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“Les conclusions du programme européen Vidrio sur la protection des vitraux par verrière extérieure”. Pallot-Frossard I, Van Grieken R, Godoi R, Kontozova V, et al, Monumental: revue scientifique et technique , 113 (2007)
Keywords: A3 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“Transport and deposition of airborne pollutants in exhibition areas located in historical buildings: study in Wawel Castle Museum in Cracow, Poland”. Worobiec A, Samek J, Krata A, van Meel K, Krupińska B, Stefaniak EA, Karaszkiewicz P, Van Grieken R, Journal of cultural heritage 11, 354 (2010). http://doi.org/10.1016/J.CULHER.2009.11.009
Abstract: Historical buildings and castles that have been turned nowadays into museums, as an exhibition area for precious cultural heritage (CH) items, need more attention since they are CH objects by themselves. Moreover, the preservation techniques require often, significant interventions; however such changes are not always possible or are very limited. The aim of the present study was to investigate the influence of outdoor air pollution on the composition of particulate matter and gases inside the museum of Wawel Castle in Cracow, Poland. During this study a combination of micro and trace analysis techniques were applied, including energy dispersive X-ray fluorescence (EDXRF) and electron probe microanalysis (EPMA). An intensive transport of air pollutants coupled with accumulation of the particles inside the museum was noticed (considerably higher in winter than summer). A high content of carbon and organic matter agglomerated with inorganic particles was determined. Those particles are of special concern because of their adhesive properties and reactivity. It was also noted that the conditions inside the museum favour the reaction of the particles with gaseous pollutants. It was especially the case for nitrate particles.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Laboratory Experimental Medicine and Pediatrics (LEMP)
DOI: 10.1016/J.CULHER.2009.11.009
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“Investigation of inclusions trapped inside Libyan desert glass by Raman microscopy”. Swaenen M, Stefaniak EA, Frost R, Worobiec A, Van Grieken R, Analytical and bioanalytical chemistry 397, 2659 (2010). http://doi.org/10.1007/S00216-009-3351-2
Abstract: Several specimens of Libyan desert glass (LDG), an enigmatic natural glass from Egypt, were subjected to investigation by micro-Raman spectroscopy. The spectra of inclusions inside the LDG samples were successfully measured through the layers of glass and the mineral species were identified on this basis. The presence of cristobalite as typical for high-temperature melt products was confirmed, together with co-existing quartz. TiO2 was determined in two polymorphic species rutile and anatase. Micro-Raman spectroscopy proved also the presence of minerals unusual for high-temperature glasses such as anhydrite and aragonite.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Laboratory Experimental Medicine and Pediatrics (LEMP)
DOI: 10.1007/S00216-009-3351-2
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“A brief history of 50 years of ICXOM”. Janssens K, , 1 (2010)
Abstract: The ICXOM series of meetings began in 1956 and for over 50 years have been conferences devoted to the topic of “X-ray microanalysis”, both for those interested in developing instrumentation and methods of analysis and for scientists mainly interested in using X-ray micro-analysers for investigations of an applied nature. This contribution surveys the ICXOM series origins, its development and trends over the years.
Keywords: P1 Proceeding; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“Micro X-ray diffraction and fluorescence tomography for the study of multilayered automotive paints”. de Nolf W, Janssens K, Surface and interface analysis 42, 411 (2010). http://doi.org/10.1002/SIA.3125
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.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 1.132
Times cited: 70
DOI: 10.1002/SIA.3125
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“Heavy metal analysis around Iskenderun Bay in Turkey”. Čevik U, Koz B, Makarovska Y, X-ray spectrometry 39, 202 (2010). http://doi.org/10.1002/XRS.1250
Abstract: The heavy metal analysis around Iskenderun Bay in Turkey was carried out using mosses, soils, mussels, and sediments. This region is one of the most industrial areas of Turkey, including iron-steel plants, beverage, liquefied petroleum gas (LPG) plants, and oil transfer docks. Energy dispersive X-ray fluorescence spectrometry (Epsilon 5, PANalytical, Almelo, The Netherlands) was used to analyze all samples. V, Cr, Mn, Fe, Ni, Cu, Zn, As, and Pb elements were observed in all samples studied. Although Ce was detected in some mosses and soils, Sn was detected only in some moss samples. Pb concentrations in the moss samples are higher than the soil, the mussel, and the sediment samples. This can be attributed to the mosses that absorb heavy metals such as Pb easily from the air. As the aim of this study was to analyze heavy metals, the evaluation of these elements with their potential hazards for ecology and humans is briefly discussed
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1002/XRS.1250
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“Preconcentration methods for the analysis of liquid samples by X-ray fluorescence techniques”. Marguí, E, Van Grieken R, Fontàs C, Hidalgo M, Queralt I, Applied spectroscopy reviews 45, 179 (2010). http://doi.org/10.1080/05704920903584198
Abstract: This article gives an overview of the state-of-the-art of multi-element and single-element preconcentration procedures prior to X-ray fluorescence (XRF) analysis of liquid samples. Many of these preconcentration methods were developed long ago and the purpose of this review is to present some new efficient variations of these methods and new techniques extending the possibilities of XRF for liquid solutions analysis. In addition, trends and future perspectives in this domain are also commented on and discussed in the last section of the review.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1080/05704920903584198
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“Elemental concentrations in aerosols at the Belgian coast versus seasons and air mass trajectories”. van Meel K, Horemans B, Krata A, Bencs L, Buczyńska AJ, Dirtu AC, Worobiec A, Van Grieken R, Environmental chemistry letters 8, 157 (2010). http://doi.org/10.1007/S10311-009-0203-4
Abstract: Marine aerosols have extensively been monitored in the framework of a research project to investigate the inorganic and organic nutrient fluxes of the atmospheric nitrogen input into the North Sea. As a part of this project bulk analysis was also performed by energy dispersive X-ray fluorescence (EDXRF) on a total of 366 samples in order to provide detailed elemental composition. Samples have been clustered per campaign and differences were related to backward trajectories. Elements as Cl, Si, and S appeared to be the best tracers for coastal aerosols. Therefore they have been chosen to represent each campaign and to map the seasonal variations. It is clear that Cl is an excellent tracer for oceanic trajectories, while a less clear correlation between the soil dust components and the air mass trajectories is found.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Laboratory Experimental Medicine and Pediatrics (LEMP); Toxicological Centre
DOI: 10.1007/S10311-009-0203-4
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“Chemical analysis of 16th to 19th century Limoges School painted enamel objects in three museums of the Low Countries”. van der Linden V, Schalm O, Houbraken J, Thomas M, Meesdom E, Devos A, van Dooren R, Nieuwdorp H, Janssen E, Janssens K, X-ray spectrometry 39, 112 (2010). http://doi.org/10.1002/XRS.1207
Abstract: In this study, the results of analysing of a series of 16th-19th century painted enamel objects of the Limoges School currently in collections in three Dutch and Flemish museums by means of portable and micro x-ray fluorescence analysis (PXRF and µ-XRF) and electron probe micro analysis (EPMA) are presented. The aim of the investigation was the authentication of specific pieces. Therefore, the glass compositions as well as the (glass) colouring agents used by the Limoges' artists were studied as a function of the age of the objects. Due to the evolution of these properties, it is possible to approximately date these objects based on their chemical composition. The complete émail peint collection of the Museum Boijmans-Van Beuningen (Rotterdam, The Netherlands), consisting of 20 émail peint plaques, was analysed with µ-XRF. Quantitative information was obtained by EPMA analysis of 15 enamel fragments of objects from museum and private collections in the Low Countries. PXRF analyses were performed on the painted enamel collection of the Antwerp Vleeshuis Museum (13 objects) and the Mayer van den Bergh Museum (4 objects) and on a set of 18 plaques that were donated to the Boijmans-Van Beuningen Museum by a private collector. The results obtained by means of EPMA, µ-XRF and PXRF proved to be useful in the discrimination of 16th century painted enamel objects from those of the19th century. From a total of 70 objects examined, 2 objects (OM964A and OM993) featured a chemical signature that deviated from the published literature composition and pigment use consistent with its presumed period of manufacture.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 1.298
Times cited: 8
DOI: 10.1002/XRS.1207
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“James Ensor's pigment use: artistic and material evolution studied by means of portable X-ray fluorescence spectrometry”. van der Snickt G, Janssens K, Schalm O, Aibéo C, Kloust H, Alfeld M, X-ray spectrometry 39, 103 (2010). http://doi.org/10.1002/XRS.1235
Abstract: In this paper, portable X-ray fluorescence spectrometry (PXRF) was employed as a screening tool for determining and comparing the pigment use in a large series of paintings by the Belgian artist James Ensor (1860-1949). Benefits and drawbacks of PXRF as a method, and the instrument employed, are discussed from a practical, conservation and instrumental perspective. Regardless of several restrictions due to the set-up and/or the analytical method, it appeared feasible to document the evolution with time in Ensor's use of inorganic pigments and to correlate this technical evolution with stylistic developments, Nevertheless, it became clear that a full identification of all materials present can only be done by means of the analysis of (cross-sectioned) samples.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 1.298
Times cited: 25
DOI: 10.1002/XRS.1235
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“The use of full-field XRF for simultaneous elemental mapping”. Alfeld M, Janssens K, Sasov A, Liu X, Kostenko A, Rickers-Appel K, Falkenberg G, , 111 (2010). http://doi.org/10.1063/1.3399236
Abstract: The characteristics of a Full-Field X-ray Fluorescence (FF-XRF) set-up for element-specific imaging, installed at the HASYLAB synchrotron radiation source, were determined. A lateral resolution of 10 μm and limits of detection in the percentage range were found. Further potential developments in CCDs available for FF-XRF are discussed and the use of polycapillary lenses as image transfer optics is illustrated in some explorative experiments.
Keywords: P1 Proceeding; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 8
DOI: 10.1063/1.3399236
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“Argentinean prehistoric pigments' study by combined SEM/EDX and molecular spectroscopy”. Darchuk L, Tsybrii Z, Worobiec A, Vázquez C, Palacios OM, Stefaniak EA, Gatto Rotondo G, Sizov F, Van Grieken R, Spectrochimica acta: part A: molecular and biomolecular spectroscopy 75, 1398 (2010). http://doi.org/10.1016/J.SAA.2010.01.006
Abstract: Composition of the prehistoric pigments (from Carriqueo rock shelter, Rio Negro province, Argentina) has been analysed by means of molecular spectroscopy (Fourier transform infrared (FTIR) and micro-Raman) and scanning electron microscopy (SEM) coupled to an energy-dispersive X-ray spectrometer (EDS). Red and yellow pigments were recognized as red and yellow ochre. The matrix of the pigments is composed of one or more substances. According to the matrix composition yellow and red pigments were also divided into two groupsi.e. those containing kaolinite or sulphates. Green pigment was detected as green earth, made up of celadonite as a chromophore.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Laboratory Experimental Medicine and Pediatrics (LEMP)
DOI: 10.1016/J.SAA.2010.01.006
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“X ray fluorescence in member states: Belgium: integration of analysis techniques of different scales using X ray induced and electron induced X ray spectrometry for applications in preventive conservation and environmental monitoring”. Van Grieken R, Potgieter-Vermaak S, Darchuk L, Worobiec A, XRF newsletter , 9 (2009)
Keywords: A3 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Laboratory Experimental Medicine and Pediatrics (LEMP)
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“X-ray fluorescence analysis, sample preparation for”. Margu'i' E, Queralt I, Van Grieken R page 1 (2009).
Keywords: H1 Book chapter; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“Speciation and diurnal variation of thoracic, fine thoracic and sub-micrometer airborne particulate matter at naturally ventilated office environments”. Horemans B, Van Grieken R, Atmospheric environment : an international journal 44, 1497 (2010). http://doi.org/10.1016/J.ATMOSENV.2010.01.010
Abstract: Thoracic (PM10), fine thoracic (PM2.5) and sub-micrometer (PM1) airborne particulate matter was sampled during day and night. In total, about 100 indoor and outdoor samples were collected for each fraction at ten different office environments. Energy-dispersive X-ray fluorescence spectrometry and ion chromatography were applied for the quantification of some major and minor elements and ions in the collected aerosols. During daytime, mass concentrations were in the ranges: 1129, 8.124, and 6.618 μg m−3, with averages of 20 ± 1, 15.0 ± 0.9, and 11.0 ± 0.8 μg m−3, respectively. At night, mass concentrations were found to be significantly lower for all fractions. Indoor PM1 concentrations exceeded the corresponding outdoor levels during office hours and were thought to be elevated by office printers. Particles with diameters between 1 and 2.5 μm and 2.5 and 10 μm were mainly associated with soil dust elements and were clearly subjected to distinct periods of settling/resuspension. Indoor NO3 − levels were found to follow specific microclimatic conditions at the office environments, while daytime levels of sub-micrometer Cl− were possibly elevated by the use of Cl-containing cleaning products. Indoor carbon black concentrations were sometimes as high as 22 μg m−3 and were strongly correlated with outdoor traffic conditions.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1016/J.ATMOSENV.2010.01.010
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Chou L, Harlay J, Roevros N, Lannuzel D, Rebreanu L, van der Zee C, Lapernat P-E, Daro M-H, Aerts K, Godoi R, Van Grieken R (2009) Role of oceanic production and dissolution of calcium carbonate in climate change (CCCC): final report
Keywords: Minutes and reports; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“Inferring episodic atmospheric iron fluxes in the Western South Atlantic”. Evangelista H, Maldonado J, dos Santos EA, Godoi RHM, Garcia CAE, Garcia VMT, Johnson E, da Cunha KD, Leite CB, Van Grieken R, van Meel K, Makarovska Y, Gaiero DM, Atmospheric environment : an international journal 44, 703 (2010). http://doi.org/10.1016/J.ATMOSENV.2009.11.018
Abstract: Iron (Fe) and other trace elements such as Zn, Mn, Ni and Cu are known as key-factors in marine biogeochemical cycles. It is believed that ocean primary productivity blooms in iron deficient regions can be triggered by iron in aeolian dust. Up to now, scarce aerosol elemental composition, based on measurements over sea at the Western South Atlantic (WSA), exist. An association between the Patagonian semi-desert dust/Fe and chlorophyll-a variability at the Argentinean continental shelf is essentially inferred from models. We present here experimental data of Fe enriched aerosols over the WSA between latitudes 22°S62°S, during 4 oceanographic campaigns between 2002 and 2005. These data allowed inferring the atmospheric Fe flux onto different latitudinal bands which varied from 30.4 to 1688 nmolFe m−2 day−1 (October 29thNovember 15th, 2003); 5.831586 nmolFe m−2 day−1 (February 15thMarch 6th, 2004) and 4.73586 nmolFe m−2 day−1(October 21stNovember 5th, 2005).
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1016/J.ATMOSENV.2009.11.018
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“Radiation dose estimation and mass attenuation coefficients of cement samples used in Turkey”. Damla N, Čevik U, Kobya AI, Celik A, Celik N, Van Grieken R, Journal of hazardous materials 176, 644 (2010). http://doi.org/10.1016/J.JHAZMAT.2009.11.080
Abstract: Different cement samples commonly used in building construction in Turkey have been analyzed for natural radioactivity using gamma-ray spectrometry. The mean activity concentrations observed in the cement samples were 52, 40 and 324 Bq kg−1 for 226Ra, 232Th and 40K, respectively. The measured activity concentrations for these radionuclides were compared with the reported data of other countries and world average limits. The radiological hazard parameters such as radium equivalent activities (Raeq), gamma index (Iγ) and alpha index (Iα) indices as well as terrestrial absorbed dose and annual effective dose rate were calculated and compared with the international data. The Raeq values of cement are lower than the limit of 370 Bq kg−1, equivalent to a gamma dose of 1.5 mSv y−1. Moreover, the mass attenuation coefficients were determined experimentally and calculated theoretically using XCOM in some cement samples. Also, chemical compositions analyses of the cement samples were investigated.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1016/J.JHAZMAT.2009.11.080
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“Indoor air quality assessment of elementary schools in Curitiba, Brazil”. Godoi RHM, Avigo D, Campos VD, Tavares TM, de Marchi MRR, Van Grieken R, Godoi AFL, Water, air, and soil pollution : focus 9, 171 (2009). http://doi.org/10.1007/S11267-009-9220-3
Abstract: The promotion of good indoor air quality in schools is of particular public concern for two main reasons: (1) school-age children spend at least 30% of their time inside classrooms and (2) indoor air quality in urban areas is substantially influenced by the outdoor pollutants, exposing tenants to potentially toxic substances. Two schools in Curitiba, Brazil, were selected to characterize the gaseous compounds indoor and outdoor of the classrooms. The concentrations of benzene, toluene, ethylbenzene, and the isomers xylenes (BTEX); NO2; SO2; O3; acetic acid (HAc); and formic acid (HFor) were assessed using passive diffusion tubes. BTEX were analyzed by gas chromatographyion trap mass spectrometry and other collected gasses by ion chromatography. The concentration of NO2 varied between 9.5 and 23 µg m−3, whereas SO2 showed an interval from 0.1 to 4.8 µg m−3. Within the schools, BTEX concentrations were predominant. Formic and acetic acids inside the classrooms revealed intermediate concentrations of 1.5 µg m−3 and 1.2 µg m−3, respectively.
Keywords: A3 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1007/S11267-009-9220-3
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“Determination of BTEX by GCMS in air of offset printing plants: comparison between conventional and ecological inks”. Godoi AFL, Sawada EY, de Marchi MRR, Van Grieken R, Godoi RHM, Water, air, and soil pollution : focus 9, 163 (2009). http://doi.org/10.1007/S11267-009-9219-9
Abstract: The use of inks containing organic solvents by the offset printing process implies in the release of volatile organic compounds to the work environment. Many of these compounds such as benzene, toluene, ethylbenzene, and the xylene isomers (well known by the acronym BTEX) are extremely toxic. In this study, the BTEX concentrations were determined in two different printing plants that use distinct types of inks: the conventional and the so-called ecological, which is manufactured based on vegetal oil. Concentration ranges were 4384, 153,480, 2133, 5459, and 2236 μg m−3 for benzene, toluene, ethylbenzene, m + p-xylene, and o-xylene, respectively, for the conventional printing plant. At the ecological printing plant, concentration ranges were below limit of detection (<LD)-31, <LD-618, <LD-1,690, <LD-10,500, <LD-3,360 μg m−3 for benzene, toluene, ethylbenzene, m + p-xylene, and o-xylene, respectively. BTEX concentrations are lower at the ecological printing environment than in the conventional, where mineral oil-based inks are used. However, the worker who cleans the printing matrices is exposed to high concentrations of ethylbenzene and xylenes, due probably to the cleaning products composition (containing high amounts of BTEX). Although the BTEX concentrations found in both printing work environments were below the limits considered by the Brazilian Law for Activities and Unhealthy Operations (NR-15), the exposure to such vapors characterizes risk to the workers health for some of the evaluated samples, mainly the personal ones.
Keywords: A3 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1007/S11267-009-9219-9
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“Analysis of micro computed tomography images, a look inside historic enamelled metal objects”. van der Linden V, Van de Casteele E, Thomas MS, de Vos A, Janssen E, Janssens K, Applied physics A : materials science &, processing 98, 385 (2010). http://doi.org/10.1007/S00339-009-5394-9
Abstract: In this study the usefulness of micro-Computed Tomography (µ-CT) for the in-depth analysis of enamelled metal objects was tested. Usually investigations of enamelled metal artefacts are restricted to non-destructive surface analysis or analysis of cross sections after destructive sampling. Radiography, a commonly used technique in the field of cultural heritage studies, is limited to providing two-dimensional information about a three-dimensional object (Lang and Middleton, Radiography of Cultural Material, pp. 6061, Elsevier-Butterworth-Heinemann, Amsterdam-Stoneham-London, 2005). Obtaining virtual slices and information about the internal structure of these objects was made possible by CT analysis. With this technique the underlying metal work was studied without removing the decorative enamel layer. Moreover visible defects such as cracks were measured in both width and depth and as of yet invisible defects and weaker areas are visualised. All these features are of great interest to restorers and conservators as they allow a view inside these objects without so much as touching them.
Keywords: A1 Journal article; Vision lab; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 1.455
Times cited: 3
DOI: 10.1007/S00339-009-5394-9
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“Interfaced SEM/EDX and micro-Raman spectrometry for characterisation of heterogeneous environmental particles: fundamental and practical challenges”. Worobiec A, Potgieter-Vermaak S, Brooker A, Darchuk L, Stefaniak E, Van Grieken R, Microchemical journal 94, 65 (2010). http://doi.org/10.1016/J.MICROC.2009.09.003
Abstract: The molecular character of atmospheric particulate matter is of prime importance when interpreting air pollution trends and its subsequent influence on environmental monitoring and preventative conservation. The known methods of estimating the molecular composition normally involve elemental analysis of particles (both as bulk and computer controlled analyses of single particles) with subsequent multivariate analyses to clusterise the elements in groups of elements that are closely related to each other. With this approach one can at best suggest associations. Evidently the application of molecular spectroscopy in addition to elemental concentration profiles would provide intimate information regarding the nature of the particles and consequently their fate. This paper gives an overview of research performed in our laboratory and describes the optimisation of experimental parameters to use scanning electron microscopy with energy-dispersive X-ray detection (SEM/EDX) or electron probe X-ray microanalysis (EPXMA) in parallel with micro-Raman Spectrometry (MRS) to investigate single environmental particles. The challenges associated with the two stand-alone techniques are revealed and consequently those posed with an interfaced approach are discussed. Preliminary results, of an initial investigation of the SEM/EDX interfaced with MRS to ultra-fine heterogeneous environmental particles, are given.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Laboratory Experimental Medicine and Pediatrics (LEMP)
DOI: 10.1016/J.MICROC.2009.09.003
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“Spatially resolved micro-X-ray fluorescence and micro-X-ray absorption fine structure study of a fractured granite bore core following a radiotracer experiment”. Denecke MA, Brendebach B, de Nolf W, Falkenberg G, Janssens K, Simon R, Spectrochimica acta: part B : atomic spectroscopy 64, 791 (2009). http://doi.org/10.1016/J.SAB.2009.05.025
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.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.241
Times cited: 21
DOI: 10.1016/J.SAB.2009.05.025
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“Possibilities and limitations of synchrotron X-ray powder diffraction with double crystal and double multilayer monochromators for microscopic speciation studies”. de Nolf W, Jaroszewicz J, Terzano R, Lind OC, Salbu B, Vekemans B, Janssens K, Falkenberg G, Spectrochimica acta: part B : atomic spectroscopy 64, 775 (2009). http://doi.org/10.1016/J.SAB.2009.06.003
Abstract: The performance of a combined microbeam X-ray fluorescence/X-ray powder diffraction (XRF/XRPD) measurement station at Hamburger Synchrotronstrahlungslabor (HASYLAB) Beamline L is discussed in comparison to that at European Synchrotron Radiation Facility (ESRF) ID18F/ID22. The angular resolution in the X-ray diffractograms is documented when different combinations of X-ray source, optics and X-ray diffraction detectors are employed. Typical angular resolution values in the range 0.30.5° are obtained at the bending magnet source when a pink beam form of excitation is employed. A similar setup at European Synchrotron Radiation Facility beamlines ID18F and ID22 allows to reach angular resolution values of 0.10.15°. In order to document the possibilities and limitations for speciation of metals in environmental materials by means of Hamburger Synchrotronstrahlungslabor Beamline L X-ray fluorescence/X-ray powder diffraction setup, two case studies are discussed, one involved in the identification of the crystal phases in which heavy metals such as chromium, iron, barium and lead are present in polluted soils of an industrial site (Val Basento, Italy) and another involved in the speciation of uranium in depleted uranium particles (Ceja Mountains, Kosovo). In the former case, the angular resolution is sufficient to allow identification of most crystalline phases present while in the latter case, it is necessary to dispose of an angular resolution of ca. 0.2° to distinguish between different forms of oxidized uranium.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.241
Times cited: 7
DOI: 10.1016/J.SAB.2009.06.003
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“Enamels in stained glass windows: preparation, chemical composition, microstructure and causes of deterioration”. Schalm O, van der Linden V, Frederickx P, Luyten S, van der Snickt G, Caen J, Schryvers D, Janssens K, Cornelis E, van Dyck D, Schreiner M, Spectrochimica acta: part B : atomic spectroscopy 64, 812 (2009). http://doi.org/10.1016/j.sab.2009.06.005
Abstract: Stained glass windows incorporating dark blue and purple enamel paint layers are in some cases subject to severe degradation while others from the same period survived the ravages of time. A series of dark blue, greenblue and purple enamel glass paints from the same region (Northwestern Europe) and from the same period (16early 20th centuries) has been studied by means of a combination of microscopic X-ray fluorescence analysis, electron probe micro analysis and transmission electron microscopy with the aim of better understanding the causes of the degradation. The chemical composition of the enamels diverges from the average chemical composition of window glass. Some of the compositions appear to be unstable, for example those with a high concentration of K2O and a low content of CaO and PbO. In other cases, the deterioration of the paint layers was caused by the less than optimal vitrification of the enamel during the firing process. Recipes and chemical compositions indicate that glassmakers of the 1617th century had full control over the color of the enamel glass paints they made. They mainly used three types of coloring agents, based on Co (dark blue), Mn (purple) and Cu (light-blue or greenblue) as coloring elements. Bluepurple enamel paints were obtained by mixing two different coloring agents. The coloring agent for redpurple enamel, introduced during the 19th century, was colloidal gold embedded in grains of lead glass.
Keywords: A1 Journal article; Electron microscopy for materials research (EMAT); AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Vision lab
Impact Factor: 3.241
Times cited: 28
DOI: 10.1016/j.sab.2009.06.005
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“Determination of chemical composition of individual airborne particles by SEM/EDX and micro-Raman spectrometry : a review”. Stefaniak EA, Buczyńska A, Novakovic V, Kuduk R, Van Grieken R, Journal of physics : conference series 162, 012019 (2009). http://doi.org/10.1088/1742-6596/162/1/012019
Abstract: The strategies for sampling and analysis by SEM/EDX and micro-Raman spectrometry for individual airborne particles analysis as applied at the University of Antwerp (Belgium) by the MITAC group have been reviewed. Microbeam techniques provide detailed information concerning the origin, formation, transport, reactivity, transformation reactions and environmental impact of particulate matter. Moreover, some particles of certain chemical properties have been recognized as a threat for human health and cultural heritage objects. However, the small sizes of particles result in specific problems with respect to single particle analysis. Development of equipment and software for improvement of analysis and quantification are reported.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1088/1742-6596/162/1/012019
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“Composition of pigments on human bones found in excavations in Argentina studied with micro-Raman spectrometry and scanning electron microscopy”. Darchuk L, Stefaniak EA, Vázquez C, Palacios OM, Worobiec A, Van Grieken R, e-Preservation Science 6, 112 (2009)
Abstract: Results on analysis of prehistoric pigments from excavations and pigments on coloured child bones from North Patagonia, Argentina, are reported. To analyze their composition we used two micro-analytical techniques: micro- Raman spectrometry (MRS) and scanning electron microscopy coupled with X-ray micro-analysis (SEM/EDX). Most investigated excavated pigments show red or yellow ochres consistent with reddish or yellow minerals, such as á- and ã-goethite, haematite, erdite, haapalaite and jarosite. Raman spectra show also evidence of calcium oxalate monohydrate and calcite indicating lichen activity. Pigments covering human bones were identified as hematite and magnetite. This study allows us to infer that pigments found in excavation were employed for burial ceremonies, even though distances between excavated pigment archaeological site and buried remains are quite far, more than 50 km in a straight line.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Laboratory Experimental Medicine and Pediatrics (LEMP)
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“Tracing the metal pollution history of the Tisza River through the analysis of a sediment depth profile”. Nguyen HL, Braun M, Szaloki I, Baeyens W, Van Grieken R, Leermakers M, Water, air and soil pollution 200, 119 (2009). http://doi.org/10.1007/S11270-008-9898-2
Abstract: The vertical profiles of 20 major and trace metals were investigated along a 180-cm-long sediment core, which was sampled at Kiss-Janosne-Holt Tisza, an oxbow lake located in the upper part of the Tisza River in Hungary. The vertical profiles showed sharp peaks at different depths, reflecting historical pollution events and unusual changes of river water characteristics. Five different groups of metals, containing metals which were strongly correlated and showing a similar behaviour, could be distinguished by factor analysis. Six areas, with variable degrees and types of contamination, were classified in the sediment core with cluster analysis. The most polluted sections were found in the upper 50-cm part (significantly contaminated by Cu, Zn, Pb, Cd and Hg) and the deeper 100120-cm part (characterised by high concentrations of metals associated with mining activities, such as Fe and Mn, as well as Cu, Zn and Pb). In recent years, important pollution events, such as the one which took place in March of 2000, were the reason for pollution of the upper sediment layers, whereas mining activities during the last century were responsible for the pollution of the deeper core sections.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1007/S11270-008-9898-2
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“Characterization of gas concrete materials used in buildings of Turkey”. Damla N, Čevik U, Kobya AI, Celik A, Van Grieken R, Kobya Y, Journal of hazardous materials 168, 681 (2009). http://doi.org/10.1016/J.JHAZMAT.2009.02.092
Abstract: The activity concentration of 226Ra, 232Th and 40K in gas concrete samples collected from different suppliers and some provinces in Turkey were measured using gamma-ray spectrometry. Knowledge of radioactivity in gas concrete used in building materials enables one to assess any possible radiological risks to human health. The mean activity concentrations observed in the gas concrete samples were 82.0, 28.2 and 383.9 Bq kg−1 for 226Ra, 232Th and 40K, respectively. The radium equivalent activity, external and internal hazard indices as well as terrestrial absorbed dose and annual effective dose rate was calculated. The results indicate that the radium equivalent activity values of gas concrete samples are lower than the limit of 370 Bq kg−1, equivalent to a gamma-dose of 1.5 mSv y−1. Moreover, mass attenuation coefficients were measured in some gas concrete samples. It was found that the mass attenuation coefficients decreased with increasing photon energies. Also, chemical compositions and structural analysis (XRD and SEM) of the gas concrete samples were investigated.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1016/J.JHAZMAT.2009.02.092
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“Atmospheric nitrogen fluxes at the Belgian coast: 2004-2006”. Bencs L, Krata A, Horemans B, Buczyńska AJ, Dirtu AC, Godoi AFL, Godoi RHM, Potgieter-Vermaak S, Van Grieken R, Atmospheric environment : an international journal 43, 3786 (2009). http://doi.org/10.1016/J.ATMOSENV.2009.04.002
Abstract: Daily and seasonal variations in dry and wet atmospheric nitrogen fluxes have been studied during four campaigns between 2004 and 2006 at a coastal site of the Southern North Sea at De Haan (Belgium) located at coordinates of 51.1723° N and 3.0369° E. Concentrations of inorganic N-compounds were determined in the gaseous phase, size-segregated aerosol (coarse, medium, and fine), and rainwater samples. Dissolved organic nitrogen (DON) was quantified in rainwater. The daily variations in N-fluxes of compounds were evaluated with air-mass backward trajectories, classified into the main air-masses arriving at the sampling site (i.e., continental, North Sea, and Atlantic/UK/Channel). The three, non-episodic campaigns showed broadly consistent fluxes, but during the late summer campaign exceptionally high episodic N-deposition was observed. The average dry and wet fluxes for non-episodic campaigns amounted to 2.6 and 4.0 mg N m−2 d−1, respectively, whereas during the episodic late summer period these fluxes were as high as 5.2 and 6.2 mg N m−2 d−1, respectively. Non-episodic seasons/campaigns experienced average aerosol fluxes of 0.91.4 mg N m−2 d−1. Generally, the contribution of aerosol NH4+ was more significant in the medium and fine particulate fractions than that of aerosol NO3−, whereas the latter contributed more in the coarse fraction, especially in continental air-masses. During the dry mid-summer campaign, the DON contributed considerably (15%) to the total N-budget. Exceptionally high episodic aerosol-N inputs have been observed for the late summer campaign, with especially high deposition rates of 3.6 and 2.9 mg N m−2 d−1 for Atlantic/UK/Channel and North Sea-continental (mixed) air-masses, respectively. During this pollution episode, the flux of NH4+ was dominating in each aerosol fraction/air-mass, except for coarse continental aerosols. High deposition of gaseous-N was also observed in this campaign with an average total N-flux of 22.5-times higher than in other campaigns.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1016/J.ATMOSENV.2009.04.002
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