“The ID21 X-ray and infrared microscopy beamline at the ESRF: status and recent applications to artistic materials”. Cotte M, Pouyet E, Salome M, Rivard C, De Nolf W, Castillo-Michel H, Fabris T, Monico L, Janssens K, Wang T, Sciau P, Verger L, Cormier L, Dargaud O, Brun E, Bugnazet D, Fayard B, Hesse B, del Real AEP, Veronesi G, Langlois J, Balcar N, Vandenberghe Y, Sole VA, Kieffer J, Barrett R, Cohen C, Cornu C, Baker R, Gagliardini E, Papillon E, Susini J, Journal of analytical atomic spectrometry 32, 477 (2017). http://doi.org/10.1039/C6JA00356G
Abstract: The ID21 beamline (European Synchrotron Radiation facility, France) is a multi micro-analytical platform combining X-ray and infrared micro-probes, for characterization of elements, species, molecular groups and crystalline structures in complex materials. Applications are mainly in the fields of cultural heritage, life science, environmental and earth sciences, materials sciences. Here, we first present the status of instruments: (i) the scanning micro-spectroscopy end-station, operating from 2.0 to 9.2 keV, under vacuum and offering cryo conditions, for the acquisition of 2D micro X-ray fluorescence (mu XRF) maps, single point micro X-ray Absorption Near Edge Structure (mu XANES) spectra and speciation maps with sub-micrometric resolution; (ii) the XANES full-field end-station, operating in the same vacuum and energy conditions, for the acquisition of hyper-spectral radiographs of thin concentrated samples, resulting in speciation maps with micrometric resolution and millimetric field of view; (iii) the scanning micro-X-ray diffraction (mu XRD)/mu XRF end-station, operating at 8.5 keV, in air, for the acquisition of 2D crystalline phase maps, with micrometric resolution; and (iv) the scanning infrared microscope, operating in the mid-infrared range for the acquisition of molecular maps and some structural maps with micrometric resolution. Recent hardware and software developments are presented, as well as new protocols for improved sample preparation of thin sections. Secondly, a review of recent applications for the study of cultural heritage is presented, illustrated by various examples: determination of the origin of the color in blue Chinese porcelains and in brown Sevres porcelains; detection of lead in ink on Herculaneum papyri; identification and degradation of modeling materials used by Auguste Rodin and of chrome yellow pigments used by Vincent van Gogh. Cryo capabilities are illustrated by the analysis of plants exposed to chromate solutions. These examples show the variety of materials analyzed, of questions tackled, and particularly the multiple advantages of the ID21 analytical platform for the analysis of ancient and artistic materials.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.379
Times cited: 39
DOI: 10.1039/C6JA00356G
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“Thermodynamic and experimental study of the degradation of the red pigment mercury sulfide”. Radepont M, Coquinot Y, Janssens K, Ezrati J-J, de Nolf W, Cotte M, Journal of analytical atomic spectrometry 30, 599 (2015). http://doi.org/10.1039/C4JA00372A
Abstract: The red pigment mercury sulfide, called cinnabar or vermilion, is well known to suffer from an alteration giving rise to a grey, grey-white or black color at the surface of degraded works of art. This phenomenon can dramatically affect the esthetical value of artworks. This work aims at assessing the factors (light, halides) influencing the instability of red mercury sulfide and understanding (by combining thermodynamic and experimental approaches) the chemical equilibria governing the formation and evolution of the different degradation compounds. From the thermodynamic study of the Hg-S-Cl-H2O system, it was concluded that Hg(0), Hg3S2Cl2, and Hg2Cl2 can be formed from the reaction of alpha-HgS with ClO(g). In the second part, the artificial ageing experiments presented were carried out on model samples following the conditions assessed in the first part, in order to reproduce natural ageing observed on red mercury sulfide. Similarly to degradation compounds detected on original works of art, mercury chlorine compounds such as calomel (Hg2Cl2) and corderoite (alpha-Hg3S2Cl2) were identified on the surface of alpha-HgS model samples, when exposed to light and a sodium hypochlorite solution. Sulfates were detected as well, and more particularly gypsum (CaSO4 center dot 2H(2)O) when Ca was originally present in the model sample. The relationship between color and composition is discussed as well.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.379
Times cited: 26
DOI: 10.1039/C4JA00372A
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“Trace analysis allows to distinguish between Venetian and facon-de-Venise glass vessels of the 16th and 17th century”. de Raedt I, Janssens K, Veeckman J, Vincze L, Vekemans B, Jeffries T, Journal of analytical atomic spectrometry 16, 1012 (2001). http://doi.org/10.1039/B102597J
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.379
Times cited: 49
DOI: 10.1039/B102597J
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“The use of LA-ICP-MS for the characterization of the micro-heterogeneity of heavy metals in BCR CRM 680”. Kempenaers L, Bings NH, Jeffries TE, Vekemans B, Janssens K, Journal of analytical atomic spectrometry 16, 1006 (2001). http://doi.org/10.1039/B102512K
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.379
Times cited: 23
DOI: 10.1039/B102512K
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“The use of lead-glass capillaries for microfocusing of highly energetic (0-60 KeV) synchrotron radiation”. Janssens K, Vincze L, Vekemans B, Adams F, Haller M, Knöchel A, Journal of analytical atomic spectrometry 13, 339 (1998). http://doi.org/10.1039/A707700I
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.379
DOI: 10.1039/A707700I
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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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“Visualization of As(III) and As(V) distributions in degraded paint micro-samples from Baroque- and Rococo-era paintings”. Vermeulen M, Nuyts G, Sanyova J, Vila A, Buti D, Suuronen J-P, Janssens K, Journal of analytical atomic spectrometry 31, 1913 (2016). http://doi.org/10.1039/C6JA00134C
Abstract: Orpiment and realgar, both arsenic sulfide pigments respectively used for their vivid yellow and red-orange hues, are two of many artists' pigments that appear not to be stable upon light exposure, quickly degrading to arsenic trioxide and arsenate. This often results in whitening or transparency in the painted surfaces. While conventional techniques such as microscopic Raman (mu-RS) and microscopic Fourier transform infrared (mu-FTIR) spectroscopies can allow a quick and relatively easy identification of the orpiment, realgar, artificial arsenic sulfide glass and, to some extent, arsenic oxide, the identification and visualization of distributions of the degradation products – and especially arsenate compounds – in the paint micro-samples is generally more challenging. This challenge is due to the rather unfavorable limit of detection and low spectral resolution of such conventional spectroscopic techniques. This restricts the conclusions that can be drawn regarding the conservation state of valuable works of art. In this paper, we present how synchrotron radiation (SR) based techniques can overcome this challenge while working on painting cross-sections taken from a 17th-century painting by the Flemish artist Daniel Seghers (oil on canvas, Statens Museum for Kunst, Denmark) and an 18th-century French Chinoiserie (private collection, France). SR micro-X-ray fluorescence (m-XRF) mapping analysis performed on a visually degraded orpiment-containing paint stratigraphy reveals that arsenic is distributed throughout the entire cross-section, while X-ray absorption near edge structure (mu-XANES) demonstrated that the arsenic is present in both arsenite (As-III) and arsenate (As-V) forms. The latter compound(s), despite being barely identifiable by means of FTIR, were not only located at the surface of large and partially altered grains of arsenic sulfide but also spread throughout the entire paint stratigraphy. Their presence and distribution are attributed either to the complete degradation of smaller arsenic sulfide grains or to migration of the arsenates within the paint layer away from their original location of formation. The combination of mu-XRF and mu-XANES was very useful for the characterization of the advanced degradation state of the arsenic-containing pigments in paint systems; this type of information could not be obtained by means of conventional spectroscopic methods of microanalysis.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.379
Times cited: 20
DOI: 10.1039/C6JA00134C
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“Development of a multi-method analytical approach based on the combination of synchrotron radiation X-ray micro-analytical techniques and vibrational micro-spectroscopy methods to unveil the causes and mechanism of darkening of “fake-gilded&rdquo, decorations in a Cimabue painting”. Monico L, Prati S, Sciutto G, Catelli E, Romani A, Balbas DQ, Li Z, De Meyer S, Nuyts G, Janssens K, Cotte M, Garrevoet J, Falkenberg G, Tardillo Suarez VI, Tucoulou R, Mazzeo R, Journal of analytical atomic spectrometry 37, 114 (2022). http://doi.org/10.1039/D1JA00271F
Abstract: Redox processes activated by environmental factors have been identified as the main cause of the chromatic alterations of a number of artists' pigments, including the yellow pigment orpiment (As2S3). Although a general comprehension of the mechanisms has been provided through characterization of degradation compounds of As2S3, experimental evidences to prove how other paint components and how different environmental agents influence the formation pathways of specific secondary compounds are still lacking. Thus, it becomes fundamental to develop a methodological strategy which enable achieving a discrimination among the causes affecting the chemical stability of more heterogenous As2S3-based paints and defining the mechanism through which the alteration establishes and evolves, with the ultimate goal of optimizing the preventive conservation measures of unique masterpieces. In this paper, we propose a comprehensive multi-material and multi-method approach based on the combination of synchrotron radiation X-ray micro-analytical techniques (i.e., X-ray diffraction, X-ray fluorescence and X-ray absorption near edge structure spectroscopy at S K-/Ag L-3-/As K-edges) and vibrational micro-spectroscopy methods to unveil the causes and mechanism of darkening of “fake-gilded” decorations in tempera paintings, originally consisting of an unusual mixture of As2S3 and metallic silver (Ag-0). Such degradation process is a not yet understood phenomenon threatening a series of Old Master paintings, including those by the Italian painters Cimabue and Pietro Lorenzetti. The high specificity, sensitivity and lateral resolution of the employed analytical methods allowed providing first-time evidence for the presence of black acanthite (alpha-Ag2S), mimetite [Pb-5(AsO4)(3)Cl] and syngenite [K2Ca(SO4)(2)center dot H2O] as degradation products of the “fake-gilded” decorations in the Maesta by Cimabue (Church of Santa Maria dei Servi, Bologna, Italy). Furthermore, the study of the painting combined with that of tempera paint mock-ups permitted to explore and define the environmental agents and internal factors causing the darkening, by proving that: (i) Ag-0 and moisture are key-factors for triggering the transformation of As2S3 to alpha-Ag2S and As-oxides; (ii) S2--ions arising from the degradation of As2S3 are the main responsible for the formation of alpha-Ag2S; (iii) light exposure strengthens the tendency of the paint components towards alteration. Based on our findings, we finally propose a degradation mechanism of As2S3/Ag-0-based tempera paints.
Keywords: A1 Journal article; Antwerp X-ray Imaging and Spectroscopy (AXIS)
Impact Factor: 3.4
DOI: 10.1039/D1JA00271F
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“Analysis of speleothems by electron and X-ray microprobes”. Kuczumow A, Vekemans B, Schalm O, Gysels K, Ro C-U, Van Grieken R, Journal of analytical atomic spectrometry 16, 90 (2001). http://doi.org/10.1039/B007725I
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1039/B007725I
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“Application of high-energy polarised beam energy dispersive X-ray fluorescence spectrometry to cadmium determination in saline solutions”. van Meel K, Fontàs C, Van Grieken R, Queralt I, Hidalgo M, Marguí, E, Journal of analytical atomic spectrometry 23, 1034 (2008). http://doi.org/10.1039/B718382H
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1039/B718382H
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“Characteristics of atomic absorption calibration curves with the transversely heated graphite furnace”. Bencs L, Szakács O, Szoboszlai N, Ajtony Z, Bozsai G, Journal of analytical atomic spectrometry 18, 105 (2003). http://doi.org/10.1039/B208198A
Abstract: Calibration curves with two quasi-linear sections ("double sloping'') were observed for the medium volatile elements, Cr and Cu, with the use of a SIMAA 6000 graphite furnace atomic absorption spectrometer under interrupted internal gas flow conditions. If a standard transversally heated graphite atomizer (THGA) tube was shortened by 0.5 mm at both of its ends, (i.e. the gaps were enlarged between graphite furnace housing and tube ends), a stronger declination of the calibration curves resulted. Elements with fairly high diffusion coefficients (>5.8 cm(2) s(-1)) and with short appearance time of their transients (<0.6 s), such as Cr and Cu, have shown the most characteristic sensitivity drop towards higher concentrations. This anomalous feature could be eliminated in three different ways; (1) by applying end-capped THGA tubes, (2) using mini-flow (50 cm(3) min(-1)) conditions during the atomization stage, and (3) by adding Pd-Mg chemical modifier. For the low volatile Mo and V, the calibration curves had no irregular shape. For Ag, Co, Cr, Cu, Mn and Ni, the mini-flow settings improved the linearity of the calibration curves and extended the upper limit of the linear calibration range by a factor of 1.5-2.0. The irregular characteristic of the analytical curves was interpreted as an increased vapour loss at higher analyte concentrations through the opened ends of the standard THGA tubes. This vapour loss was associated with the significantly diverse expulsion velocities of atoms, caused by the difference in temperature and concentration gradients, when evaporating amounts of analytes with more than one order of magnitude difference.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1039/B208198A
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“Combined 1D, 2D and 3D micro-XRF techniques for the analysis of illuminated manuscripts”. Lachmann T, van der Snickt G, Haschke M, Mantouvalou I, Journal of analytical atomic spectrometry 31, 1989 (2016). http://doi.org/10.1039/C6JA00220J
Abstract: The combination of several micro-XRF analysis modes is presented for the investigation of an illuminated parchment manuscript. With a commercial instrument, conventional micro-XRF spot analysis (0D) and mapping (2D) are performed, yielding detailed lateral elemental information. Depth resolution becomes accessible by mounting an additional polycapillary lens in front of an SDD detector. Quantitative confocal depth profiles (1D) are presented as well as the full separation of the front and the backside decorations with the help of fast 3D mappings of specific areas. Only through the use of these multidimensional modes can elemental information be assigned both to lateral and depth positions, making the analysis of such heterogeneous samples feasible.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1039/C6JA00220J
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“Comparison between direct current and radiofrequency glow discharge mass spectrometry for the analysis of oxide-based samples”. de Gendt S, Van Grieken R, Hang W, Harrison WW, Journal of analytical atomic spectrometry 10, 689 (1995). http://doi.org/10.1039/JA9951000689
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1039/JA9951000689
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“Critical assessment and proposal for reconstruction of a grazing emission X-ray fluorescence instrument”. Kuczumow A, Schmeling M, Van Grieken R, Journal of analytical atomic spectrometry 15, 535 (2000). http://doi.org/10.1039/A908661G
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1039/A908661G
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“Elemental x-ray images obtained by grazing-exit electron probe microanalysis (GE-EPMA)”. Tsuji K, Nullens R, Wagatsuma K, Van Grieken RE, Journal of analytical atomic spectrometry 14, 1711 (1999). http://doi.org/10.1039/A905301H
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1039/A905301H
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“Improved radiographic methods for the investigation of paintings using laboratory and synchrotron X-ray sources”. Schalm O, Cabal A, van Espen P, Laquière N, Storme P, Journal of analytical atomic spectrometry 26, 1068 (2011). http://doi.org/10.1039/C0JA00242A
Abstract: It is generally known that radiographic inspection of 1517th century paintings can easily be done with a polychromatic X-ray source using a voltage between 20 kV and 40 kV in combination with classic X-ray films. Unfortunately, the spatial structure of numerous 19th and early 20th century paintings cannot be visualized with conventional radiography due to several reasons such as the use of lead white grounds or low absorbing pigments. Radiographic images are blurred or worse, they do not contain the picture of the painting. During the last decades, many technological innovations have been introduced in the field of radiography but their possibilities in cultural heritage have not been explored in full detail. In our investigation we used phosphor imaging plates, energy dispersive detectors and CCD-cameras in combination with synchrotron radiation and conventional X-ray tubes in order to improve the quality of radiographic images. Several promising techniques that could improve the quality of radiographs of paintings were identified.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1039/C0JA00242A
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“Inorganic nitrogen speciation in single micrometer-size particles by laser microprobe mass analysis”. Bruynseels F, Otten P, Van Grieken R, Journal of analytical atomic spectrometry 3, 237 (1988). http://doi.org/10.1039/JA9880300237
Abstract: Individual micrometer-size particles of inorganic nitrogen salts, such as NaNO3, NaNO2, (NH4)2SO4, NH4Cl, NH4NO3 and their mixtures, were analysed in the laser microprobe mass analyser. The cluster-ion distributions of the salts are systematically described and can be used to gain speciation information. The results can be used to study the distribution of the atmospheric aerosol inorganic nitrogen compounds and to investigate their chemical transformations under ambient conditions.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1039/JA9880300237
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“Optimization of secondary cathode thickness for direct current glow discharge mass spectrometric analysis of glass”. Schelles W, de Gendt S, Van Grieken RE, Journal of analytical atomic spectrometry 11, 937 (1996). http://doi.org/10.1039/JA9961100937
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1039/JA9961100937
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“Processing of three-dimensional microscopic X-ray fluorescence data”. Vekemans B, Vincze L, Brenker FE, Adams F, Journal of analytical atomic spectrometry 19, 1302 (2004). http://doi.org/10.1039/B404300F
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1039/B404300F
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“Quantification of boron in cells for evaluation of drug agents used in boron neutron capture therapy”. Verlinden B, Van Hoecke K, Aerts A, Daems N, Dobney A, Janssens K, Cardinaels T, Journal Of Analytical Atomic Spectrometry 36, 598 (2021). http://doi.org/10.1039/D0JA00456A
Abstract: Boron neutron capture therapy (BNCT) is an extensively studied radiotherapeutic strategy for cancer treatment. BNCT is based on irradiation of malignant tumour cells with neutrons after uptake of a B-10 containing molecule. Alpha particles, locally produced by neutron irradiation kill the cancer cells. Important for ongoing research regarding cellular uptake and cytotoxicity of a large variety of B-10 containing molecules is the accurate determination of boron concentrations in cell cultures. In this work, the sample preparation for quantitative inductively coupled plasma mass spectrometry (ICP-MS) analysis on cell cultures was optimized. By making use of acid digestion combined with UV digestion, low detection limits (0.4 mu g L-1) and full recoveries of boron could be achieved while measurements were free of spectral and non-spectral interferences. Finally, cell-associated boron in the form of 4-borono-l-phenylalanine (l-BPA) in vascular endothelial cell cultures could be determined with ICP-MS as (1.26 +/- 0.10) x 10(9) boron atoms per cell. The developed method can prove its importance for further BNCT research and elemental analysis of cell cultures.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 3.379
DOI: 10.1039/D0JA00456A
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“Quantification problems in light element determination by grazing emission X-ray fluorescence”. Kuczumow A, Claes M, Schmeling M, Van Grieken R, de Gendt S, Journal of analytical atomic spectrometry 15, 415 (2000). http://doi.org/10.1039/A908724I
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1039/A908724I
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“Quantitative analysis of iron-rich and other oxide-based samples by means of glow discharge mass spectrometry”. de Gendt S, Schelles W, Van Grieken R, Müller V, Journal of analytical atomic spectrometry 10, 681 (1995). http://doi.org/10.1039/JA9951000681
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1039/JA9951000681
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“Quantitative analysis of zirconium oxide by direct glow discharge mass spectrometry using a secondary cathode”. Schelles W, Van Grieken R, Journal of analytical atomic spectrometry 12, 49 (1997)
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“Quantitative characterisation of the leaching of lead and other elements from glazed surfaces of historical ceramics”. Szalóki I, Braun M, Van Grieken R, Journal of analytical atomic spectrometry 15, 843 (2000). http://doi.org/10.1039/B000746N
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1039/B000746N
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“Spectrometric determination of silicon in food and biological samples: an interlaboratory trial”. van Dyck K, Robberecht H, van Cauwenbergh R, Deelstra H, Arnaud J, Willemyns L, Benijts F, Centeno JA, Taylor H, Soares ME, Bastos ML, Ferreira MA, d'Haese PC, Lamberts LV, Hoenig M, Knapp G, Lugowski SJ, Moens L, Riondato J, Van Grieken R, Claes M, Verheyen R, Clement L, Uytterhoeven M, Journal of analytical atomic spectrometry 15, 735 (2000). http://doi.org/10.1039/B000572J
Abstract: Accuracy and precision of silicon determination in biological matrices (serum, urine, water, beer and spinach) by spectrometric techniques (when necessary after acid destruction) were assessed by means of a collaborative interlaboratory trial. The trial was set up in accordance with ISO 5725-2 (1994). The relative overall repeatability standard deviation was acceptable. It varied between 4% for spinach powder (mean content: 176 mg kg(-1)) and 11% for serum (mean content: 5.33 mg L-1). On the other hand, the relative overall between-laboratory standard deviation was found to vary from a satisfactorily 15% for spinach after destruction (mean content: 3.32 mg L-1) to an unacceptable 107% for spinach powder (mean content: 176 mg kg(-1)). The overall conclusion of the trial was that silicon determination in biological matrices can properly be performed by spectrometric techniques. However, when sample pretreatment (i.e., acid destruction) is needed prior to silicon determination problems still remain.
Keywords: A1 Journal article; Behavioural Ecology & Ecophysiology; Pathophysiology; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1039/B000572J
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