaging of cultural heritage artefacts in the mid-infrared range Type A1 Journal article
  Year 2014 Publication The analyst Abbreviated Journal Analyst  
  Volume 139 Issue 10 Pages 2489-2498  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract In this paper we demonstrate that by means of scanning reflection FTIR spectroscopy, it is possible to record highly specific distribution maps of organic and inorganic compounds from flat, macroscopic objects with cultural heritage value in a non-invasive manner. Our previous work involved the recording of macroscopic distributions of chemical elements or crystal phases from painted works of art based on respectively macroscopic X-ray fluorescence or X-ray powder diffraction analysis. The use of infrared radiation instead of X-rays has the advantage that more specific information about the nature and distribution of the chemical compounds present can be gathered. This higher imaging specificity represents a clear advantage for the characterization of painting and artist materials. It allows the distribution of metallo-organic compounds to be visualized and permits distinguishing between pigmented materials containing the same key metal. The prototype instrument allows the recording of hyperspectral datacubes by scanning the surface of the artefact in a contactless and sequential single-point measuring mode, while recording the spectrum of reflected infrared radiation. After the acquisition, spectral line intensities of individual bands and chemical distribution maps can be extracted from the datacube to identify the compounds present and/or to highlight their spatial distribution. Not only is information gained on the surface of the investigated artefacts, but also images of overpainted paint layers and, if present, the underdrawing may be revealed in this manner. A current major limitation is the long scanning times required to record these maps.  
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  Language Wos 000334734200028 Publication Date 2014-02-19  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0003-2654 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 3.885 Times cited (up) 25 Open Access  
  Notes ; ; Approved Most recent IF: 3.885; 2014 IF: 4.107  
  Call Number UA @ admin @ c:irua:116595 Serial 5699  
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Author Cotte, M.; Checroun, E.; De Nolf, W.; Taniguchi, Y.; De Viguerie, L.; Burghammer, M.; Walter, P.; Rivard, C.; Salome, M.; Janssens, K.; Susini, J. pdf  doi
openurl 
  Title Lead soaps in paintings : friends or foes? Type A1 Journal article
  Year 2017 Publication Studies in conservation Abbreviated Journal Stud Conserv  
  Volume 62 Issue 1 Pages 2-23  
  Keywords A1 Journal article; Art; History; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract The origin(s) and role(s) of metal soaps in paints are a worldwide concern today. These hybrid compounds, containing both fatty acid chains and metals associated with a carboxylate function, are increasingly identified in paints. As reviewed in the first part of this work, the presence of metal soaps in paints is differently interpreted in scientific publications: metal soaps are sometimes considered to play a positive role as anchor points, during paint drying processes; they can also be considered as responsible for many degradation processes (protrusions, efflorescences, darkening, etc.). Their origins are also interpreted in various ways. In some paintings (in particular from the twentieth century), they have sometimes introduced on purpose, as additives, to modify the physical properties of the painting materials. In older paintings, metal soaps are usually thought to result from an uncontrolled reaction of oil with lead-based pigments, in particular lead white, red lead, and lead tin yellow. In the second part of this work, the review of historical recipes of lead-based paint shows an important number of recipes based on controlled mixing of oil with lead driers. In the third part, the experimental reproduction of such traditional recipes using walnut oil and litharge (PbO) shows that lead soaps can be formed, both in about one hour at approximate to 100 degrees C, or in about one month at room temperature. It shows as well that after a few years, litharge is no longer detected in the paint medium, while different lead carbonates are. Finally, the micro-infrared spectroscopy and micro-X-ray diffraction re-analysis of protrusions from a nine-year model painting shows together with lead soaps, the presence of Pb-5(CO3)(3)(OH)(2)O ('synthetic plumbonacrite'), an unusual phase recently observed in a protrusion from a painting by Vincent Van Gogh. This work highlights (i) the multiple origins and roles of metal soaps in paints and (ii) the importance of combining the analysis of fragments from historical paintings with the analysis and reproduction of historical recipes. In particular, we show that the components detected today in historical paintings may severely differ from those originally used or prepared by the painter, complicating the assessment of the painter's intentions. More than the presence of metal soaps, the key questions to be tackled should be about their origins and (re)mobilization.  
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  Language Wos 000393691200002 Publication Date 2016-10-03  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0039-3630; 2047-0584 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 0.578 Times cited (up) 26 Open Access  
  Notes ; This work was supported by the European Synchrotron Radiation Facility. ; Approved Most recent IF: 0.578  
  Call Number UA @ admin @ c:irua:141976 Serial 5690  
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Author Radepont, M.; Coquinot, Y.; Janssens, K.; Ezrati, J.-J.; de Nolf, W.; Cotte, M. url  doi
openurl 
  Title Thermodynamic and experimental study of the degradation of the red pigment mercury sulfide Type A1 Journal article
  Year 2015 Publication Journal of analytical atomic spectrometry Abbreviated Journal J Anal Atom Spectrom  
  Volume 30 Issue 3 Pages 599-612  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract The red pigment mercury sulfide, called cinnabar or vermilion, is well known to suffer from an alteration giving rise to a grey, grey-white or black color at the surface of degraded works of art. This phenomenon can dramatically affect the esthetical value of artworks. This work aims at assessing the factors (light, halides) influencing the instability of red mercury sulfide and understanding (by combining thermodynamic and experimental approaches) the chemical equilibria governing the formation and evolution of the different degradation compounds. From the thermodynamic study of the Hg-S-Cl-H2O system, it was concluded that Hg(0), Hg3S2Cl2, and Hg2Cl2 can be formed from the reaction of alpha-HgS with ClO(g). In the second part, the artificial ageing experiments presented were carried out on model samples following the conditions assessed in the first part, in order to reproduce natural ageing observed on red mercury sulfide. Similarly to degradation compounds detected on original works of art, mercury chlorine compounds such as calomel (Hg2Cl2) and corderoite (alpha-Hg3S2Cl2) were identified on the surface of alpha-HgS model samples, when exposed to light and a sodium hypochlorite solution. Sulfates were detected as well, and more particularly gypsum (CaSO4 center dot 2H(2)O) when Ca was originally present in the model sample. The relationship between color and composition is discussed as well.  
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  Language Wos 000350650800005 Publication Date 2015-01-02  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0267-9477 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 3.379 Times cited (up) 26 Open Access  
  Notes ; The authors gratefully acknowledge the ESRF for granting beamtime under proposal no. EC720. Michel Dubus is thanked for providing precious advices concerning ageing protocols. This research was supported by Belgian Science Policy project S2-ART (BELSPO S4DA), the GOA “SOLARPAINT” (Research Fund University of Antwerp, Belgium) and FWO (Brussels, Belgium) projects no. G.0C12.13, G.0704.08 and G.01769.09. ; Approved Most recent IF: 3.379; 2015 IF: 3.466  
  Call Number UA @ admin @ c:irua:125474 Serial 5877  
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Author Rouchon, V.; Duranton, M.; Burgaud, C.; Pellizzi, E.; Lavédrine, B.; Janssens, K.; de Nolf, W.; Nuyts, G.; Vanmeert, F.; Hellemans, K. doi  openurl
  Title Room-temperature study of iron gall ink impregnated paper degradation under various oxygen and humidity conditions : time-dependent monitoring by viscosity and X-ray absorption near-edge spectrometry measurements Type A1 Journal article
  Year 2011 Publication Analytical chemistry Abbreviated Journal Anal Chem  
  Volume 83 Issue 7 Pages 2589-2597  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract Many western manuscripts were written using iron gall inks. These inks can damage the paper via two major mechanisms: (a) acid hydrolysis, enhanced by humidity, and (b) oxidative depolymerization provoked by the presence of oxygen and free iron(II) ions. The degradation of unsized Whatman paper impregnated with different combinations of iron sulfate, gallic acid, and gum arabic was studied at room temperature in order to assess the relative importance of each mechanism. The samples were stored in various environments including a dry and/or an oxygen-free atmosphere. The cellulose depolymerization was monitored by viscometry and related to changes in the oxidation state of iron, determined by X-ray absorption near-edge spectrometry. The results indicate that residual amounts of oxygen (less than 0.1%) promote cellulose depolymerization, whereas the level of relative humidity has no impact. The cellulose depolymerization also appears closely correlated to oxidative mechanisms. Regarding the oxidation of iron, it only occurs in the simultaneous presence of oxygen and moisture, suggesting the occurrence of rustlike oxidative mechanisms. Finally, the presence of gallic acid has a strong influence, which is only partially explained by its capacity to reduce iron(III) to iron(II).  
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  Language Wos 000288887700028 Publication Date 2011-03-04  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0003-2700; 5206-882x ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 6.32 Times cited (up) 28 Open Access  
  Notes ; This research was supported by the French Ministry of Culture within the National Program of Research (“La conservation des manuscrits: etude du vieillissement naturel de papiers impregnes d'encres ferrogalliques”). It was funded by grants from HASYLAB (experiments I-20090280 EC and II-20060245 EC) and SOLEIL (proposals 20060396 and 20080761) and was supported by the Interuniversity Attraction Poles Programme Belgian Science Policy (1UAP V1/16). The text also presents results of GOA “XANES meets ELNES” (Research Fund University of Antwerp, Belgium) and from FWO (Brussels, Belgium) projects nos. G.0689.06, G.0704.08 and G017909N. We are thankful to Dr. Dominique Thaudiere, Dr. Solenn Reguer, Dr. Andrea Somogyi, Dr. Karen Appel, Dr. Manuela Borchert, and Dr. Gerald Falkenberg for their assistance and help during the experiments performed at SOLEIL beamline “DIFFABS” and at HASYLAB Beam line “L” respectively. ; Approved Most recent IF: 6.32; 2011 IF: 5.856  
  Call Number UA @ admin @ c:irua:89593 Serial 5822  
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Author van der Snickt, G.; Miliani, C.; Janssens, K.; Brunetti, B.G.; Romani, A.; Rosi, F.; Walter, P.; Castaing, J.; de Nolf, W.; Klaassen, L.; Labarque, I.; Wittermann, R. doi  openurl
  Title Material analyses of “Christ with singing and music-making Angels”, a late 15th-C panel painting attributed to Hans Memling and assistants : part 1 : non-invasive in situ investigations Type A1 Journal article
  Year 2011 Publication Journal of analytical atomic spectrometry Abbreviated Journal J Anal Atom Spectrom  
  Volume 26 Issue 11 Pages 2216-2229  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract In cultural heritage science, compositional data is traditionally obtained from works of art through the analysis of samples by means of various bench-top instruments (scanning electron microscope, Raman spectrometer, etc.). Alternatively, the object can be transported to a laboratory where it may be examined, usually by spectroscopic methods working in reflection mode. However, this paper describes how a complementary set of mobile and portable instruments was deployed in situ to gain a comprehensive view on the materials and related ageing compounds of an (almost) unmovable 15th-C polyptych, prior to and in preparation of the extraction of a limited number of samples. In line with the methodological approach discussed, PXRF was first employed as an efficient screening tool. The ensuing elemental data was supplemented by more specific information on both organic as inorganic materials supplied by reflection near- and mid-FTIR spectroscopy and fluorimetry. In completion, a limited number of diffraction patterns were collected with a mobile XRD instrument in order to identify the constituent crystalline phases in pigments, grounding materials and degradation products. In this way, it could be demonstrated how a rich array of colours was obtained by means of a limited palette of pigments: lead white, lead tin yellow, azurite, natural ultramarine, bone black, vermillion, madder lake, and a green copper-organo complex were detected and situated on the panels. Remarkably, next to chalk also gypsum was found in the ground layer(s) of this Western European easel painting. The relatively large surface of the background was covered with gold leaf; the analyses seem to point towards the labour-intensive water gilding technique. The versatility of this combination of analytical techniques was further illustrated by the accurate characterisation of degradation products affecting the readability and conservation of the painting: the overall presence of a calcium oxalate-based film of variable thickness was established. Nevertheless, further analysis of cross-sectioned samples was considered desirable in order to study the stratigraphy, to gain direct access to altered and sub-imposed layers and to allow highly detailed analysis of micrometric degradation products by state-of-the art techniques (i.e. synchrotron radiation).  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000296021800010 Publication Date 2011-09-23  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0267-9477 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 3.379 Times cited (up) 32 Open Access  
  Notes ; This research was supported by the Interuniversity Attraction Poles Programme – Belgian Science Policy (IUAP VI/16). The text also presents results of GOA “XANES meets ELNES” (Research Fund University of Antwerp, Belgium) and from FWO (Brussels, Belgium) projects no. G.0103.04, G.0689.06 and G.0704.08. The staff of the Royal Museum of Fine Arts Antwerp is acknowledged for this pleasant cooperation and the authorisation for the publication of the images in this article. Therefore, a word of gratitude to Paul Huvenne, Yolande Deckers, Stef Antonissen and Gwen Borms. In addition, the authors would like to thank the MOLAB's team operators Chiari Anselmi and Federica Presciutti. MOLAB analyses have been carried out through the support of the EU within the 6th Framework Programme (Contract Eu-ARTECH, RII3-CT-2004-506171). ; Approved Most recent IF: 3.379; 2011 IF: 3.220  
  Call Number UA @ admin @ c:irua:93680 Serial 5705  
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Author de Nolf, W.; Dik, J.; van der Snickt, G.; Wallert, A.; Janssens, K. doi  openurl
  Title High energy X-ray powder diffraction for the imaging of (hidden) paintings Type A1 Journal article
  Year 2011 Publication Journal of analytical atomic spectrometry Abbreviated Journal J Anal Atom Spectrom  
  Volume 26 Issue 5 Pages 910-916  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract Over the past few years a number of innovative imaging techniques have been introduced for the visualization of hidden paint layers in Old Master Paintings. These include X-ray fluorescence scanning, TeraHertz imaging, optical coherence tomography and other acoustics-based forms of visualization. All of these techniques are usually a trade-off between their penetrative capability on the one side and their analytical precision in terms of spatial resolution and material identification on the other. Here, we present the first-time use of High-Energy X-ray Powder Diffraction imaging (HE-XRPD) in the study of hidden layers in paintings. As an imaging tool, it combines high-depth sensitivity with fingerprint identification of most inorganic painting materials. The potential as well as some limitations of this technique are demonstrated using model paintings as well as an authentic 16th century painting.  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000289731900005 Publication Date 2011-03-17  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0267-9477 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 3.379 Times cited (up) 34 Open Access  
  Notes ; ; Approved Most recent IF: 3.379; 2011 IF: 3.220  
  Call Number UA @ admin @ c:irua:89922 Serial 5640  
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Author Cotte, M.; Pouyet, E.; Salome, M.; Rivard, C.; De Nolf, W.; Castillo-Michel, H.; Fabris, T.; Monico, L.; Janssens, K.; Wang, T.; Sciau, P.; Verger, L.; Cormier, L.; Dargaud, O.; Brun, E.; Bugnazet, D.; Fayard, B.; Hesse, B.; del Real, A.E.P.; Veronesi, G.; Langlois, J.; Balcar, N.; Vandenberghe, Y.; Sole, V.A.; Kieffer, J.; Barrett, R.; Cohen, C.; Cornu, C.; Baker, R.; Gagliardini, E.; Papillon, E.; Susini, J. doi  openurl
  Title The ID21 X-ray and infrared microscopy beamline at the ESRF: status and recent applications to artistic materials Type A1 Journal article
  Year 2017 Publication Journal of analytical atomic spectrometry Abbreviated Journal J Anal Atom Spectrom  
  Volume 32 Issue 3 Pages 477-493  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract The ID21 beamline (European Synchrotron Radiation facility, France) is a multi micro-analytical platform combining X-ray and infrared micro-probes, for characterization of elements, species, molecular groups and crystalline structures in complex materials. Applications are mainly in the fields of cultural heritage, life science, environmental and earth sciences, materials sciences. Here, we first present the status of instruments: (i) the scanning micro-spectroscopy end-station, operating from 2.0 to 9.2 keV, under vacuum and offering cryo conditions, for the acquisition of 2D micro X-ray fluorescence (mu XRF) maps, single point micro X-ray Absorption Near Edge Structure (mu XANES) spectra and speciation maps with sub-micrometric resolution; (ii) the XANES full-field end-station, operating in the same vacuum and energy conditions, for the acquisition of hyper-spectral radiographs of thin concentrated samples, resulting in speciation maps with micrometric resolution and millimetric field of view; (iii) the scanning micro-X-ray diffraction (mu XRD)/mu XRF end-station, operating at 8.5 keV, in air, for the acquisition of 2D crystalline phase maps, with micrometric resolution; and (iv) the scanning infrared microscope, operating in the mid-infrared range for the acquisition of molecular maps and some structural maps with micrometric resolution. Recent hardware and software developments are presented, as well as new protocols for improved sample preparation of thin sections. Secondly, a review of recent applications for the study of cultural heritage is presented, illustrated by various examples: determination of the origin of the color in blue Chinese porcelains and in brown Sevres porcelains; detection of lead in ink on Herculaneum papyri; identification and degradation of modeling materials used by Auguste Rodin and of chrome yellow pigments used by Vincent van Gogh. Cryo capabilities are illustrated by the analysis of plants exposed to chromate solutions. These examples show the variety of materials analyzed, of questions tackled, and particularly the multiple advantages of the ID21 analytical platform for the analysis of ancient and artistic materials.  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000396286900002 Publication Date 2016-12-14  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0267-9477 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 3.379 Times cited (up) 39 Open Access  
  Notes ; ; Approved Most recent IF: 3.379  
  Call Number UA @ admin @ c:irua:142493 Serial 5874  
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Author Radepont, M.; de Nolf, W.; Janssens, K.; van der Snickt, G.; Coquinot, Y.; Klaassen, L.; Cotte, M. doi  openurl
  Title The use of microscopic X-ray diffraction for the study of HgS and its degradation products corderoite (\alpha-Hg3S2Cl2), kenhsuite (\gamma-Hg3S2Cl2) and calomel (Hg2Cl2) in historical paintings Type A1 Journal article
  Year 2011 Publication Journal of analytical atomic spectrometry Abbreviated Journal J Anal Atom Spectrom  
  Volume 26 Issue 5 Pages 959-968  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract Since antiquity, the red pigment mercury sulfide (α-HgS), called cinnabar in its natural form or vermilion red when synthetic, was very often used in frescoes and paintings, even if it was known to suffer occasionally from degradation. The paint hereby acquires a black or silver-grey aspect. The chemical characterization of these alteration products is rather challenging mainly because of the micrometric size and heterogeneity of the surface layers that develop and that are responsible for the color change. Methods such as electron microscopy, synchrotron-based microscopic X-ray fluorescence, microscopic X-ray absorption near edge spectroscopy, Raman microscopy and secondary ion microscopy have been previously employed to identify the (Hg- and S-) compounds present and to study their co-localization. Next to these, also microscopic X-ray diffraction (XRD) (either by making use of laboratory X-ray sources or when used at a synchrotron facility) allows the identification of the crystal phases that are present in degraded HgS paint layers. In this paper we employ these various forms of micro-XRD to analyze degraded red paint in different paintings and compare the results with other X-ray based methods. Whereas the elemental analyses of the degradation products revealed, next to mercury and sulfur, the presence of chlorine, X-ray diffraction allowed the identification, next to α-HgS, of the Hg and S-containing compound calomel (Hg2Cl2) but also of the Hg, S and Cl-containing minerals corderoite (α-Hg3S2Cl2) and kenhsuite (γ-Hg3S2Cl2). These observations are consistent with X-ray absorption spectroscopy measurements performed at the S- and Cl-edges.  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000289731900011 Publication Date 2011-03-03  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0267-9477 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 3.379 Times cited (up) 40 Open Access  
  Notes ; The authors gratefully acknowledge GOA programme “XANES meets EELS'' (University of Antwerp Research Council), the IUAP VI/P16 programme ”Nacho'' (BELSPO, Brussels, Belgium) and FWO (Brussels, Belgium) projects no. G.0689.06, G.0704.08 and G017909N for financial support, the ESRF for granting beamtime under proposals no. EC442 and EC720, and Gema Martinez-Criado for practical help on ID18F. The KMSKA staff is also gratefully acknowledged for their help and interest. Javier Chillida is thanked for providing us with the Pedralbes samples. The authors are also indebted to the CHARISMA project (grant agreement 228330) for financial support. ; Approved Most recent IF: 3.379; 2011 IF: 3.220  
  Call Number UA @ admin @ c:irua:89927 Serial 5896  
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Author Janssens, K.; Alfeld, M.; van der Snickt, G.; de Nolf, W.; Vanmeert, F.; Radepont, M.; Monico, L.; et al. doi  openurl
  Title The use of synchrotron radiation for the characterization of artists' pigments and paintings Type A1 Journal article
  Year 2013 Publication Annual review of analytical chemistry Abbreviated Journal Annu Rev Anal Chem  
  Volume 6 Issue Pages 399-425  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  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.  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000323887500019 Publication Date 2013-06-18  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 1936-1327 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 7.435 Times cited (up) 46 Open Access  
  Notes ; ; Approved Most recent IF: 7.435; 2013 IF: 7.814  
  Call Number UA @ admin @ c:irua:111315 Serial 5902  
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Author Janssens, K.; de Nolf, W.; van der Snickt, G.; Vincze, L.; Vekemans, B.; Terzano, R.; Brenker, F.E. doi  openurl
  Title Recent trends in quantitative aspects of microscopic X-ray fluorescence analysis Type A1 Journal article
  Year 2010 Publication Trends in analytical chemistry Abbreviated Journal Trac-Trend Anal Chem  
  Volume 29 Issue 6 Pages 464-478  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000279235000014 Publication Date 2010-03-23  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0165-9936 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 8.442 Times cited (up) 48 Open Access  
  Notes ; This research was supported by the Interuniversity Attraction Poles Programme-Belgian Science Policy (IUAP VI/16). The text also presents results of FWO (Brussels, Belgium) projects nr. G.0704.08 and G.0179.09 and from the UA-BOF GOA programme. ; Approved Most recent IF: 8.442; 2010 IF: 6.602  
  Call Number UA @ admin @ c:irua:83903 Serial 5806  
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Author Lind, O.C.; Salbu, B.; Skipperud, L.; Janssens, K.; Jaroszewicz, J.; de Nolf, W. doi  openurl
  Title Solid state speciation and potential bioavailability of depleted uranium particles from Kosovo and Kuwait Type A1 Journal article
  Year 2009 Publication Journal of environmental radioactivity Abbreviated Journal J Environ Radioactiv  
  Volume 100 Issue 4 Pages 301-307  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract A combination of synchrotron radiation based X-ray microscopic techniques (ì-XRF, ì-XANES, ì-XRD) applied on single depleted uranium (DU) particles and semi-bulk leaching experiments has been employed to link the potential bioavailability of DU particles to site-specific particle characteristics. The oxidation states and crystallographic forms of U in DU particles have been determined for individual particles isolated from selected samples collected at different sites in Kosovo and Kuwait that were contaminated by DU ammunition during the 1999 Balkan conflict and the 1991 Gulf war. Furthermore, small soil or sand samples heavily contaminated with DU particles were subjected to simulated gastrointestinal fluid (0.16 M HCl) extractions. Characteristics of DU particles in Kosovo soils collected in 2000 and in Kuwait soils collected in 2002 varied significantly depending on the release scenario and to some extent on weathering conditions. Oxidized U (+6) was determined in large, fragile and bright yellow DU particles released during fire at a DU ammunition storage facility and crystalline phases such as schoepite (UO3·2.25H2O), dehydrated schoepite (UO3·0.75H2O) and metaschoepite (UO3·2.0H2O) were identified. As expected, these DU particles were rapidly dissolved in 0.16 M HCl (84 ± 3% extracted after 2 h) indicating a high degree of potential mobility and bioavailability. In contrast, the 2 h extraction of samples contaminated with DU particles originating either from corrosion of unspent DU penetrators or from impacted DU ammunition appeared to be much slower (2030%) as uranium was less oxidized (+4 to +6). Crystalline phases such as UO2, UC and metallic U or UTi alloy were determined in impacted DU particles from Kosovo and Kuwait, while the UO2,34 phase, only determined in particles from Kosovo, could reflect a more corrosive environment. Although the results are based on a limited number of DU particles, they indicate that the structure and extractability of DU particles released from similar sources (metallic U penetrators) will depend on the release scenarios (fire, impact) and to some extent environmental conditions. However, most of the DU particles (7396%) in all investigated samples were dissolved in 0.16 M HCl after one week indicating that a majority of the DU material is bioaccessible.  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000264649500004 Publication Date 2009-02-18  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0265-931x ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 2.31 Times cited (up) 49 Open Access  
  Notes Approved Most recent IF: 2.31; 2009 IF: 1.268  
  Call Number UA @ admin @ c:irua:76413 Serial 5834  
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Author Janssens, K.; van der Snickt, G.; Vanmeert, F.; Legrand, S.; Nuyts, G.; Alfeld, M.; Monico, L.; Anaf, W.; de Nolf, W.; Vermeulen, M.; Verbeeck, J.; De Wael, K. pdf  doi
openurl 
  Title Non-invasive and non-destructive examination of artistic pigments, paints, and paintings by means of X-Ray methods Type A1 Journal article
  Year 2016 Publication Topics in Current Chemistry Abbreviated Journal Topics Curr Chem  
  Volume 374 Issue 374 Pages 81  
  Keywords A1 Journal article; Electron microscopy for materials research (EMAT); AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract Recent studies are concisely reviewed, in which X-ray beams of (sub)micrometre to millimetre dimensions have been used for non-destructive analysis and characterization of pigments, minute paint samples, and/or entire paintings from the seventeenth to the early twentieth century painters. The overview presented encompasses the use of laboratory and synchrotron radiation-based instrumentation and deals with the use of several variants of X-ray fluorescence (XRF) as a method of elemental analysis and imaging, as well as with the combined use of X-ray diffraction (XRD) and X-ray absorption spectroscopy (XAS). Microscopic XRF is a variant of the method that is well suited to visualize the elemental distribution of key elements, mostly metals, present in paint multi-layers, on the length scale from 1 to 100 μm inside micro-samples taken from paintings. In the context of the characterization of artists pigments subjected to natural degradation, the use of methods limited to elemental analysis or imaging usually is not sufficient to elucidate the chemical transformations that have taken place. However, at synchrotron facilities, combinations of μ-XRF with related methods such as μ-XAS and μ-XRD have proven themselves to be very suitable for such studies. Their use is often combined with microscopic Fourier transform infra-red spectroscopy and/or Raman microscopy since these methods deliver complementary information of high molecular specificity at more or less the same length scale as the X-ray microprobe techniques. Since microscopic investigation of a relatively limited number of minute paint samples, taken from a given work of art, may not yield representative information about the entire artefact, several methods for macroscopic, non-invasive imaging have recently been developed. Those based on XRF scanning and full-field hyperspectral imaging appear very promising; some recent published results are discussed.  
  Address  
  Corporate Author Thesis  
  Publisher Springer international publishing ag Place of Publication Cham Editor  
  Language Wos 000391178900006 Publication Date 2016-11-21  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 2365-0869;2364-8961; ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 4.033 Times cited (up) 50 Open Access  
  Notes ; ; Approved Most recent IF: 4.033  
  Call Number UA @ lucian @ c:irua:139930UA @ admin @ c:irua:139930 Serial 4443  
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Author van der Snickt, G.; de Nolf, W.; Vekemans, B.; Janssens, K. doi  openurl
  Title μ-XRF/μ-RS vs. SR μ-XRD for pigment identification in illuminated manuscripts Type A1 Journal article
  Year 2008 Publication Applied physics A : materials science & processing Abbreviated Journal Appl Phys A-Mater  
  Volume 92 Issue 1 Pages 59-68  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract For the non-destructive identification of pigments and colorants in works of art, in archaeological and in forensic materials, a wide range of analytical techniques can be used. Bearing in mind that every method holds particular limitations, two complementary spectroscopic techniques, namely confocal ì-Raman spectroscopy (ì-RS) and ì-X-ray fluorescence spectroscopy (ì-XRF), were joined in one instrument. The combined ì-XRF and ì-RS device, called PRAXIS unites both complementary techniques in one mobile setup, which allows ì- and in situ analysis. ì-XRF allows one to collect elemental and spatially-resolved information in a non-destructive way on major and minor constituents of a variety of materials. However, the main disadvantages of ì-XRF are the penetration depth of the X-rays and the fact that only elements and not specific molecular combinations of elements can be detected. As a result ì-XRF is often not specific enough to identify the pigments within complex mixtures. Confocal Raman microscopy (ì-RS) can offer a surplus as molecular information can be obtained from single pigment grains. However, in some cases the presence of a strong fluorescence background limits the applicability. In this paper, the concrete analytical possibilities of the combined PRAXIS device are evaluated by comparing the results on an illuminated sheet of parchment with the analytical information supplied by synchrotron radiation ì-X-ray diffraction (SR ì-XRD), a highly specific technique.  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000256426000008 Publication Date 2008-03-19  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0947-8396 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 1.455 Times cited (up) 56 Open Access  
  Notes Approved Most recent IF: 1.455; 2008 IF: 1.884  
  Call Number UA @ admin @ c:irua:74465 Serial 5695  
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Author van der Snickt, G.; Janssens, K.; Dik, J.; de Nolf, W.; Vanmeert, F.; Jaroszewicz, J.; Cotte, M.; Falkenberg, G.; Van der Loeff, L. doi  openurl
  Title 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 Type A1 Journal article
  Year 2012 Publication Analytical chemistry Abbreviated Journal Anal Chem  
  Volume 84 Issue 23 Pages 10221-10228  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  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.  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000311815300013 Publication Date 2012-08-30  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0003-2700; 5206-882x ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 6.32 Times cited (up) 59 Open Access  
  Notes ; This research was supported by BELSPO via the Interuniversity Attraction Poles Programme (IUAP VI/16) and the S2-ART project (SD/RI/04A) and funded by Grants from the ESRF (EC-442) and PETRA-III (I-20120312 EC). The text also presents results of GOA “XANES meets ELNES” (Research Fund University of Antwerp, Belgium) and from FWO (Brussels, Belgium) project nos. G.0103.04, G.0689.06, and G.0704.08. The staff of the Kroller-Muller Museum and painting conservators Margje Leeuwestein and Esther Van Duijn are acknowledged for this pleasant cooperation and the authorization for the publication of the images in this article. ; Approved Most recent IF: 6.32; 2012 IF: 5.695  
  Call Number UA @ admin @ c:irua:105971 Serial 5526  
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Author Terzano, R.; Spagnuolo, M.; Vekemans, B.; de Nolf, W.; Janssens, K.; Falkenberg, G.; Ruggiero, P. doi  openurl
  Title Assessing the origin and fate of CR, Ni, Cu, Zn, Ph, and V in industrial polluted soil by combined microspectroscopic techniques and bulk extraction methods Type A1 Journal article
  Year 2007 Publication Environmental science & technology Abbreviated Journal  
  Volume 41 Issue 19 Pages 6762-6769  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000249840600024 Publication Date 2007-08-29  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor Times cited (up) 61 Open Access  
  Notes Approved Most recent IF: NA  
  Call Number UA @ admin @ c:irua:66622 Serial 5481  
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Author de Nolf, W.; Vanmeert, F.; Janssens, K. pdf  doi
openurl 
  Title XRDUA : crystalline phase distribution maps by two-dimensional scanning and tomographic (micro) X-ray powder diffraction Type A1 Journal article
  Year 2014 Publication Journal of applied crystallography Abbreviated Journal  
  Volume 47 Issue 3 Pages 1107-1117  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract Imaging of crystalline phase distributions in heterogeneous materials, either plane projected or in virtual cross sections of the object under investigation, can be achieved by scanning X-ray powder diffraction employing X-ray micro beams and X-ray-sensitive area detectors. Software exists to convert the two-dimensional powder diffraction patterns that are recorded by these detectors to one-dimensional diffractograms, which may be analysed by the broad variety of powder diffraction software developed by the crystallography community. However, employing these tools for the construction of crystalline phase distribution maps proves to be very difficult, especially when employing micro-focused X-ray beams, as most diffraction software tools have mainly been developed having structure solution in mind and are not suitable for phase imaging purposes. XRDUA has been developed to facilitate the execution of the complete sequence of data reduction and interpretation steps required to convert large sequences of powder diffraction patterns into a limited set of crystalline phase maps in an integrated fashion.  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000336738500031 Publication Date 2014-05-28  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0021-8898 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor Times cited (up) 62 Open Access  
  Notes ; The authors would like to thank the synchrotron beamline staff at ID15 (ESRF, Grenoble, France), MicroXAS (SLS, Villigen, Switzerland) and PO6/BL-L (Petra III/Hasylab, Hamburg, Germany) for accommodating the experiments presented in this paper. Support from FWO 'Big Science' project G0C1213N as well as from the BELSPO project 'S2ART' (SD/RI/04A) is acknowledged. ; Approved Most recent IF: NA  
  Call Number UA @ admin @ c:irua:117758 Serial 5920  
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Author de Nolf, W.; Janssens, K. doi  openurl
  Title Micro X-ray diffraction and fluorescence tomography for the study of multilayered automotive paints Type A1 Journal article
  Year 2010 Publication Surface and interface analysis Abbreviated Journal Surf Interface Anal  
  Volume 42 Issue 5 Pages 411-418  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract Combined microscopic X-ray fluorescence/microscopic X-ray diffraction (µ-XRF/µ-XRD) tomography is a recently developed method that allows the visualization of the distribution of chemical elements and the associated crystalline phases inside complex, heterogeneous materials of extended thickness (millimeter range) in a nondestructive fashion. In this paper, the accuracy and resolution with which the individual layers in a multilayer stack of automotive paints can be distinguished is evaluated, and some of their properties measured. A paint layer system of eight layers was investigated, in which eight different crystalline substances were identified, each layer consisting of an organic, synthetic resin doped with finely milled inorganic compounds that serve as pigments or to strengthen the layer. In the XRD tomograms, all paint layers could be straightforwardly distinguished and their average thickness calculated. In case the filtered back projection method was used for tomogram reconstruction, a spatial resolution comparable to the microbeam size was obtained indicating no significant reconstruction blurring. When a more robust reconstruction method, such as the maximum-likelihood expectation maximization method, was employed, tomograms showing fewer artifacts were obtained, but with a spatial resolution that was two times worse. In the corresponding XRF tomograms, significant self-absorption distorted the element-specific tomograms corresponding to the low-energy (<7 keV) characteristic radiation and limited their usefulness. It can be concluded that microbeam XRD tomography allows the accurate visualization of the distribution of crystalline phases in multilayered automotive paint materials of millimeter dimensions with sufficient resolution to allow separate characterization of each layer in terms of its crystal-phase composition and thickness.  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000277350900012 Publication Date 2009-11-10  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0142-2421 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 1.132 Times cited (up) 70 Open Access  
  Notes ; This research was supported by the Interuniversity Attraction Poles Programme-Belgian Science Policy (IUAP VI/16) and funded by beam time grants from HASYLAB. This paper also presents results from a GOA project of the Research Fund of the University of Antwerp (Belgium), and of FWO (Brussels, Belgium) project nos. G.0177.03, G.0103.04, and G.0689.06. We also would like to acknowledge the Institute of Forensic Research in Krakow, Poland, and in particular Dr J. Zieba for providing the paint layer sample. ; Approved Most recent IF: 1.132; 2010 IF: 1.249  
  Call Number UA @ admin @ c:irua:82764 Serial 5717  
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Author Monico, L.; van der Snickt, G.; Janssens, K.; de Nolf, W.; Miliani, C.; Dik, J.; Radepont, M.; Hendriks, E.; Geldof, M.; Cotte, M. doi  openurl
  Title Degradation process of lead chromate in paintings by Vincent van Gogh studied by means of synchrotron X-ray spectromicroscopy and related methods : 2 : original paint layer samples Type A1 Journal article
  Year 2011 Publication Analytical chemistry Abbreviated Journal Anal Chem  
  Volume 83 Issue 4 Pages 1224-1231  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract The darkening of the original yellow areas painted with the chrome yellow pigment (PbCrO4, PbCrO4·xPbSO4, or PbCrO4·xPbO) is a phenomenon widely observed on several paintings by Vincent van Gogh, such as the famous different versions of Sunflowers. During our previous investigations on artificially aged model samples of lead chromate, we established for the first time that darkening of chrome yellow is caused by reduction of PbCrO4 to Cr2O3·2H2O (viridian green), likely accompanied by the presence of another Cr(III) compound, such as either Cr2(SO4)3·H2O or (CH3CO2)7Cr3(OH)2 [chromium(III) acetate hydroxide]. In the second part of this work, in order to demonstrate that this reduction phenomenon effectively takes place in real paintings, we study original paint samples from two paintings of V. van Gogh. As with the model samples, in view of the thin superficial alteration layers that are present, high lateral resolution spectroscopic methods that make use of synchrotron radiation (SR), such as microscopic X-ray absorption near edge (μ-XANES) and X-ray fluorescence spectrometry (μ-XRF) were employed. Additionally, μ-Raman and mid-FTIR analyses were carried out to completely characterize the samples. On both paint microsamples, the local presence of reduced Cr was demonstrated by means of μ-XANES point measurements. The presence of Cr(III) was revealed in specific areas, in some cases correlated to the presence of Ba(sulfate) and/or to that of aluminum silicate compounds.  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000287176900012 Publication Date 2011-02-14  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0003-2700; 5206-882x ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 6.32 Times cited (up) 84 Open Access  
  Notes ; This research was funded by grants from ESRF (experiment EC-504) and by HASYLAB (experiments 11-20080130 EC and 11-20070157 EC) and was supported by the Interuniversity Attraction Poles Programme-Belgian Science Policy (IUAP VI/16). The text also presents results of GOA “XANES meets ELNES” (Research Fund University of Antwerp, Belgium) and from FWO (Brussels, Belgium) project nos. G.0103.04, G.0689.06, and G.0704.08. The staff of the Van Gogh Museum, Amsterdam, is acknowledged for their agreeable cooperation and for the authorization to publish the images of the paintings in this article. L.M. was financially supported by the Erasmus Placement in the framework of Lifelong Learning Programme (A.Y. 2009-2010). The EU Community's FP7 Research Infrastructures program under the CHARISMA Project (Grant Agreement 228330) is also acknowledged. ; Approved Most recent IF: 6.32; 2011 IF: 5.856  
  Call Number UA @ admin @ c:irua:88795 Serial 5571  
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Author van der Snickt, G.; Dik, J.; Cotte, M.; Janssens, K.; Jaroszewicz, J.; de Nolf, W.; Groenewegen, J.; van der Loeff, L. doi  openurl
  Title Characterization of a degraded cadmium yellow (CdS) pigment in an oil painting by means of synchrotron radiation based X-ray techniques Type A1 Journal article
  Year 2009 Publication Analytical chemistry Abbreviated Journal Anal Chem  
  Volume 81 Issue 7 Pages 2600-2610  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract On several paintings of James Ensor (1860−1949), a gradual fading of originally bright yellow areas, painted with the pigment cadmium yellow (CdS), is observed. Additionally, in some areas exposed to light, the formation of small white-colored globules on top of the original paint surface is observed. In this paper the chemical transformation leading to the color change and to the formation of the globules is elucidated. Microscopic X-ray absorption near-edge spectroscopy (ì-XANES) experiments show that sulfur, originally present in sulfidic form (S2−), is oxidized during the transformation to the sulfate form (S6+). Upon formation (at or immediately below the surface), the highly soluble cadmium sulfate is assumed to be transported to the surface in solution and reprecipitates there, forming the whitish globules. The presence of cadmium sulfate (CdSO4·2H2O) and ammonium cadmium sulfate [(NH4)2Cd(SO4)2] at the surface is confirmed by microscopic X-ray diffraction measurements, where the latter salt is suspected to result from a secondary reaction of cadmium sulfate with ammonia. Measurements performed on cross sections reveal that the oxidation front has penetrated into the yellow paint down to ca. 1−2 ìm. The morphology and elemental distribution of the paint and degradation product were examined by means of scanning electron microscopy equipped with an energy-dispersive spectrometer (SEM-EDS) and synchrotron radiation based micro-X-ray fluorescence spectrometry (SR ì-XRF). In addition, ultraviolet-induced visible fluorescence photography (UIVFP) revealed itself to be a straightforward technique for documenting the occurrence of this specific kind of degradation on a macroscale by painting conservators.  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000264759400025 Publication Date 2009-03-11  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0003-2700; 5206-882x ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 6.32 Times cited (up) 91 Open Access  
  Notes Approved Most recent IF: 6.32; 2009 IF: 5.214  
  Call Number UA @ admin @ c:irua:76415 Serial 5501  
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Author Alfeld, M.; Janssens, K.; Dik, J.; de Nolf, W.; van der Snickt, G. doi  openurl
  Title Optimization of mobile scanning macro-XRF systems for the in situ investigation of historical paintings Type A1 Journal article
  Year 2011 Publication Journal of analytical atomic spectrometry Abbreviated Journal J Anal Atom Spectrom  
  Volume 26 Issue 5 Pages 899-909  
  Keywords A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract Elemental distribution maps are of great interest in the study of historical paintings, as they allow to investigate the pigment use of the artist, to image changes made in the painting during or after its creation and in some cases to reveal discarded paintings that were later over painted. Yet a method that allows to record such maps of a broad range of elements in a fast, non-destructive and in situ manner is not yet commonly available; a dedicated mobile scanning XRF instrument might fill this gap. In this paper we present three self-built scanning macro-XRF instruments, each based on the experience gained with its precursor. These instruments are compared in terms of sensitivity and limits of detection, which includes a discussion of the use of polycapillary optics and pinhole collimators as beam defining devices. Furthermore, the imaging capabilities of the instruments are demonstrated in three exemplary cases: (parts of) historical paintings from the 15th to the 19th century are examined. These cases illustrate the value of element specific distribution maps in the study of historical paintings and allow in the case of Vincent van Gogh's Patch of Grass a direct comparison between in situ and synchrotron based scanning macro-XRF.  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Editor  
  Language Wos 000289731900004 Publication Date 2011-03-21  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0267-9477 ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 3.379 Times cited (up) 107 Open Access  
  Notes ; The investigation of the “Triptych of the Seven Sacraments'' was done in collaboration with Griet Steyaert, independent restorer, and Lizet Klaassen, Royal Museum of Fine Arts (Antwerp, Belgium). The investigation of ”Patch of Grass'' was realized in collaboration with Luuk van der Loeff, Kroller-Muller-Museum (Otterlo, The Netherlands). M. Alfeld is a PhD fellowship of the Research Foundation-Flanders (FWO). This research was supported by the Interuniversity Attraction Poles Programme-Belgian Science Policy (IUAP VI/16) NACHO. The text also presents results of GOA "XANES meets ELNES'' (Research Fund University of Antwerp, Belgium) and from FWO (Brussels, Belgium) projects no. G.0103.04, G.0689.06 and G.0704.08. Further, the work presented was sponsored by the Innovational Research Incentives Scheme of the Netherlands Organization for Scientific Research, NWO (proj. no. 016.118.303). ; Approved Most recent IF: 3.379; 2011 IF: 3.220  
  Call Number UA @ admin @ c:irua:89919 Serial 5758  
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Author Monico, L.; van der Snickt, G.; Janssens, K.; de Nolf, W.; Miliani, C.; Verbeeck, J.; Tian, H.; Tan, H.; Dik, J.; Radepont, M.; Cotte, M. pdf  doi
openurl 
  Title Degradation process of lead chromate in paintings by Vincent van Gogh studied by means of synchrotron X-ray spectromicroscopy and related methods : 1 : artificially aged model samples Type A1 Journal article
  Year 2011 Publication Analytical chemistry Abbreviated Journal Anal Chem  
  Volume 83 Issue 4 Pages 1214-1223  
  Keywords A1 Journal article; Electron microscopy for materials research (EMAT); AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)  
  Abstract On several paintings by artists of the end of the 19th century and the beginning of the 20th Century a darkening of the original yellow areas, painted with the chrome yellow pigment (PbCrO4, PbCrO4·xPbSO4, or PbCrO4·xPbO) is observed. The most famous of these are the various Sunflowers paintings Vincent van Gogh made during his career. In the first part of this work, we attempt to elucidate the degradation process of chrome yellow by studying artificially aged model samples. In view of the very thin (1−3 μm) alteration layers that are formed, high lateral resolution spectroscopic methods such as microscopic X-ray absorption near edge (μ-XANES), X-ray fluorescence spectrometry (μ-XRF), and electron energy loss spectrometry (EELS) were employed. Some of these use synchrotron radiation (SR). Additionally, microscopic SR X-ray diffraction (SR μ-XRD), μ-Raman, and mid-FTIR spectroscopy were employed to completely characterize the samples. The formation of Cr(III) compounds at the surface of the chrome yellow paint layers is particularly observed in one aged model sample taken from a historic paint tube (ca. 1914). About two-thirds of the chromium that is present at the surface has reduced from the hexavalent to the trivalent state. The EELS and μ-XANES spectra are consistent with the presence of Cr2O3·2H2O (viridian). Moreover, as demonstrated by μ-XANES, the presence of another Cr(III) compound, such as either Cr2(SO4)3·H2O or (CH3CO2)7Cr3(OH)2 [chromium(III) acetate hydroxide], is likely.  
  Address  
  Corporate Author Thesis  
  Publisher Place of Publication Washington, D.C. Editor  
  Language Wos 000287176900011 Publication Date 2011-02-14  
  Series Editor Series Title Abbreviated Series Title  
  Series Volume Series Issue Edition  
  ISSN 0003-2700;1520-6882; ISBN Additional Links UA library record; WoS full record; WoS citing articles  
  Impact Factor 6.32 Times cited (up) 113 Open Access  
  Notes Iuap; Fwo Approved Most recent IF: 6.32; 2011 IF: 5.856  
  Call Number UA @ lucian @ c:irua:88794UA @ admin @ c:irua:88794 Serial 632  
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