“Grazing-exit particle-induced X-ray emission analysis with extremely low background”. Tsuji K, Spolnik Z, Wagatsuma K, Van Grieken RE, Vis RD, Analytical chemistry 71, 5033 (1999). http://doi.org/10.1021/AC990568U
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/AC990568U
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“High-energy polarized-beam energy-dispersive X-ray fluorescence analysis combined with activated thin layers for cadmium determination at trace levels in complex environmental liquid samples”. Marguí, E, Fontàs C, van Meel K, Van Grieken R, Queralt I, Hidalgo M, Analytical chemistry 80, 2357 (2008). http://doi.org/10.1021/AC7018427
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/AC7018427
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“Interface for reproducible, multishot direct analysis of solid-phase microextraction samples”. Newsome GA, Kavich G, Alvarez-Martin A, Analytical Chemistry 92, 4182 (2020). http://doi.org/10.1021/ACS.ANALCHEM.9B05691
Abstract: An enclosed interface that joins a direct analysis in real time (DART) probe, solid-phase microextraction (SPME) fiber, and the inlet of a high-resolution mass spectrometer is described. Unlike other systems to couple SPME sampling to ambient mass spectrometry, the interface is able to perform discrete analyses on different areas of a single SPME fiber device for up to three technical replicate measurements of one sampling event. Inlet flow speed and desorption temperature are optimized, and reproducibility is demonstrated between replicate analyses on the same derivatized SPME fiber and with sequential fiber sampling events, yielding analyte measurement center of variance (CV) from 3 to 6%. Conditioning is also performed with the enclosed DART. The interface is a straightforward addition to commercially available technologies, and machine diagrams for custom components operated with SPME/DART/MS equipment are included.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
Impact Factor: 7.4
DOI: 10.1021/ACS.ANALCHEM.9B05691
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“Laser microprobe mass spectrometric identification of sulfur species in single micrometer-size particles”. Bruynseels FJ, Van Grieken RE, Analytical chemistry 56, 871 (1984). http://doi.org/10.1021/AC00270A004
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/AC00270A004
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“Laser microprobe mass spectrometry : 1 : basic principles and performance characteristics”. Denoyer E, Van Grieken R, Adams F, Ntausch DFS, Analytical chemistry 54, 26a (1982). http://doi.org/10.1021/AC00238A722
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/AC00238A722
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“Method for the determination of Pd-catalyst residues in active pharmaceutical ingredients by means of high-energy polarized-beam energy dispersive X-ray fluorescence”. Marguí, E, van Meel K, Van Grieken R, Buendía A, Fontás C, Hidalgo M, Queralt I, Analytical chemistry 81, 1404 (2009). http://doi.org/10.1021/AC8021373
Abstract: In medicinal chemistry, Pd is perhaps the most-widely utilized precious metal, as catalyst in reactions which represent key transformations toward the synthesis of new active pharmaceutical ingredients (APIs). The disadvantage of this metal-catalyzed chemistry is that expensive and toxic metal residues are invariably left bound to the desired product. Thus, stringent regulatory guidelines exist for the amount of residual Pd that a drug candidate is allowed to contain. In this work, a rapid and simple method for the determination of Pd in API samples by high-energy polarized-beam energy dispersive X-ray fluorescence spectrometry has been developed and validated according to the specification limits of current legislation (10 mg kg−1 Pd) and the International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH guidelines). Sample and calibration standards preparation includes a first step of homogenization and then, in a second step, the pressing of the powdered material into pellets without any chemical treatment. The use of several synthetic calibration standards made of cellulose to simulate the API matrix appears to be an effective means to obtain reliable calibration curves with a good spread of data points over the working range. With the use of the best measuring conditions, the limit of detection (0.11 mg kg−1 Pd) as well as the limit of quantitation (0.37 mg kg−1 Pd) achieved meet rigorous requirements. The repeatability of the XRF measurement appeared to be less than 2%, while the precision of the whole method was around 7%. Trueness was evaluated by analyzing spiked API samples at the level of the specification limit and calculating the recovery factor, which was better than 95%. To study the applicability of the developed methodology for the intended purpose, three batches of the studied API were analyzed for their Pd content, and the attained results were comparable to those obtained by the daily routine method (acid digestion plus atomic spectroscopy) used in most pharmaceutical laboratories.
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/AC8021373
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“Parameter evaluation for the analysis of oxide-based samples with radio ferquency glow discharge mass spectrometry”. de Gendt S, Van Grieken RE, Ohorodnik SK, Harrison WW, Analytical chemistry 67, 1026 (1995). http://doi.org/10.1021/AC00102A002
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/AC00102A002
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“Quantitative determination of low-Z elements in single atmospheric particles on boron substrates by automated scanning electron microscopy: energy-dispersive X-ray spectrometry”. Choël M, Deboudt K, Osán J, Flament P, Van Grieken R, Analytical chemistry 77, 5686 (2005). http://doi.org/10.1021/AC050739X
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/AC050739X
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“Sub-part-per-billion determination of total dissolved selenium and selenite in environmental waters by X-ray fluorescence spectrometry”. Robberecht HJ, Van Grieken RE, Analytical chemistry 52, 449 (1980). http://doi.org/10.1021/AC50053A017
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/AC50053A017
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“Three-dimensional trace element analysis by confocal X-ray microfluorescence imaging”. Vincze L, Vekemans B, Brenker FE, Falkenberg G, Rickers K, Somogyi A, Kersten M, Adams F, Analytical chemistry 76, 6786 (2004). http://doi.org/10.1021/AC049274L
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/AC049274L
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“X-ray spectrometry”. Szalóki I, Osán J, Van Grieken RE, Analytical chemistry 78, 4069 (2006). http://doi.org/10.1021/AC060688J
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/AC060688J
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“X-ray spectrometry”. Szalóki I, Osán J, Van Grieken RE, Analytical chemistry 76, 3445 (2004). http://doi.org/10.1021/AC0400820
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/AC0400820
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“X-ray spectrometry”. Szalóki I, Török SB, Injuk J, Van Grieken RE, Analytical chemistry 74, 2895 (2002). http://doi.org/10.1021/AC020241K
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/AC020241K
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“X-ray spectrometry”. Szalóki I, Török SB, Ro C-U, Injuk J, Van Grieken RE, Analytical chemistry 72, 211 (2000). http://doi.org/10.1021/A1000018H
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/A1000018H
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“X-ray spectrometry”. Török S, Labar J, Schmeling M, Van Grieken R, Analytical chemistry 70, 495r (1998)
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“X-ray spectrometry”. Török SB, Labar J, Injuk J, Van Grieken RE, Analytical chemistry R68, 467 (1996)
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“X-ray spectrometry”. Török SB, Van Grieken RE, Analytical chemistry 64r, 180 (1992)
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
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“X-ray spectrometry”. Markowicz AA, Van Grieken RE, Analytical chemistry 62, 101r (1990). http://doi.org/10.1021/AC00211A001
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/AC00211A001
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“X-ray spectrometry”. Markowicz AA, Van Grieken RE, Analytical chemistry 60, 28r (1988). http://doi.org/10.1021/AC00163A002
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/AC00163A002
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“X-ray spectrometry”. Markowicz AA, Van Grieken RE, Analytical chemistry 58, 279r (1986). http://doi.org/10.1021/AC00296A019
Keywords: A1 Journal article; AXES (Antwerp X-ray Analysis, Electrochemistry and Speciation)
DOI: 10.1021/AC00296A019
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“Chemical mapping of the degradation of geranium lake in paint cross sections by MALDI-MSI”. Alvarez-Martin A, Quanico J, Scovacricchi T, Avranovich Clerici E, Baggerman G, Janssens K, Analytical chemistry 95, 18215 (2023). http://doi.org/10.1021/ACS.ANALCHEM.3C03992
Abstract: Matrix assisted laser desorption ionization-mass spectrometry imaging (MALDI-MSI) has become a powerful method to extract spatially resolved chemical information in complex materials. This study provides the first use of MALDI-MSI to define spatial–temporal changes in oil paints. Due to the highly heterogeneous nature of oil paints, the sample preparation had to be optimized to prevent molecules from delocalizing. Here, we present a new protocol for the layer-specific analysis of oil paint cross sections achieving a lateral resolution of 10 μm and without losing ionization efficiency due to topographic effects. The efficacy of this method was investigated in oil paint samples containing a mixture of two historic organic pigments, geranium lake and lead white, a mixture often employed in the work of painter Vincent Van Gogh. This methodology not only allows for spatial visualization of the molecules responsible for the pink hue of the paint but also helps to elucidate the chemical changes behind the discoloration of paintings with this composition. The results demonstrate that this approach provides valuable molecular compositional information about the degradation pathways of pigments in specific paint layers and their interaction with the binding medium and other paint components and with light over time. Since a spatial correlation between molecular species and the visual pattern of the discoloration pattern can be made, we expect that mass spectrometry imaging will become highly relevant in future degradation studies of many more historical pigments and paints.
Keywords: A1 Journal article; Antwerp X-ray Imaging and Spectroscopy (AXIS); Ecosphere
Impact Factor: 7.4
DOI: 10.1021/ACS.ANALCHEM.3C03992
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“Micro to nano : multiscale IR analyses reveal zinc soap heterogeneity in a 19th-century painting by Corot”. Ma X, Pavlidis G, Dillon E, Beltran V, Schwartz JJ, Thoury M, Borondics F, Sandt C, Kjoller K, Berrie BH, Centrone A, Analytical chemistry 94, 3103 (2022). http://doi.org/10.1021/ACS.ANALCHEM.1C04182
Abstract: Formation and aggregation of metal carboxylates (metal soaps) can degrade the appearance and integrity of oil paints, challenging efforts to conserve painted works of art. Endeavors to understand the root cause of metal soap formation have been hampered by the limited spatial resolution of Fourier transform infrared microscopy (mu-FTIR). We overcome this limitation using optical photothermal infrared spectroscopy (O-PTIR) and photothermal-induced resonance (PTIR), two novel methods that provide IR spectra with approximate to 500 and approximate to 10 nm spatial resolutions, respectively. The distribution of chemical phases in thin sections from the top layer of a 19th-century painting is investigated at multiple scales (mu-FTIR approximate to 10(2) mu m(3), O-PTIR approximate to 10(-1) mu m(3), PTIR approximate to 10(-5) mu m(3)). The paint samples analyzed here are found to be mixtures of pigments (cobalt green, lead white), cured oil, and a rich array of intermixed, small (often << 0.1 mu m(3)) zinc soap domains. We identify Zn stearate and Zn oleate crystalline soaps with characteristic narrow IR peaks (approximate to 1530-1558 cm(-1)) and a heterogeneous, disordered, water-permeable, tetrahedral zinc soap phase, with a characteristic broad peak centered at approximate to 1596 cm(-1). We show that the high signal-to-noise ratio and spatial resolution afforded by O-PTIR are ideal for identifying phase-separated (or locally concentrated) species with low average concentration, while PTIR provides an unprecedented nanoscale view of distributions and associations of species in paint. This newly accessible nanocompositional information will advance our knowledge of chemical processes in oil paint and will stimulate new art conservation practices.
Keywords: A1 Journal article; Antwerp Electrochemical and Analytical Sciences Lab (A-Sense Lab)
DOI: 10.1021/ACS.ANALCHEM.1C04182
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