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“Chemical imaging of stained-glass windows by means of macro X-ray fluorescence (MA-XRF) scanning”. van der Snickt G, Legrand S, Caen J, Vanmeert F, Alfeld M, Janssens K, Microchemical journal 124, 615 (2016). http://doi.org/10.1016/J.MICROC.2015.10.010
Abstract: Since the recent development of a mobile setup, MA-XRF scanning proved a valuable tool for the non-invasive, technical study of paintings. In this work, the applicability of MA-XRF scanning for investigating stained-glass windows inside a conservation studio is assessed by analysis of a high-profile, well-studied late-mediaeval panel. Although accurate quantification of components is not feasible with this analytical imaging technique, plotting the detected intensities of K versus Ca in a scatter plot allowed distinguishing glass fragments of different compositional types within the same panel. In particular, clusters in the Ca/K correlation plot revealed the presence of two subtypes of potash glass and three subtypes of high lime low alkali glass. MA-XRF results proved consistent with previous quantitative SEM-EDX analysis on two samples and analytical-based theories on glass production in the Low Countries formulated in literature. A bi-plot of the intensities of the more energetic Rb-K versus Sr-K emission lines yielded a similar glass type differentiation and is here presented as suitable alternative in case the Ca/K signal ratio is affected by superimposed weathering crusts. Apart from identification of the chromophores responsible for the green, blue and red glass colors, contrasting the associated elemental distribution maps obtained on the exterior and interior side of the glass permitted discriminating between colored pot metal glass and multi-layered flashed glass as well. Finally, the benefit of obtaining compositional information from the entire surface, as opposed to point analysis, was illustrated by the discovery of what appears to be a green cobalt glass a feature that was previously missed on this well-studied stained-glass window, both by connoisseurs and spectroscopic sample analysis. (C) 2015 Elsevier B.V. All rights reserved.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Antwerp Cultural Heritage Sciences (ARCHES)
Impact Factor: 3.034
Times cited: 22
DOI: 10.1016/J.MICROC.2015.10.010
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“Chromium speciation methods and infrared spectroscopy for studying the chemical reactivity of lead chromate-based pigments in oil medium”. Monico L, Janssens K, Cotte M, Sorace L, Vanmeert F, Brunetti BG, Miliani C, Microchemical journal
T2 –, TECHNART Conference, APR 27-30, 2015, Catania, ITALY 124, 272 (2016). http://doi.org/10.1016/J.MICROC.2015.08.028
Abstract: Environmental factors, such as light, humidity and temperature are triggering agents for the alteration of organic and/or inorganic constituents of oil paintings. The oxidation of the organic material is favored by increasing of relative humidity and temperature, whereas processes involving changes of the oxidation states of a number of inorganic pigments (e.g., vermilion, cadmium yellows, zinc yellows, chrome yellows) are mainly activated by light-exposure. In view of the optimization of the long-term conservation and restoration strategies of paintings it is of relevant interest to establish the consequences of thermal parameters (temperature and relative humidity) on the chemical/photochemical-reactivity and the nature of the alteration products of light sensitive-pigments in oil medium. To this aim here we propose a multi-method analytical approach based on the combination of diffuse reflectance UV-Vis, FTIR, synchrotron radiation (SR)-based micro X-ray fluorescence (mu-XRF)/micro-X-ray absorption neat edge structure ()CANES) and electron paramagnetic resonance (EPR) spectroscopies for studying the effects of different relative humidity conditions before and after light exposure on the reactivity of a series of lead chromate-based pigments [such as PbCrO4 center dot PbO (monoclinic), PbCrO4 (monoclinic) and PbCr0.2S0.8O4 (orthorhombic)] in an oil medium. The investigation of paint models was also compared to that of a late 19th century historical orthorhombic PbCr0.4S0.6O4 oil paint. Diffuse reflectance UV-Vis and FTIR spectroscopies were used to obtain information associated with chromatic changes and the formation of organo-metal degradation products at the paint surface. SR-based Cr K-edge mu-XANES/mu-XRF mapping analysis and EPR spectroscopy were employed in a complementary fashion to determine the amount, nature and distribution of Cr(III) and Cr(V)-based alteration compounds within the paints with micrometric spatial resolution. Under the employed thermal aging conditions, lead(II)-carboxylates and reduced Cr-compounds (in abundance of up to about 35% at the surface) have been identified in the lead chromate-based paints. The tendency of chromates to become reduced increased with increasing moisture levels and was favored for the orthorhombic PbCr0.2S0.8O4 compounds. The redox process gave rise to the formation of Cr(V)-species in relative amount much higher than that was formed in the equivalent paint which was exposed only to light. After light-exposure of the thermally aged paints, compounds ascribable to the oxidation of the organic binder were detected for all the types of pigments. Nevertheless, the previous thermal treatment increased the tendency toward photo-reduction of only the PbCr0.2S0.8O4 pigment. For this light-sensitive compound, the thickness variation of the reduced Cr-rich (ca. 70%) photo-alteration layer with moisture levels could be ascribed to a surface passivation phenomenon that had already occurred before photochemical aging. (C) 2015 Elsevier B.V. All rights reserved.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.034
Times cited: 23
DOI: 10.1016/J.MICROC.2015.08.028
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“Development of a new portable X-ray powder diffractometer and its demonstration to on-site analysis of two selected old master paintings from the Rijksmuseum”. Hirayama A, Abe Y, van Loon A, De Keyser N, Noble P, Vanmeert F, Janssens K, Tantrakarn K, Taniguchi K, Nakai I, Microchemical journal 138, 266 (2018). http://doi.org/10.1016/J.MICROC.2018.01.003
Abstract: A portable X-ray powder diffractometer (p-XRD) PT-APXRD III has been developed for onsite analysis of paintings and archaeological samples. By using a Cu anode X-ray tube and a silicon drift diode (SDD) detector, diffraction patterns with a high signalnoise (S/N) ratio can be recorded. The X-ray tube can be operated at a maximum voltage of 60 kV, which makes it possible to simultaneously record X-ray fluorescence spectra up to the high-energy region. The total weight of this instrument is 16 kg, which can be carried anywhere and the goniometer unit (5.6 kg) can be placed on a tripod for analysis of mural paintings. We brought the instrument to the Rijksmuseum in the Netherlands to examine its applicability for the analysis of oil paintings. We successfully analyzed two seventeenthcentury oil paintings by Johannes Vermeer and Jan Davidsz de Heem (copy after). Ultramarine blue, leadtin yellow type I, and Naples yellow were identified from the diffraction patterns, demonstrating the high practicality of this instrument. Furthermore, it was found from the SEM-EDX analysis of a paint cross section that the yellow pigment was applied in separate layers rather than being mixed. This diffractometer will be commercially available in the near future and will have many applications in the field of material analysis. (C) 2018 Elsevier B.V. All rights reserved.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.034
Times cited: 2
DOI: 10.1016/J.MICROC.2018.01.003
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“Evaluation of airborne particles at the Alhambra monument in Granada, Spain”. Horemans B, Cardell C, Bencs L, Kontozova-Deutsch V, De Wael K, Van Grieken R, Microchemical journal 99, 429 (2011). http://doi.org/10.1016/J.MICROC.2011.06.018
Abstract: As a part of an ongoing investigation regarding the air quality at the Alhambra monument (UNESCO World Cultural Heritage), indoor and outdoor atmospheric aerosols (PM1 and PM10-1) and pollutant gases (O3, NO2, SO2 and NH3) were studied during summer and winter. Bulk elements, ionic compounds and black carbon (BC) in aerosols were analyzed with X-ray fluorescence spectrometry, ion chromatography and aethalometry/reflectometry, respectively. Natural PM10-1 aerosols, such as carbonate-rich soil and sea salts, reacted with a typical urban atmosphere, producing a mixture of particulates with diverse chemical composition. The content/formation of secondary inorganic aerosols depended on the air temperature and absolute humidity. Ratios of typical mineral elements (i.e., Ti/Fe and Si/Fe) showed that Saharan dust events contribute to the composition of the observed mineral aerosol content. BC, V and Ni originated from diesel exhaust, while Cu, Cr, Pb and Zn came mainly from non-exhaust vehicular emissions. Weathering phenomena, such as blackening and pigment discoloration, which could arise from gradual aerosol deposition indoors, are discussed.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.034
Times cited: 39
DOI: 10.1016/J.MICROC.2011.06.018
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“In situ macro X-ray fluorescence (MA-XRF) scanning as a non-invasive tool to probe for subsurface modifications in paintings by PP Rubens”. van der Snickt G, Legrand S, Slama I, Van Zuien E, Gruber G, Van der Stighelen K, Klaassen L, Oberthaler E, Janssens K, Microchemical journal 138, 238 (2018). http://doi.org/10.1016/J.MICROC.2018.01.019
Abstract: Within the last decade, the established synchrotron- and laboratory-based micro-XRF scanning technology inspired the development of mobile instruments that allow performing in situ experiments on paintings on a macro scale. Since the development of the first mobile scanner at the start of this decade, this chemical imaging technique has brought new insights with respect to several iconic paintings, especially in cases when standard imaging techniques such as X-Ray Radiography (XRR) or Infrared Refiectography (IRR) yielded ambiguous results. The ability of scanning MA-XRF to visualise the distribution of elements detected at and below the paint surface renders this spectrometric method particularly helpful for studying painting techniques and revealing materials that remain hidden below the paint surface. The latter aspect is especially relevant for the technical study of works by Pieter Paul Rubens (1577-1640) as this highly productive seventeenth century master is particularly renowned for the continuous application of modifications during (and even after) the entire course of the creative process. In this work, the added value of MA-XRF scanning experiments for visualising these subsurface features is exemplified by interpreting the chemical images obtained on three of Rubens' key works. Special attention is given to three types of adjustments that are particularly relevant for the technical study of Rubens' oeuvre: (1) compositional changes ('pentimenti'), exemplified by results obtained on The Portrait of Helene Fourment (ca. 1638), (2) extensions to the support ('Anstlickungen.), illustrated by imaging experiments performed on the Venus Frigida (1614) and (3) Rubens' intriguing halos around flesh tones, as found amongst others in The Incredulity of Saint Thomas (1613). The ensuing insights in the paint stratigraphy and the underlying supporting structure illustrate the potential of MA-XRF scanning for the non-invasive, comparative study of Rubens' oeuvre. The results do not only augment the understanding of the complex genesis of Rubens' works of art and his efficient painting technique, but prove valuable during conservation treatments as well, as addressed in this paper. (C) 2018 Elsevier B.V. All rights reserved.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.034
Times cited: 5
DOI: 10.1016/J.MICROC.2018.01.019
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“Macro X-ray fluorescence (MA-XRF) scanning of illuminated manuscript fragments: potentialities and challenges”. Ricciardi P, Legrand S, Bertolotti G, Janssens K, Microchemical journal
T2 –, TECHNART Conference, APR 27-30, 2015, Catania, ITALY 124, 785 (2016). http://doi.org/10.1016/J.MICROC.2015.10.020
Abstract: Macro X-ray fluorescence scanning (MA-XRF) is gradually becoming an established technique for the non-invasive analytical investigation of painted surfaces. This paper discusses some of the benefits and limitations of employing MA-XRF for the study of manuscript illuminations. Art historical research on this type of artefacts that is based on scientific measurements is often limited by the fact that usually no sampling can take place. Hence there is a need for non-invasive analytical tools that make it possible to conduct systematic investigations. As a representative example of this type of objects, a 15th century Italian manuscript fragment from the collection of the Fitzwilliam Museum in Cambridge (UK) is investigated. The aims of the study were to gain insight into the materials and techniques employed by Renaissance illuminators and to help answer specific questions regarding the fragment's authorship and geographic origin. The complementarity and advantages of MA-XRF mapping versus site-specific analyses are discussed. For this purpose, MA-XRF data are evaluated and compared with the results of other analytical techniques. The interpretation of the elemental maps is discussed along with the challenges faced during the analysis. (C) 2015 Elsevier B.V. All rights reserved.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.034
Times cited: 24
DOI: 10.1016/J.MICROC.2015.10.020
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“Non-invasive analysis of a 15th century illuminated manuscript fragment: point-based vs imaging spectroscopy”. Legrand S, Ricciardi P, Nodari L, Janssens K, Microchemical journal 138, 162 (2018). http://doi.org/10.1016/J.MICROC.2018.01.001
Abstract: Illuminated manuscript fragments are some of the best preserved objects of Western cultural heritage. Therefore, scholars are limited to non-invasive – often point-based – methods, to answer questions on material usage, technique, origin and previous treatments. These powerful methods yield specific information; however, the information is limited to the number of points analyzed. Imaging spectroscopies such as MA-XRF and MA-rFTIR combine specificity with the power of imaging, resulting in distribution images that are interpretable by non-spectroscopists and the public at large. In this paper the possible added value of using imaging spectroscopy is discussed. Do these methods yield the same results as an extensive point-based spectroscopic campaign and can they bring novel information? As a case study, a 15th century illuminated manuscript fragment is employed in order to explore the differences between these approaches and present an inventory of their advantages and limitations. (C) 2018 Elsevier B.V. All rights reserved.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.034
Times cited: 12
DOI: 10.1016/J.MICROC.2018.01.001
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“Optimization of sample clean-up for the GC-C-IRMS and GC-IT-MS analysis of PAHs from air particulate matter”. Buczyńska AJ, Geypens B, Van Grieken R, De Wael K, Microchemical journal 119, 83 (2015). http://doi.org/10.1016/J.MICROC.2014.10.009
Abstract: The optimization of sample clean-up for the analysis of air particulate matter PAHs stable carbon isotope ratio using Solid Phase Extraction (SPE) cartridges is described in this paper. Various adsorbents, such as silica gel, alumina, florisil, commercially available for sample purification were compared. Best performance for the clean-up of 24-h air particulate matter samples was obtained with activated silica-gel columns in terms of selectivity and reproducibility. One step clean-up was optimized for concentration determination and in case of co-elutions, a second step was additionally used for carbon isotope ratio analysis. The method was subsequently validated with standard reference material and was checked for carbon isotope fractionation artefacts. No significant differences in δ13C values were found for unprocessed solutions of PAHs and solution subjected to the extraction and purification procedure. The procedure was tested on air particulate matter samples collected in three different locations in Belgium. Statistically significant differences in carbon isotope ratio of PAHs between Borgerhout location and Zelzate or Gent were noticed, confirming the differences in distribution and diagnostic ratios found during the concentration analyses and different PAH sources in these locations. The results, therefore, seem very promising for the use of δ13C of PAHs as an additional information helpful in source identification of these pollutants
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.034
Times cited: 7
DOI: 10.1016/J.MICROC.2014.10.009
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“Protecting and stimulating effect on the degradation of eosin lakes. Part 1 : lead white and cobalt blue”. Alvarez-Martin A, Janssens K, Microchemical journal 141, 51 (2018). http://doi.org/10.1016/J.MICROC.2018.05.005
Abstract: An important problem encountered during the preservation of paintings and other artworks is the fading of the original colors due to exposure of the colorants to light. This fact is clearly evidenced in some of Vincent Van Gogh's paintings in which an organic red, eosin or geranium lake, is present. The identification of eosin and the characterization of its degradation products in paintings represents a challenge because of (i) the generally low concentration of the pigment remaining after an aging period of ca 100 years, (ii) the scarcity of the paint micro samples available for analysis and the difficulty of obtaining additional ones and (iii) the complexity of the degradation behavior of eosin when it is mixed with organic or inorganic pigments, binding media or varnish. This study presents an accelerated aging experiment of eosin paint models in order to understand better the discoloration process; more specifically the influence of different metals with which eosin forms complexes and of the presence of admixture pigments such as lead white and cobalt blue on the lightfastness of eosin is evaluated. Paint model samples were prepared using eosin, lead white, and cobalt blue in different mixing ratios and were characterized with several techniques before and after aging. The possible formation of intermediate molecular forms during the aging experiment and the influence of pigment ratios on the discoloration process were monitored at periodic intervals using a combination of LTV Visible and attenuated total Reflectance-Fourier transform infrared (ATR-FTIR) spectroscopies. Raman spectroscopy, scanning electron microscopy coupled to energy-dispersive X-ray analysis (SEM-EDX) and optical microscopy (OM) analyses were performed to gain information about the discoloration processes taking place within the paint models. Eosin precipitated on lead, aluminum and potassium/aluminum salts was used. These three lakes showed similar discoloration rates under light exposure. In contrast, the presence and relative abundance of the admixture pigments lead white and cobalt blue had a significant influence on the (speed of the) eosin discoloration process. The presence of lead white and cobalt blue appears to stimulate the eosin degradation. However, the cobalt blue shows less influence in the discoloration process, showing a protective effect during the first stages of the aging. This may be qualitatively explained in terms of the ability of lead white to scatter light towards eosin molecules and the absorption characteristics of cobalt blue in the green range of the electromagnetic spectrum, shielding eosin from incoming light. The color changes observed in the paint reconstructions are similar to discoloration phenomena visible in some Van Gogh paintings and can offer an explanation of the gradual discoloration process that took place over the years. These insights will be helpful to estimate the original hues color used/intended by the artist.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.034
Times cited: 3
DOI: 10.1016/J.MICROC.2018.05.005
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“Rembrandt's 'Saul and David' (c. 1652) : use of multiple types of smalt evidenced by means of non-destructive imaging”. Janssens K, van der Snickt G, Alfeld M, Noble P, van Loon A, Delaney J, Conover D, Zeibel J, Dik J, Microchemical journal 126, 515 (2016). http://doi.org/10.1016/J.MICROC.2016.01.013
Abstract: The painting Saul and David, considered to date from c. 1652 and previously attributed to Rembrandt van Rijn and/or his studio, is a complex work of art that has been recently subjected to intensive investigation and conservation treatment. The goal of the research was to give insight into the painting's physical construction and condition in preparation for conservation treatment. It was also anticipated that analysis would shed light on authenticity questions and Rembrandt's role in the creation of the painting. The painting depicts the Old Testament figures of King Saul and David. At left is Saul, seated, holding a spear and wiping a tear from his eye with a curtain. David kneels before him at the right playing his harp. In the past, the large sections with the life-size figures were cut apart and later reassembled. A third piece of canvas was added to replace a missing piece of canvas above the head of David. As part of the investigation into the authenticity of the curtain area, a number of paint micro samples were examined with LM and SEM-EDX. Given that the earth, smalt and lake pigments used in the painting could not be imaged with traditional imaging techniques, the entire painting was also examined with state of the art non-destructive imaging techniques. Special attention was devoted to the presence of cobalt-containing materials, specifically the blue glass pigment smalt considered characteristic for the late Rembrandt. A combination of quantitative electron microprobe analysis and macroscopic X-ray fluorescence scanning revealed that three types of cobalt-containing materials are present in the painting. The first type is a cobalt drier that was found in the overpaint used to cover up the canvas inset and the joins that were added in the 19th century. The other two Co-containing materials are part of the original paint used by Rembrandt and comprise two varieties of smalt, a K-rich glass pigment that derives its gray-blue color by doping with Co-ions. Smalt paint with a higher Ni content (NiO:CoO ratio of around 1:4) was used to depict the blue stripes in Saul's colorful turban, while smalt with a lower Ni content was employed (NiO:CoO ratio of around 1:5) for the broad expanses of Saul's garments. The presence of two types of smalt not only supports the recent re-attribution of the painting to Rembrandt, but also that the picture was painted in two phases. Saul's dark red garment is painted in a rough, “loose” manner and the now discolored smalt-rich layer was found to have been partially removed during a past restoration treatment/s. In contrast, the blue-green smalt in the turban is much better preserved and provides a colorful accent. While the use of different types of smalt in a Rembrandt painting has been previously identified using quantitative EDX analysis of paint cross-sections, to the best of our knowledge this is the first time such a distinction has been observed in a 17th-century painting using non-destructive imaging techniques. In addition to the XRF-based non-invasive elemental mapping, hyperspectral imaging in the visual to near-infrared (VNIR) region was also carried out. (C) 2016 Elsevier B.V. All rights reserved.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.034
Times cited: 18
DOI: 10.1016/J.MICROC.2016.01.013
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“Simplex Volume Maximization (SiVM): a matrix factorization algorithm with non-negative constrains and low computing demands for the interpretation of full spectral X-ray fluorescence imaging data”. Alfeld M, Wahabzada M, Bauckhage C, Kersting K, van der Snickt G, Noble P, Janssens K, Wellenreuther G, Falkenberg G, Microchemical journal 132, 179 (2017). http://doi.org/10.1016/J.MICROC.2017.02.001
Abstract: Technological progress allows for an ever-faster acquisition of hyperspectral data, challenging the users to keep up with interpreting the recorded data. Matrix factorization, the representation of data sets by bases (or loads) and coefficient (or score) images is long used to support the interpretation of complex data sets. We propose in this publication Simplex Volume Maximization (SiVM) for the analysis of X-ray fluorescence (XRF) imaging data sets. SiVM selects archetypical data points that represents the data set and thus provides easily understandable bases, preserves the non-negative character of XRF data sets and has low demands concerning computing resources. We apply SiVM on an XRF data set of Hans Memling's Portrait of a man from the Lespinette family from the collection of the Mauritshuis (The Hague, NL) and discuss capabilities and shortcomings of SiVM. (C) 2017 Elsevier B.V. All rights reserved.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.034
Times cited: 8
DOI: 10.1016/J.MICROC.2017.02.001
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“Urban air pollutants and their micro effects on medieval stained glass windows”. Kontozova-Deutsch V, Deutsch F, Godoi RHM, Van Grieken R, De Wael K, Microchemical journal 99, 508 (2011). http://doi.org/10.1016/J.MICROC.2011.07.003
Abstract: Levels of urban gaseous and particulate pollutants were investigated in the Cathedral of Cologne, Germany in the framework of the EU-project VIDRIO. The purpose of this study was to evaluate the influence of a protective double glazing system on the preservation of ancient stained glass windows by sampling at protected and unprotected windows (indoors, in the interspace and outdoor of the Cathedral). The interspace between the ancient stained glass window and the protective glazing is flushed in the Cathedral by indoor air, hence isolating the historic glass from the outdoor air and exposing it to indoor air on both sides of the glass panels. Concentrations of aggressive gaseous pollutants such as NO2, SO2, O3 and CO2 as well as elemental concentrations of bulk particles and relative abundances of single particles were surveyed at all sampling locations. Elemental concentrations in bulk particulate matter were found to be significantly lower inside the Cathedral in comparison to the outdoor air. This result is advantageous for the stained glass windows. Single particle analysis of the samples from Cologne showed also soil dust and organic particles as well as sulphates and nitrates, from which the latter two compounds are dangerous for the stained glass windows. On the base of the obtained results, it can be concluded that the protective glazing system in the Cathedral of Cologne can be considered as predominantly advantageous from both the gases' point of view (except for NO2-candles burning) and from the particles' point of view.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.034
Times cited: 6
DOI: 10.1016/J.MICROC.2011.07.003
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“Multi-modal approach for the characterization of resin carriers in Daylight Fluorescent Pigments”. Álvarez-Martín A, De Winter S, Nuyts G, Hermans J, Janssens K, van der Snickt G, Microchemical Journal 159, 105340 (2020). http://doi.org/10.1016/J.MICROC.2020.105340
Abstract: Almost seventy years after artists such as Frank Stella (1936), Andy Warhol (1928-1987), James Rosenquist (1933-2017), Herb Aach (1923-1985) and Richard Bowman (1918-2001) started to incorporate Daylight Fluorescent Pigments (DFPs) in their artworks, the extent of the conservation problems that are associated with these pigments has increased progressively. Since their first appearance on the market, their composition has constantly been improved in terms of permanency. However, conservation practices on the artworks that are used in, are complicated by the fact that the composition of DFPs is proprietary and the information provided by the manufactures is limited. To be able to propose adequate conservation strategies for artworks containing DFPs, a thorough understanding of the DFPs composition must be acquired. In contrast with previous research that concentrated on identification of the coloring dye, this paper focuses on the characterization of the resin, used as the carrier for the dye. The proposed approach, involving ATR-FTIR, SPME-GC-MS and XRF analysis, provided additional insights on the organic and inorganic components of the resin. Using this approach, we investigated historical DFPs and new formulations, as well as different series from the main manufacturing companies (DayGlo, Swada, Radiant Color and Kremer) in order to obtain a full characterization of DFPs used by the artists along the years. First, the initial PCA-assisted ATR-FTIR spectroscopy allowed for an efficient classification of the main monomers in the resin polymer. Next, a further distinction was made by mass spectrometry and XRF which were optimized to allow a more specific classification of the resin and for detection of additives. In this paper we show the potential of SPME-GC-MS, never applied for the characterization of artistic materials, at present undervalued for heritage science purposes. We anticipate that this information will be highly relevant in the future stability studies and for defining (preventive) conservation strategies of fluorescent artworks.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Antwerp Cultural Heritage Sciences (ARCHES)
Impact Factor: 4.8
DOI: 10.1016/J.MICROC.2020.105340
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“SPME-GC–MS for the off-gassing analysis of a complex museum object”. Alvarez-Martin A, Kavich G, Microchemical Journal 167, 106276 (2021). http://doi.org/10.1016/J.MICROC.2021.106276
Abstract: The identification of volatile organic compounds (VOCs) emitted by a complex museum object, composed of materials of different nature, has been optimized by solid-phase microextraction coupled to gas chromatography-mass spectrometry (SPME-GC–MS). The performance of two fiber coatings and four sampling times were tested and compared in order to define the best sampling conditions. The method allowed a fair extraction of volatile and semivolatile compounds emitted naturally by the object, without any type of accelerating aging. In addition, on-fiber derivatization was applied to improve the extraction efficiency and reduce the sampling time of harmful carboxylic acids emitted by the object. The results obtained are of prime importance to show the off-gassing activity of a valuable museum object in order to take further decisions related with its storage and display conditions.
Keywords: A1 Journal article; Engineering sciences. Technology; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Antwerp X-ray Imaging and Spectroscopy (AXIS)
Impact Factor: 3.034
DOI: 10.1016/J.MICROC.2021.106276
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“Electrochemical deposition of a copper carboxylate layer on copper as potential corrosion inhibitor”. Elia A, De Wael K, Dowsett M, Adriaens A, Journal of solid state electrochemistry 16, 143 (2011). http://doi.org/10.1007/S10008-010-1283-6
Abstract: Carboxylic acids and sodium carboxylates are used to protect metals against aqueous and atmospheric corrosion. In this paper, we describe the application of a layer of copper carboxylate on the surface of a copper electrode by means of cyclic voltammetry technique and tests which measure the corresponding resistance to aqueous corrosion. Unlike the soaking process, which also forms a film on the surface, the use of cyclic voltammetry allows one to follow the deposition process of the copper carboxylates onto the electrode. The modified electrodes have been characterised with infrared spectroscopy. In addition, the corrosion resistance of the film has been investigated using polarisation resistance and Tafel plot measurements.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 2.316
Times cited: 8
DOI: 10.1007/S10008-010-1283-6
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“Influence of the deposition method, temperature and deposition time on the corrosion inhibition of lead dodecanoate coatings deposited on lead surfaces”. De Keersmaecker M, De Wael K, Adriaens A, Journal of solid state electrochemistry 17, 1259 (2013). http://doi.org/10.1007/S10008-012-1964-4
Abstract: Electrochemical impedance measurements have been used to investigate the influence of the deposition method, including time and temperature, upon the corrosion inhibition characteristics of lead dodecanoate coatings on lead electrodes. The results were analysed using multivariate statistics and show that, in general, these easily prepared coatings are very protective against corrosion. The temperature proves to be an important parameter for the quality and the corrosion inhibition efficiency of the coating. A comparison between two different electrochemically assisted deposition methods, immersion using a reduction pretreatment and cyclic voltammetry, does not show significant differences. Using the immersion technique at room temperature, the deposition time was tested as the third influencing parameter for the corrosion inhibition efficiency of the deposited lead dodecanoate coatings. A longer deposition time of the lead into the sodium dodecanoate solution provides a layer with a somewhat higher corrosion resistance.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 2.316
Times cited: 4
DOI: 10.1007/S10008-012-1964-4
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“Micro-Raman analysis for the identification of pigments from 19th and 20th century paintings”. Aibéo CL, Goffin S, Schalm O, van der Snickt G, Laquière N, Eyskens P, Janssens K, Journal of Raman spectroscopy 39, 1091 (2008). http://doi.org/10.1002/JRS.1990
Abstract: In this article, results using confocal µ-Raman to analyse the cross-section of paint samples are presented. Results obtained with light microscopy, scanning electron microscopy (SEM) combined with an energy dispersive X-ray analysis (EDX) and micro-X-ray fluorescence (µ-XRF) are mentioned and compared to the ones obtained with confocal (MRS). In some cases, pigment identification was possible only by combining analytical results from different techniques. The samples were drawn from five paintings belonging to the Academy of Fine Arts of Antwerp, which are part of a collection of 34 paintings made by students from the Academy between 1819 and 1920. Since, on the one hand, the painting techniques and materials, especially pigments, used in this period are still not completely known, and on the other hand, this collection constitutes a very important and reliable resource of information, these paintings were chosen for a systematic investigation. They represent the evolution of painting in Belgium over approximately a century.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 2.969
Times cited: 28
DOI: 10.1002/JRS.1990
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“In vitro validation of a mobile Raman-XRF micro-analytical instrument's capabilities on the diagnosis of Byzantine icons”. Andrikopoulos KS, Daniilia S, Roussel B, Janssens K, Journal of Raman spectroscopy 37, 1026 (2006). http://doi.org/10.1002/JRS.1612
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 2.969
Times cited: 53
DOI: 10.1002/JRS.1612
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“Raman study of different crystalline forms of PbCrO4 and PbCr1-xSxO4 solid solutions for the noninvasive identification of chrome yellows in paintings : a focus on works by Vincent van Gogh”. Monico L, Janssens K, Hendriks E, Brunetti BG, Miliani C, Journal of Raman spectroscopy 45, 1034 (2014). http://doi.org/10.1002/JRS.4548
Abstract: Chrome yellows, a class of pigments frequently used by painters of the Impressionism and Post-impressionism period, are known for their different chemical stability; the latter depends on the chemical composition (PbCrO4, PbCr1-xSxO4) and crystalline structure (monoclinic or orthorhombic) of the material. The possibility to distinguish among different forms of this pigment is therefore relevant in order to extend knowledge on the corresponding degradation process that is observed on several original paintings. For this purpose, three paintings conserved at the Van Gogh Museum (Amsterdam) were analyzed using noninvasive Raman spectroscopy, while equivalent investigations employing bench-top instrumentation were performed to obtain information from micro-samples originating from these works of art. In each painting, the chrome yellow was identified either as monoclinic PbCrO4 or in the form of monoclinic PbCr1-xSxO4 (x<0.25) or S-rich orthorhombic PbCr1-xSxO4 (x similar to 0.5). Our ability to make this fairly subtle distinction is based on a Raman study of several oil paint model samples made up of monoclinic and/or orthorhombic crystalline forms of PbCrO4 and PbCr1-xSxO4 (0.1x0.8). These paints were studied using several excitation wavelengths (namely 785.0, 532.0, 514.5, and 488nm). Because of the absence of the resonance Raman effect, which strongly enhances the chromate symmetric stretching band, and the absence of any laser-induced photodecomposition, it is advantageous to acquire data at 785.0nm. The band-shape and the position of the chromate bending modes proved to be more sensitive to the solid solution composition and crystalline structure than the stretching modes and can be used as distinctive spectral markers to discriminate among the different chrome yellow forms that are present. Copyright (c) 2014 John Wiley & Sons, Ltd.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 2.969
Times cited: 34
DOI: 10.1002/JRS.4548
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“Some critical observations about the degradation of glass : the formation of lamellae explained”. Schalm O, Nuyts G, Janssens K, Journal Of Non-Crystalline Solids 569, 120984 (2021). http://doi.org/10.1016/J.JNONCRYSOL.2021.120984
Abstract: This study demonstrates that the mechanism responsible for the transformation of glass into a degradation layer is pH-dependent. In acid conditions, the transformed glass is homogeneous and brittle. In mild alkaline conditions, transformed glass is heterogeneous due to the presence of lamellae composed of silica nanoparticles and the occurrence of Ca-rich inclusions. The fundamental difference between acid and alkaline conditions cannot be explained by the currently accepted degradation mechanism based on ion exchange. To explain this critical observation, we propose a refined degradation mechanism based on existing knowledge that involves several inwardly moving reaction fronts. The fronts responsible for the transformation of the silicate network into amorphous silica are also responsible for the morphology of the transformed glass. We have identified the feedback mechanism that explains the formation of lamellae in alkaline conditions.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 2.124
DOI: 10.1016/J.JNONCRYSOL.2021.120984
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“Boosting biomolecular interactions through DNA origami nano-tailored biosensing interfaces”. Rutten I, Daems D, Lammertyn J, Journal Of Materials Chemistry B 8, 3606 (2020). http://doi.org/10.1039/C9TB02439E
Abstract: The interaction between a bioreceptor and its target is key in developing sensitive, specific and robust diagnostic devices. Suboptimal interbioreceptor distances and bioreceptor orientation on the sensor surface, resulting from uncontrolled deposition, impede biomolecular interactions and lead to a decreased biosensor performance. In this work, we studied and implemented a 3D DNA origami design, for the first time comprised of assay specifically tailored anchoring points for the nanostructuring of the bioreceptor layer on the surface of disc-shaped microparticles in the continuous microfluidic environment of the innovative EvalutionTM platform. This bioreceptor immobilization strategy resulted in the formation of a less densely packed surface with reduced steric hindrance and favoured upward orientation. This increased bioreceptor accessibility led to a 4-fold enhanced binding kinetics and a 6-fold increase in binding efficiency compared to a directly immobilized non-DNA origami reference system. Moreover, the DNA origami nanotailored biosensing concept outperformed traditional aptamer coupling with respect to limit of detection (11 × improved) and signal-to-noise ratio (2.5 × improved) in an aptamer-based sandwich bioassay. In conclusion, our results highlight the potential of these DNA origami nanotailored surfaces to improve biomolecular interactions at the sensing surface, thereby increasing the overall performance of biosensing devices. The combination of the intrinsic advantages of DNA origami together with a smart design enables bottom-up nanoscale engineering of the sensor surface, leading towards the next generation of improved diagnostic sensing devices.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 7
Times cited: 2
DOI: 10.1039/C9TB02439E
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“Controlled formation of amine-templated mesostructured zirconia with remarkably high thermal stability”. Cassiers K, Linssen T, Aerts K, Cool P, Lebedev O, Van Tendeloo G, van Grieken R, Vansant EF, Journal of materials chemistry 13, 3033 (2003). http://doi.org/10.1039/b310200a
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT); Laboratory of adsorption and catalysis (LADCA); AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 26
DOI: 10.1039/b310200a
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“Antarctic fish versus human cytoglobins : the same but yet so different”. Cuypers B, Vermeylen S, Hammerschmid D, Trashin S, Rahemi V, Konijnenberg A, De Schutter A, Cheng C-HC, Giordano D, Verde C, De Wael K, Sobott F, Dewilde S, Van Doorslaer S, Journal of inorganic biochemistry 173, 66 (2017). http://doi.org/10.1016/J.JINORGBIO.2017.04.025
Abstract: The cytoglobins of the Antarctic fish Chaenocephalus aceratus and Dissostichus mawsoni have many features in common with human cytoglobin. These cytoglobins are heme proteins in which the ferric and ferrous forms have a characteristic hexacoordination of the heme iron, i.e. axial ligation of two endogenous histidine residues, as confirmed by electron paramagnetic resonance, resonance Raman and optical absorption spectroscopy. The combined spectroscopic analysis revealed only small variations in the heme-pocket structure, in line with the small variations observed for the redox potential. Nevertheless, some striking differences were also discovered. Resonance Raman spectroscopy showed that the stabilization of an exogenous heme ligand, such as CO, occurs differently in human cytoglobin in comparison with Antarctic fish cytoglobins. Furthermore, while it has been extensively reported that human cytoglobin is essentially monomeric and can form an intramolecular disulfide bridge that can influence the ligand binding kinetics, 3D modeling of the Antarctic fish cytoglobins indicates that the cysteine residues are too far apart to form such an intramolecular bridge. Moreover, gel filtration and mass spectrometry reveal the occurrence of non-covalent multimers (up to pentamers) in the Antarctic fish cytoglobins that are formed at low concentrations. Stabilization of these oligomers by disulfide-bridge formation is possible, but not essential. If intermolecular disulfide bridges are formed, they influence the heme-pocket structure, as is shown by EPR measurements.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.348
Times cited: 7
DOI: 10.1016/J.JINORGBIO.2017.04.025
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“Electrochemical reduction of nalidixic acid at glassy carbon electrodemodified with multi-walled carbon nanotubes”. Patiño Y, Pilehvar S, Díaz E, Ordóñez S, De Wael K, Journal of hazardous materials 323, 621 (2017). http://doi.org/10.1016/J.JHAZMAT.2016.10.023
Abstract: The aqueous phase electrochemical degradation of nalidixic acid (NAL) is studied in this work, using cyclic voltammetry (CV) and differential pulse voltammetry (DPV) as instrumental techniques. The promotional effect of multi-walled carbon nanotubes (MWCNT) on the the performance of glassy carbon electrodes is demonstrated, being observed that these materials catalyze the NAL reduction. The effect of surface functional groups on MWCNT −MWCNT-COOH and MWCNT-NH2was also studied. The modification of glassy carbon electrode (GCE) with MWCNT leads to an improved performance for NAL reduction following the order of MWCNT > MWCNT-NH2 > MWCNT-COOH. The best behavior at MWCNT-GCE is mainly due to both the increased electrode active area and the enhanced MWCNT adsorption properties. The NAL degradation was carried out under optimal conditions (pH = 5.0, deposition time = 20 s and volume of MWCNT = 10 μL) using MWCNT-GCE obtaining an irreversible reduction of NAL to less toxic products. Paramaters as the number of DPV cycles and the volume/area (V/A) ratio were optimized for maximize pollutant degradation. It was observed that after 15 DPV scans and V/A = 8, a complete reduction was obtained, obtaining two sub-products identified by liquid chromatography-mass spectrometry (LCMS).
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 6.065
Times cited: 4
DOI: 10.1016/J.JHAZMAT.2016.10.023
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“Insight to ternary complexes of co-adsorption of norfloxacin and Cu(II) onto montmorillonite at different pH using EXAFS”. Pei Z-G, Shan X-Q, Zhang S-Z, Kong J-J, Wen B, Zhang J, Zheng L-R, Xie Y-N, Janssens K, Journal of hazardous materials 186, 842 (2011). http://doi.org/10.1016/J.JHAZMAT.2010.11.076
Abstract: Co-adsorption of norfloxacin (Nor) and Cu(II) on montmorillonite at pH 4.5, 7.0 and 9.0 was studied by integrated batch adsorption experiments and extended X-ray absorption fine structure (EXAFS) spectroscopy. Under such pH conditions the dominant species of Nor are cation (Nor+), zwitterion (Nor±), and anion (Nor−), respectively. Results indicated that Nor sorption decreased with an increase of solution pH. The presence of Cu(II) slightly suppressed the Nor+ sorption at pH 4.5, while increased Nor± and Nor−sorption on montmorillonite at pH 7.0 and 9.0, respectively. In contrast, Nor increased Cu(II) adsorption at pH 4.5, but had little effect on the adsorption of Cu(II) on montmorillonite at pH 7.0 and 9.0. Spectroscopic results showed that, at pH 4.5, Nor+ was sorbed on montmorillonite by the formation of outer-sphere montmorilloniteNorCu(II) ternary surface complex. At pH 7.0, montmorilloniteNorCu(II) and montmorilloniteCu(II)Nor ternary surface complexes co-exist. At pH 9.0, montmorilloniteCu(II)Nor ternary surface complex was likely formed, which was different to Cu(II)(Nor)2 precipitate of the solution.
Keywords: A1 Journal article; Engineering sciences. Technology; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 6.065
Times cited: 25
DOI: 10.1016/J.JHAZMAT.2010.11.076
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“Trace-elemental anomalies in surface water near a small lead-zinc mineralization at Menez-Albot (Brittany, France)”. Vandelannoote R, Blommaert W, Sadurski A, Van 'T Dack L, Gijbels R, Van Grieken R, Bosch B, Leleu M, Rochon J, Sarcia C, Sureau JF;, Journal of geochemical exploration 20, 33 (1984). http://doi.org/10.1016/0375-6742(84)90088-8
Abstract: Sensitive multi-element analysis techniques were applied to water samples collected in the vicinity of a small Zn-Pb-Cu sulfide mineralization in the region of Menez-Albot (Finistère, France). The variation of the trace-element content along a local stream shows the presence of the mineralization, mainly through a simultaneous positive anomaly in solution for a group of about 10 elements (e.g. Ni, Cu, Zn, As, Sb) which are connected with this type of mineralization. The anomaly decreases steeply due to the influx of swamp water rich in Fe, Mn and organic matter. The precipitation barrier is reflected in the stream sediment composition. Contamination from fertilizers was observed in some samples.
Keywords: A1 Journal article; Plasma Lab for Applications in Sustainability and Medicine – Antwerp (PLASMANT); AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 2.747
Times cited: 4
DOI: 10.1016/0375-6742(84)90088-8
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“Characterization of uranium and plutonium containing particles originating from the nuclear weapons accident in Thule, Greenland, 1968”. Lind OC, Salbu B, Janssens K, Proost K, Dahlgaard H, Journal of environmental radioactivity 81, 21 (2005). http://doi.org/10.1016/J.JENVRAD.2004.10.013
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 2.31
Times cited: 37
DOI: 10.1016/J.JENVRAD.2004.10.013
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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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“Oxidation states of uranium in depleted uranium particles from Kuwait”. Salbu B, Janssens K, Lind OC, Proost K, Gijsels L, Danesi PR, Journal of environmental radioactivity 78, 125 (2004). http://doi.org/10.1016/J.JENVAD.2004.04.001
Abstract: The oxidation states of uranium in depleted uranium (DU) particles were determined by synchrotron radiation based mu-XANES, applied to individual particles isolated from selected samples collected at different sites in Kuwait. Based on scanning electron microscopy with X-ray microanalysis prior to mu-XANES, DU particles ranging from sub-microns to several hundred micrometers were observed. The.median particle size depended on sources and sampling sites; small-sized particles (median 13 mum) were identified in swipes taken from the inside of DU penetrators holes in tanks and in sandy soil collected below DU penetrators, while larger particles (median 44 mum) were associated with fire in a DU ammunition storage facility. Furthermore, the U-236/U-235 ratios obtained from accelerator mass spectrometry demonstrated that uranium in the DU particles originated from reprocessed fuel (about 10(-2) in DU from the ammunition facility, about 10(-3) for DU in swipes). Compared to well-defined standards, all investigated DU particles were oxidized. Uranium particles collected from swipes were characterized as UO2, U3O8 or a mixture of these oxidized forms, similar to that observed in DU affected areas in Kosovo. Uranium particles formed during fire in the DU ammunition facility were, however, present as oxidation state +5 and +6, with XANES spectra similar to solid uranyl standards. Environmental or health impact assessments for areas affected by DU munitions should therefore take into account the presence of respiratory UO2, U3O8 and even UO3 particles, their corresponding weathering rates and the subsequent mobilisation of U from oxidized DU particles. (C) 2004 Elsevier Ltd. All rights reserved.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 2.31
DOI: 10.1016/J.JENVAD.2004.04.001
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“Oxidation states of uranium in DU particles from Kosovo”. Salbu B, Janssens K, Lind OC, Proost K, Danesi PR, Journal of environmental radioactivity 64, 167 (2003). http://doi.org/10.1016/S0265-931X(02)00047-4
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 2.31
DOI: 10.1016/S0265-931X(02)00047-4
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