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“Comparison of spectroscopic techniques combined with chemometrics for cocaine powder analysis”. Eliaerts J, Meert N, Dardenne P, Baeten V, Pierna J-AF, Van Durme F, De Wael K, Samyn N, Journal Of Analytical Toxicology 44, 851 (2020). http://doi.org/10.1093/JAT/BKAA101
Abstract: Spectroscopic techniques combined with chemometrics are a promising tool for analysis of seized drug powders. In this study, the performance of three spectroscopic techniques [Mid-InfraRed (MIR), Raman and Near-InfraRed (NIR)] was compared. In total, 364 seized powders were analyzed and consisted of 276 cocaine powders (with concentrations ranging from 4 to 99 w%) and 88 powders without cocaine. A classification model (using Support Vector Machines [SVM] discriminant analysis) and a quantification model (using SVM regression) were constructed with each spectral dataset in order to discriminate cocaine powders from other powders and quantify cocaine in powders classified as cocaine positive. The performances of the models were compared with gas chromatography coupled with mass spectrometry (GC-MS) and gas chromatography with flame-ionization detection (GC-FID). Different evaluation criteria were used: number of false negatives (FNs), number of false positives (FPs), accuracy, root mean square error of cross-validation (RMSECV) and determination coefficients (R-2). Ten colored powders were excluded from the classification data set due to fluorescence background observed in Raman spectra. For the classification, the best accuracy (99.7%) was obtained with MIR spectra. With Raman and NIR spectra, the accuracy was 99.5% and 98.9%, respectively. For the quantification, the best results were obtained with NIR spectra. The cocaine content was determined with a RMSECV of 3.79% and a R-2 of 0.97. The performance of MIR and Raman to predict cocaine concentrations was lower than NIR, with RMSECV of 6.76% and 6.79%, respectively and both with a R-2 of 0.90. The three spectroscopic techniques can be applied for both classification and quantification of cocaine, but some differences in performance were detected. The best classification was obtained with MIR spectra. For quantification, however, the RMSECV of MIR and Raman was twice as high in comparison with NIR. Spectroscopic techniques combined with chemometrics can reduce the workload for confirmation analysis (e.g., chromatography based) and therefore save time and resources.
Keywords: A1 Journal article; Pharmacology. Therapy; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 2.5
DOI: 10.1093/JAT/BKAA101
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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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“Matrix effects and analysis of biological material by spark source mass spectrometry”. Vos L, Van Grieken R, Fresenius' Zeitschrift für analytische Chemie 321, 32 (1985). http://doi.org/10.1007/BF00464483
Abstract: Spark-source mass spectrometric analyses of synthetic simulated biological samples were performed to determine the importance of matrix effects. A correlation between the variation of the relative sensitivity coefficients (RSC's) and the spark plasma composition, hence plasma temperature, was found. The determined RSC's were used in the analysis of four biological standard reference materials. An accuracy of 1013% and detection limits between 0.005 and 0.5 ppm were obtained during analysis under normal conditions.
Keywords: A3 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1007/BF00464483
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“Influence of spark generator parameters in the analysis of graphite-electrodes by spark source-mass spectrometry”. Vos L, Van Grieken R, International journal of mass spectrometry and ion processes 55, 233 (1984). http://doi.org/10.1016/0168-1176(84)87087-1
Abstract: Spark source mass spectrometric analyses of doped carbon samples were performed at different pulse lengths, pulse frequencies and breakdown voltages. The pulse length and pulse frequencies had no influence on the analysis. The relation between breakdown voltage, spark gap and sample matrix was determined. With increasing breakdown voltage, the abundance of the multiply charged ions was found to decrease, whereas the abundance of the cluster ions increased. The breakdown voltage was also found to affect the absolute and relative intensities of different elements in different manners. Interpretation of these results led to some new considerations on the phenomena in a spark discharge.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1016/0168-1176(84)87087-1
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“Understanding air-tight case environments at the National Museum of the American Indian (Smithsonian Institution) by SPME-GC-MS analysis”. Alvarez-Martin A, McHugh K, Martin C, Kavich G, Kaczkowski R, Journal Of Cultural Heritage 44, 38 (2020). http://doi.org/10.1016/J.CULHER.2020.01.004
Abstract: Some volatile organic compounds (VOCs), generated and accumulated in exhibition cases, are capable of inducing degradation in historical artifacts. In this context, it is of special importance to distinguish between VOCs emitted by the construction materials and/or the historical objects, with the ultimate goal of proposing an appropriate mitigation strategy. To pursue this goal, a comprehensive analysis based on solid phase microextraction (SPME) coupled to gas chromatography-mass spectrometry (GC-MS) has been optimized. The sampling setup used in this study does not require any modification of the exhibition design, and the testing remained nearly invisible and unobtrusive to museum visitors. This methodology has been applied to an issue encountered at the National Museum of the American Indian (Smithsonian Institution), where an unpleasant smell was detected in airtight exhibition cases already on display containing sensitive historical objects. The analysis of the volatiles emitted by construction materials allowed for identification of characteristic markers emitted by each material, and the ability to identify their overall contribution in the exhibition case. Via this method, SPME-GC-MS confirmed via the detection of some specific markers that the unpleasant smell was released by one of the construction materials and had accumulated in the exhibition case. In addition, due to the measurements taken in different positions around the exhibition cases, results were useful to point out the range of efficiency of the sorbent material placed in some of the exhibition cases as a first attempt of mitigation technique. (C) 2020 Elsevier Masson SAS. All rights reserved.
Keywords: A1 Journal article; Art; History; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.1
DOI: 10.1016/J.CULHER.2020.01.004
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“Gross alpha and beta activities of airborne particulate samples from Wawel Royal Castle Museum in Cracow, Poland”. Akbulut S, Krupinska B, Worobiec A, Čevik U, Taskin H, Van Grieken R, Samek L, Wiłkojć, E, Journal of radioanalytical and nuclear chemistry 295, 1567 (2013). http://doi.org/10.1007/S10967-012-1983-8
Abstract: Soils are complex mixtures of organic, inorganic materials, and metal compounds from anthropogenic sources. In order to identify the pollution sources, their magnitude and development, several X-ray analytical methods were applied in this study. The concentrations of 16 elements were determined in all the soil samples using energy dispersive X-ray fluorescence spectrometry. Soils of unknown origin were observed by scanning electron microscopy equipped with a Si(Li) X-ray detector using Monte Carlo simulation approach. The mineralogical analyses were carried out using X-ray diffraction spectrometry. Due to the correlations between heavy metals and oxide compounds, the samples were analyzed also by electron probe microanalyzer (EPMA) in order to have information about their oxide contents. On the other hand, soil pH and salinity levels were identified owing to their influence between heavy metal and soil-surface chemistry. Moreover, the geoaccumulation index (I geo) enables the assessment of contamination by comparing current and pre-industrial concentrations.
Keywords: A1 Journal article; Engineering sciences. Technology; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Laboratory Experimental Medicine and Pediatrics (LEMP)
DOI: 10.1007/S10967-012-1983-8
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“Identification of heavy metal origins related to chemical and morphological soil properties using several non-destructive X-ray analytical methods”. Akbulut S, Van Grieken R, Kilic MA, Čevik U, Rotondo GG, Environmental monitoring and assessment 185, 2377 (2013). http://doi.org/10.1007/S10661-012-2718-6
Abstract: Soils are complex mixtures of organic, inorganic materials, and metal compounds from anthropogenic sources. In order to identify the pollution sources, their magnitude and development, several X-ray analytical methods were applied in this study. The concentrations of 16 elements were determined in all the soil samples using energy dispersive X-ray fluorescence spectrometry. Soils of unknown origin were observed by scanning electron microscopy equipped with a Si(Li) X-ray detector using Monte Carlo simulation approach. The mineralogical analyses were carried out using X-ray diffraction spectrometry. Due to the correlations between heavy metals and oxide compounds, the samples were analyzed also by electron probe microanalyzer (EPMA) in order to have information about their oxide contents. On the other hand, soil pH and salinity levels were identified owing to their influence between heavy metal and soil-surface chemistry. Moreover, the geoaccumulation index (I geo) enables the assessment of contamination by comparing current and pre-industrial concentrations.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1007/S10661-012-2718-6
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“Recognition of uranium oxides in soil particulate matter by means of ì-Raman spectrometry”. Stefaniak EA, Sajó, I, Alsecz A, Worobiec A, Máthé, Z, Török S, Van Grieken R, Journal of nuclear materials 381, 278 (2008). http://doi.org/10.1016/J.JNUCMAT.2008.08.036
Abstract: Soil samples from an abandoned uranium mine have been investigated in order to determine the molecular phases of uranium compounds. The experiments were carried out with soil particulate matter, collected randomly from the area of the formerly exploited ore. To select the particles rich with uranium, scanning electron microscopy with energy-dispersive X-ray attachment (SEM/EDX) was applied first. Afterwards, the particles were relocated and measured by l-Raman spectrometry (MRS). Residues of the main deposit, uraninite UO2, were detected, along with its alteration products. In terms of Raman scattering properties, uranium oxides are quite sensitive to the laser beam wavelength, which results in very specific features of their Raman spectra. In this paper the Raman spectra of uranium oxides of different origin and oxidation states, measured with 514 and 785 nm lasers, are also presented
Keywords: A1 Journal article; Laboratory Experimental Medicine and Pediatrics (LEMP); AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1016/J.JNUCMAT.2008.08.036
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“SnIV-containing layered double hydroxides as precursors for nano-sized ZnO/SnO2 photocatalysts”. Seftel EM, Popovici E, Mertens M, Stefaniak EA, Van Grieken R, Cool P, Vansant EF, Applied catalysis : B : environmental 84, 699 (2008). http://doi.org/10.1016/J.APCATB.2008.06.006
Abstract: Sn4+-containing LDH was prepared using the co-precipitation method at constant pH, and characterized using X-ray diffraction, UVvis diffuse reflectance spectroscopy and TG/DTG methods. The obtained product was further exposed to different thermal treatments in order to obtain nano-sized coupled ZnO/SnO2 systems with enhanced photocatalytic performances than the ones obtained by mixing the two semiconductor oxides. The formation of a well-defined ZnO/SnO2 system and the crystallite size, fully investigated using XRD, micro-Raman scattering and UVvis DR techniques, were found to be influenced by the nature of the precursors and the calcination temperature. The photocatalytic activity of the ZnO/SnO2 systems, evaluated for the photodegradation of methyl orange (MO) dye, was studied as a function of the initial pH, catalyst loading and the calcination temperature. The metal dispersion supplied by layered structures proved to be an advantage when preparing coupled ZnO/SnO2 systems, the photocatalytic activity being 2.3 times higher comparing with the physical mixtures performances. The maximum photocatalytic activity of the coupled ZnO/SnO2 system having a layered precursor was observed when using neutral pH, at a catalyst loading of 1 g/L calcined at 600 °C for 4 h.
Keywords: A1 Journal article; Laboratory of adsorption and catalysis (LADCA); AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1016/J.APCATB.2008.06.006
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“Effect of operating and sampling conditions on the exhaust gas composition of small-scale power generators”. Smits M, Vanpachtenbeke F, Horemans B, De Wael K, Hauchecorne B, Van Langenhove H, Demeestere K, Lenaerts S, PLoS ONE 7, e32825 (2012). http://doi.org/10.1371/JOURNAL.PONE.0032825
Abstract: Small stationary diesel engines, like in generator sets, have limited emission control measures and are therefore responsible for 44% of the particulate matter (PM) emissions in the United States. The diesel exhaust composition depends on operating conditions of the combustion engine. Furthermore, the measurements are influenced by the used sampling method. This study examines the effect of engine loading and exhaust gas dilution on the composition of small-scale power generators. These generators are used in different operating conditions than road-transport vehicles, resulting in different emission characteristics. Experimental data were obtained for gaseous volatile organic compounds (VOC) and PM mass concentration, elemental composition and nitrate content. The exhaust composition depends on load condition because of its effect on fuel consumption, engine wear and combustion temperature. Higher load conditions result in lower PM concentration and sharper edged particles with larger aerodynamic diameters. A positive correlation with load condition was found for K, Ca, Sr, Mn, Cu, Zn and Pb adsorbed on PM, elements that originate from lubricating oil or engine corrosion. The nitrate concentration decreases at higher load conditions, due to enhanced nitrate dissociation to gaseous NO at higher engine temperatures. Dilution on the other hand decreases PM and nitrate concentration and increases gaseous VOC and adsorbed metal content. In conclusion, these data show that operating and sampling conditions have a major effect on the exhaust gas composition of small-scale diesel generators. Therefore, care must be taken when designing new experiments or comparing literature results.
Keywords: A1 Journal article; Engineering sciences. Technology; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Sustainable Energy, Air and Water Technology (DuEL)
Impact Factor: 2.806
Times cited: 5
DOI: 10.1371/JOURNAL.PONE.0032825
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“Pixe analysis of aerosol samples collected over the atlantic-ocean from a sailboat”. Maenhaut W, Selen A, van Espen P, Van Grieken R, Winchester WJ, Nuclear instruments and methods 181, 399 (1981). http://doi.org/10.1016/0029-554X(81)90640-6
Abstract: Size-fractionated aerosol samples, collected over the Atlantic Ocean, were analyzed for up to 20 elements by PIXE. Using a sailboat as sampling platform, duplicate samples were taken for two-day periods by means of battery operated 6-stage cascade impactors, positioned about 8 m above the sea surface. In the PIXE analysis of the fine particle stages (stages 3 to 5) a 5 times smaller beam size was used than for stages 1 and 2. This led to significant improvement in the detection limits for the former stages. The results from the duplicate impactor samples were normally in good agreement, indicating that the combined uncertainty of sampling and PIXE analysis was of the order of 20%. The precision of the PIXE analysis alone was investigated by rebombarding some samples six months after the first analysis. The trends with time of the fine particle sulfur and the coarse particle iron concentrations are discussed in some detail.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Chemometrics (Mitac 3)
DOI: 10.1016/0029-554X(81)90640-6
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“Heavy metal contamination in sediments from the Belgian coast and Scheldt estuary”. Araújo MFD, Bernard PC, Van Grieken RE, Marine pollution bulletin 19, 269 (1988). http://doi.org/10.1016/0025-326X(88)90597-8
Abstract: Sixty-two samples of total sediments and the separated clay/silt size fractions were analysed by energy-dispersive X-ray fluorescence spectrometry to evaluate the pollution level and the trends in samples collected along the Belgian coast over a period of 6 yr and at four stations located in the Scheldt estuary where two of these were sampled periodically for 4 yr. Three correction methods for grain size effects were applied, either to the bulk sediment samples or to the clay/silt size fractions, and the results were compared. Local variations on the concentrations in some of the elements determined were used to establish whether they result from an anthropogenic or natural origin. The level of pollution was assessed as a function of the location, sampling date, and depth.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1016/0025-326X(88)90597-8
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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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“Characterization of polyvinyl alcohol-borax/agarose (PVA-B/AG) double network hydrogel utilized for the cleaning of works of art”. Al-Emam E, Soenen H, Caen J, Janssens K, Heritage science 8, 106 (2020). http://doi.org/10.1186/S40494-020-00447-3
Abstract: Since cleaning of artworks may cause undesirable physicochemical alterations and is a nonreversible procedure, it is mandatory to adopt the proper cleaning procedure. Such a procedure should remove undesired materials whilst preserving the original surface. In this regard, numerous gels have been developed and exploited for the cleaning of various artwork surfaces. Lately, agarose (AG) and polyvinyl alcohol-borax (PVA-B) hydrogels have been widely employed as cleaning tools by conservators. Both hydrogels show some limitations in specific cleaning practices. In this work, we investigated the influence of including increased levels of agarose into PVA-B systems. For this reason, we performed a detailed characterization on the double network (DN) hydrogel including the chemical structure, the liquid phase retention, the rheological behavior, and the self-healing behavior of various PVA-B/AG double network hydrogels. These new hydrogels revealed better properties than PVA-B hydrogels and obviated their limitations. The inclusion of AG into PVA-B systems enhanced the liquid retention capacity, shape-stability, and mechanical strength of the blend. Furthermore, AG minimized the expelling/syneresis issue that occurs when loading PVA-B systems with low polarity solvents or chelating agents. The resultant double network hydrogel exhibits relevant self-healing properties. The PVA-B/AG double network is a new and useful cleaning tool that can be added to the conservators' tool-kit. It is ideal for cleaning procedures dealing with porous and complex structured surfaces, vertical surfaces and for long time applications.
Keywords: A1 Journal article; Art; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Antwerp Cultural Heritage Sciences (ARCHES)
Impact Factor: 2.5
Times cited: 1
DOI: 10.1186/S40494-020-00447-3
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“The use of microscopic X-ray diffraction for the study of HgS and its degradation products corderoite (\alpha-Hg3S2Cl2), kenhsuite (\gamma-Hg3S2Cl2) and calomel (Hg2Cl2) in historical paintings”. Radepont M, de Nolf W, Janssens K, van der Snickt G, Coquinot Y, Klaassen L, Cotte M, Journal of analytical atomic spectrometry 26, 959 (2011). http://doi.org/10.1039/C0JA00260G
Abstract: Since antiquity, the red pigment mercury sulfide (α-HgS), called cinnabar in its natural form or vermilion red when synthetic, was very often used in frescoes and paintings, even if it was known to suffer occasionally from degradation. The paint hereby acquires a black or silver-grey aspect. The chemical characterization of these alteration products is rather challenging mainly because of the micrometric size and heterogeneity of the surface layers that develop and that are responsible for the color change. Methods such as electron microscopy, synchrotron-based microscopic X-ray fluorescence, microscopic X-ray absorption near edge spectroscopy, Raman microscopy and secondary ion microscopy have been previously employed to identify the (Hg- and S-) compounds present and to study their co-localization. Next to these, also microscopic X-ray diffraction (XRD) (either by making use of laboratory X-ray sources or when used at a synchrotron facility) allows the identification of the crystal phases that are present in degraded HgS paint layers. In this paper we employ these various forms of micro-XRD to analyze degraded red paint in different paintings and compare the results with other X-ray based methods. Whereas the elemental analyses of the degradation products revealed, next to mercury and sulfur, the presence of chlorine, X-ray diffraction allowed the identification, next to α-HgS, of the Hg and S-containing compound calomel (Hg2Cl2) but also of the Hg, S and Cl-containing minerals corderoite (α-Hg3S2Cl2) and kenhsuite (γ-Hg3S2Cl2). These observations are consistent with X-ray absorption spectroscopy measurements performed at the S- and Cl-edges.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.379
Times cited: 40
DOI: 10.1039/C0JA00260G
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“Voltammetric behaviour of drotaverine hydrochloride in surfactant media and its enhancement determination in Tween-20”. Jain R, Vikas, Rather JA, Colloids and surfaces: B : biointerfaces 82, 333 (2011). http://doi.org/10.1016/J.COLSURFB.2010.09.005
Abstract: Simple, sensitive and rapid adsorptive voltammetric behaviour of drotaverine hydrochloride onto the HMDE has been explored and validated in surfactant media by using cyclic, differential pulse and square-wave voltammetry. Addition of Tween-20 to the drotaverine hydrochloride containing electrolyte enhances the reduction current signal. The voltammograms of the drug with Tween-20 in phosphate buffers of pH 2.511.0 exhibit a single well defined reduction peak which may be due to the reduction of Cdouble bond; length as m-dashC group. The cyclic voltammetric studies indicated the reduction of drotaverine hydrochloride at the electrode surface through two electron irreversible step and diffusion-controlled. The peak current showed a linear dependence with the drug concentration over the range 0.87.2 μg mL−1. The calculated LOD and LOQ are 1.8 and 6.0 ng mL−1 by SWCAdSV and 8.1 and 27.2 ng mL−1 by DPCAdSV, respectively. The procedure was applied to the assay of the drug in tablet form with mean percentage recoveries of 100.2% with SWCAdSV and 99.7% with DPCAdSV. The validity of the proposed methods was further assessed by applying a standard addition technique.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1016/J.COLSURFB.2010.09.005
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“EPXMA survey of shelf sediments (Southern Bight, North Sea): a glance beyond the XRD-invisible”. de Maeyer-Worobiec A, Dekov VM, Laane RWPM, Van Grieken R, Microchemical journal 91, 21 (2009). http://doi.org/10.1016/J.MICROC.2008.07.001
Abstract: Shelf sediments of the southern North Sea, were studied with a microanalytical [electron probe X-ray microanalysis (EPXMA)] and two bulk [X-ray diffraction (XRD) and X-ray fluorescence (XRF)] techniques. The investigation proved that the promptness of the microanalytical method is combined with a reasonable analytical reliability. XRD studies of such a type of sediments with monotonous mineral composition are not able to provide mineralogical information beyond the main well-crystalline minerals and the mineralogical quantitative characteristic of the sediment based on XRD estimations are incorrect. The EPXMA mineralogical interpretations are based on the statistical evaluation of a huge data set (thousands of mineral particles) and provide a rather correct quantitative determination of the main minerals. The comparative EPXMAXRF study revealed that the Al, Si, K, Ca, Fe and to some extent Ti contents estimated by EPXMA are fairly reliable. In this respect the accuracy of the EPXMA-based mineral identification of the pure silicates, pure aluminosilicates, and Al-, Ca-, Fe- and Ti-containing minerals with simple composition is very high. Mg-calcite, augite and apatite determinations are assessed to be correct. The supposed accuracy of the clay mineral determinations is slightly lower (7080%) than that of the other main minerals due to the complex and varying composition of the clays. The identification of XRD-invisible accessory minerals and quantification of their presence in the sediments is an essential advantage of the EPXMA, which makes it a useful approach in tracing the origin of the sediments, the pathways of their transport and the geochemical processes they have undergone. However, the EPXMA has several flaws, which need to be solved in the future sediment investigations: (1) calibration with natural standards is needed in order to provide a higher accuracy of the mineral determinations; (2) any EPXMA study of sediments needs to be secured with XRF examinations of selected samples since EPXMA gives only semi-quantitative information about the abundance of the elements; (3) ultra-thin window EPXMA of low-Z elements has to be used since some of them (O, C) are always present in the main sediment components: silicates, aluminosilicates, carbonates and metal oxyhydroxides; (4) the interpretations of the clay fraction have to be supported with detailed XRD investigations of selected samples, while the mineralogy of the silt and sand fractions needs to be backed up with optical microscopy studies. The information from different analytical techniques (EPXMA with XRFXRD-optical microscopy of selected samples) combined with the knowledge about the most possible minerals in a given environment, would give the most reliable results in studying mineralogical composition of shelf sediments.
Keywords: A1 Journal article; Laboratory Experimental Medicine and Pediatrics (LEMP); AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1016/J.MICROC.2008.07.001
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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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“Optimization of a simple spotting procedure for x-ray fluorescence analysis of waters”. Smits J, Van Grieken R, Analytica chimica acta 88, 97 (1977). http://doi.org/10.1016/S0003-2670(01)96053-2
Abstract: Several sample preparation methods for waters for energy-dispersive x.r.f. were examined, as well as the influence of sample size on the analytical characteristics. The most satisfactory simple, rapid method proved to be spotting of 1.5 ml of water sample on a Whatman-41 cellulose filter paper provided with a wax ring of 29-mm diameter and evaporating the water with an unheated air stream from underneath. Sensitivities are below 100 p.p.b. for most elements and often below 50 p.p.b. when the optimal secondary fluorescer is used. Accuracy and precision are usually in the 1520 % range. The method is applicable to many dilute aqueous solutions as is illustrated by analysis of industrial water samples and ashed biological material.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1016/S0003-2670(01)96053-2
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“Improved calculation of displacements per atom cross section in solids by gamma and electron irradiation”. Pinera I, Cruz CM, Leyva A, Abreu Y, Cabal AE, van Espen P, Van Remortel N, Interactions With Materials And Atoms 339, 1 (2014). http://doi.org/10.1016/J.NIMB.2014.08.020
Abstract: Several authors had estimated the displacements per atom cross sections under different approximations and models, including most of the main gamma- and electron-material interaction processes. These previous works used numerical approximation formulas which are applicable for limited energy ranges. We proposed the Monte Carlo assisted Classical Method (MCCM), which relates the established theories about atom displacements to the electron and positron secondary fluence distributions calculated from the Monte Carlo simulation. In this study the MCCM procedure is adapted in order to estimate the displacements per atom cross sections for gamma and electron irradiation. The results obtained through this procedure are compared with previous theoretical calculations. An improvement in about 10-90% for the gamma irradiation induced dpa cross section is observed in our results on regard to the previous evaluations for the studied incident energies. On the other hand, the dpa cross section values produced by irradiation with electrons are improved by our calculations in about 5-50% when compared with the theoretical approximations. When thin samples are irradiated with electrons, more precise results are obtained through the MCCM (in about 20-70%) with respect to the previous studies. (C) 2014 Elsevier B.V. All rights reserved.
Keywords: A1 Journal article; Engineering sciences. Technology; Particle Physics Group; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1016/J.NIMB.2014.08.020
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“Understanding the (in)stability of semiconductor pigments by a thermodynamic approach”. Anaf W, Schalm O, Janssens K, De Wael K, Dyes and pigments 113, 409 (2015). http://doi.org/10.1016/J.DYEPIG.2014.09.015
Abstract: Several artists pigments are semiconductors. Some of these materials appear stable over time, whereas others already show remarkable signs of degradation after limited time periods. The (in)stability of these pigments can be understood using a thermodynamic approach. For several pigment-related materials, the thermodynamic oxidation and reduction potential (ϕox and ϕred) were determined and evaluated considering the absolute energy positions of the valence and conduction band edges and the water redox potentials. The positions of ϕox and ϕred can be used in a fast screening of the stability of semiconductor pigments towards photoinduced corrosion in an aqueous/humid environment. This theoretical approach corresponds well with experimental data on pigment permanence and degradation phenomena found in literature.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation); Antwerp Cultural Heritage Sciences (ARCHES)
Impact Factor: 3.473
Times cited: 14
DOI: 10.1016/J.DYEPIG.2014.09.015
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“Serum bromine levels in psoriasis”. Shani J, Barak S, Ram M, Levi D, Pfeifer Y, Schlesinger T, Avrach WW, Robberecht H, Van Grieken R, Pharmacology 25, 297 (1982). http://doi.org/10.1159/000137756
Abstract: Serum bromine levels in psoriatic Danes increased 2- to 3-fold during a 4-week bathing course in the Dead Sea. This increase correlated well with the improvement in their clinical and psychic condition. Serum bromine levels in psoriatic Danes were somewhat lower than those in healthy subjects residing in Denmark, but the difference was not significant. Israelis working in the open air in the Dead Sea area (air bromine 20-fold higher than in Jerusalem) had higher bromine levels than psoriatic or healthy Israelis residing in Jerusalem or healthy Israelis working in air-conditioned rooms in the Dead Sea area (p < 0.05), but those levels were still within the normal range. As our animal experimentation indicates that the skin is a major target organ for 82Br, applied either by bathing or as an aerosol, we conclude that the higher bromine levels noticed in the psoriatic Danes after their 4-week stay at the Dead Sea may be equally due to their contact with the bromine-containing aerosol and the high bromine level of the Dead Sea waters.
Keywords: A1 Journal article; Pharmacology. Therapy; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1159/000137756
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“Health implications of atmospheric aerosols from asbestos-bearing road pavements traditionally used in Southern Brazil”. Godoi RHM, Goncalves SJ Jr, Sayama C, Polezer G, Reis Neto JM, Alfoldy B, Van Grieken R, Riedi CA, Yamamoto CI, Godoi AFL, Bencs L, Environmental Science and Pollution Research
T2 –, 1st International Caparica Conference on Pollutant Toxic Ions and, Molecules (PTIM), 2015, Caparica, PORTUGAL 23, 25180 (2016). http://doi.org/10.1007/S11356-016-7586-0
Abstract: Serpentine and amphibole asbestos occur naturally in certain geologic settings worldwide, most commonly in association with ultramafic rocks, along associated faults. Ultramafic rocks have been used in Pin County, Southern Brazil for decades for the purpose of road paving in rural and urban areas, but without the awareness of their adverse environmental and health impact. The aim of this study was the chemical characterization of aerosols re-suspended in two rural roads of Pin, paved with ultramafic rocks and to estimate the pulmonary deposition of asbestos aerosols. Bulk aerosol samples were analyzed by means of X-ray fluorescence spectrometry and X-ray diffraction analysis, in order to characterize elemental composition and crystallinity. Single-particle compositions of aerosols were analyzed by computer-controlled electron-probe microanalysis, indicating the presence of a few percentages of serpentine and amphibole. Given the chemical composition and size distribution of aerosol particles, the deposition efficiency of chrysotile, a sub-group of serpentine, in two principal segments of the human respiratory system was estimated using a lung deposition model. As an important finding, almost half of the inhaled particles were calculated to be deposited in the respiratory system. Asbestos depositions were significant (similar to 25 %) in the lower airways, even though the selected breathing conditions (rest situation, nose breathing) implied the lowest rate of respiratory deposition. Considering the fraction of inhalable suspended chrysotile near local roads, and the long-term exposure of humans to these aerosols, chrysotile may represent a hazard, regarding more frequent development of lung cancer in the population of the exposed region.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1007/S11356-016-7586-0
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“Statistical grouping and controlling factors of dissolved trace elements in a surface water system”. Vandelannoote R, Blommaert W, Van 't dack L, Gijbels R, van Grieken R, Environmental technology letters 4, 363 (1983). http://doi.org/10.1080/09593338309384219
Abstract: Sensitive multi‐element analytical techniques were applied to determine 24 dissolved trace components in 25 different water samples from a 10 km2 zone in Brittany, France. Correspondence factor and multiple regression analyses showed that the elements considered are influenced mainly by the presence of: Fe‐Mn oxide accumulations, a local poly‐metallic sulfide mineralization, and non‐mineralized host rocks, agricultural activity and abundant organic material in local swamps. Via these numerical techniques the location of the poly‐metallic ore body can be derived from the data set.
Keywords: A3 Journal article; Plasma Lab for Applications in Sustainability and Medicine – Antwerp (PLASMANT); AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 1
DOI: 10.1080/09593338309384219
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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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“Hydrogeochemistry in the zinclead mining district of Les Malines (Gard, France)”. Bosch B, Leleu M, Oustrière P, Sarcia C, Sureau JF, Blommaert W, Gijbels R, Sadurski A, Vandelannoote R, Van Grieken R, Van 'T Dack L;, Chemical geology 55, 31 (1986). http://doi.org/10.1016/0009-2541(86)90125-7
Abstract: Sensitive multi-element analysis techniques together with major-element and isotopic analyses were applied to spring, mine and surface waters in the vicinity of an important known zinclead deposit in a carbonate environment, in the Les Malines area (Gard, France). Both the dissolved and suspended phases were investigated, and concretions and sediments were also considered in some cases. This methodological test shows that the ore body leaves various clear fingerprints, such as the Zn, As, Sb, Pb and U levels in the dissolved phase, the sulfate increment and the δ 34S. Some of the elements in solution are controlled by slightly soluble compounds, e.g. Zn by smithsonite and hydrozincite, Ba by barite, and Pb by hydrocerussite. Mapping the saturation indices for these elements appears useful for displaying the hydrogeochemical anomaly.
Keywords: A1 Journal article; Plasma Lab for Applications in Sustainability and Medicine – Antwerp (PLASMANT); AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.524
Times cited: 3
DOI: 10.1016/0009-2541(86)90125-7
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“Composition of Facon de Venise glass from early 17th century London in comparison with luxury glass of the same age”. Cagno S, de Raedt I, Jeffries T, Janssens K, Proceedings of the Society of Photo-optical Instrumentation Engineers
T2 –, Conference on Integrated Approaches to the Study of Historical Glass, (IASHG), APR 16-17, 2012, Brussels, BELGIUM , 842205 (2012). http://doi.org/10.1117/12.975212
Abstract: SEM-EDX and LA-ICP-MS analyses were performed on a set of early 17th century London glass fragments. The samples originate from two archaeological sites (Aldgate and Old Broad Street) where glass workshops were active in this period. The great majority of the samples are made of soda glass. Two distinct compositional groups are observed, each typical of one site of provenance. The samples originating from the Old Broad Street excavation feature a silica-soda-lime composition, with a moderate amount of potash. The samples from Aldgate are richer in potassium and feature higher amounts of trace elements such as Rb, Zr and Cu. The distinction between the two groups stems from different flux and silica sources used for glassmaking. A comparison with different European glass compositions of that time reveals no resemblance with genuine Venetian production, yet the composition of the Old Broad Street glass shows a close similarity to that of fragments produced 'a la facon de Venise' in Antwerp at the end of the 16th century. This coincides with historical sources attesting the arrival of glassworkers from the Low Countries in England and suggests that a transfer of technology took place near the turn of the century.
Keywords: P1 Proceeding; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Times cited: 1
DOI: 10.1117/12.975212
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“Determination of trace selenium in biological material by preconcentration and X-ray emission spectrometry”. Robberecht H, Van Grieken R, Analytica chimica acta 147, 113 (1983). http://doi.org/10.1016/0003-2670(83)80077-4
Abstract: Selenium is determined in the ng g−1 to μg g−1 range in biological and environmental samples. A wet digestion procedure was optimized with respect to volatility losses and recovery yields, by using 75Se metabolically incorporated into rat organs. Selenium is preconcentrated from the digestion liquid by a two-step reduction with 4 M HCl and ascorbic acid. The colloidal selenium formed is adsorbed on activated carbon and filtered on a Nucleopore membrane for measurement by energy-dispersive x-ray fluorescence. Almost complete recovery was obtained, and the detection limit was 20 ng, corresponding to 10 ng g−1 for a 2-g sample. Biological reference materials were analyzed with satisfactory results, and the accuracy of the method was good.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1016/0003-2670(83)80077-4
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“Iron speciation in soda-lime-silica glass: a comparison of XANES and UV-vis-NIR spectroscopy”. Ceglia A, Nuyts G, Meulebroeck W, Cagno S, Silvestri A, Zoleo A, Nys K, Janssens K, Thienpont H, Terryn H, Journal of analytical atomic spectrometry 30, 1552 (2015). http://doi.org/10.1039/C5JA00046G
Abstract: Scientific analyses of ancient glasses have been carried out for many years using elemental chemical analysis. However, it is known that the control of the redox conditions in the glass melt has a strong implication on the final hue of glass because it affects Fe2+/SFe. Therefore an increasing number of studies on the redox conditions have been published in recent years by means of synchrotron based Xray absorption spectroscopy. This is a technique which is not easily accessible and requires dedicated facilities. In this paper we describe an alternative approach by means of optical absorption spectroscopy. We synthesised 10 soda-lime-silica glasses with known redox conditions and iron concentration to calibrate the absorption at 1100 nm as a function of Fe2+ concentration. The linear extinction coefficient was also determined. These glasses were also studied by means of X-ray Absorption Near Edge Structure (XANES) spectroscopy. Electron paramagnetic resonance spectroscopy was additionally used as an ancillary method to verify the quality of our data. Furthermore 28 samples from real archaeological samples were analysed by XANES and optical spectroscopy as a case study. The Fe2+/SFe values obtained were compared and demonstrated that the two techniques were in good agreement with each other. Optical spectroscopy can be applied in situ with moderate sample preparation to determine the concentration of Fe2+. To investigate the redox conditions, especially as a first screening approach, this methodology is an important tool to take into consideration before applying more sophisticated techniques such as XANES, which is more elaborate and requires high-tech resources.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.379
Times cited: 20
DOI: 10.1039/C5JA00046G
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“A mobile instrument for in situ scanning macro-XRF investigation of historical paintings”. Alfeld M, Pedroso JV, van Hommes ME, van der Snickt G, Tauber G, Blaas J, Haschke M, Erler K, Dik J, Janssens K, Journal of analytical atomic spectrometry 28, 760 (2013). http://doi.org/10.1039/C3JA30341A
Abstract: Scanning macro-X-ray fluorescence analysis (MA-XRF) is rapidly being established as a technique for the investigation of historical paintings. The elemental distribution images acquired by this method allow for the visualization of hidden paint layers and thus provide insight into the artist's creative process and the painting's conservation history. Due to the lack of a dedicated, commercially available instrument the application of the technique was limited to a few groups that constructed their own instruments. We present the first commercially available XRF scanner for paintings, consisting of an X-ray tube mounted with a Silicon-Drift (SD) detector on a motorized stage to be moved in front of a painting. The scanner is capable of imaging the distribution of the main constituents of surface and sub-surface paint layers in an area of 80 by 60 square centimeters with dwell times below 10 ms and a lateral resolution below 100 mu m. The scanner features for a broad range of elements between Ti (Z = 22) and Mo (Z = 42) a count rate of more than 1000 counts per second (cps)?mass percent and detection limits of 100 ppm for measurements of 1 s duration. Next to a presentation of spectrometric figures of merit, the value of the technique is illustrated through a case study of a painting by Rembrandt's student Govert Flinck (1615-1660).
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.379
Times cited: 106
DOI: 10.1039/C3JA30341A
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