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  • 1.
    Blachucki, Wojciech
    et al.
    Polish Acad Sci, Inst Phys Chem, 44-52 Kasprzaka St, PL-01224 Warsaw, Poland.
    Czapla-Masztafiak, Joanna
    Polish Acad Sci, Inst Nucl Phys, 152 Radzikowskiego St, PL-31342 Krakow, Poland.
    Sá, Jacinto
    Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - Ångström, Physical Chemistry. Polish Acad Sci, Inst Phys Chem, 44-52 Kasprzaka St, PL-01224 Warsaw, Poland.
    Szlachetko, Jakub
    Polish Acad Sci, Inst Nucl Phys, 152 Radzikowskiego St, PL-31342 Krakow, Poland.
    A laboratory-based double X-ray spectrometer for simultaneous X-ray emission and X-ray absorption studies2019In: Journal of Analytical Atomic Spectrometry, ISSN 0267-9477, E-ISSN 1364-5544, Vol. 34, no 7, p. 1409-1415Article in journal (Refereed)
    Abstract [en]

    X-ray spectroscopy studies are usually performed using synchrotron radiation sources, which offer bright, coherent, energy-tuneable and monochromatic light. However, the application of synchrotron-based Xray emission spectroscopy (XES) and X-ray absorption spectroscopy (XAS) is directly constrained by the limited, infrequent access to central facilities. With the advent of new technological solutions in the field of X-ray sources, optics and detectors, the development of efficient and compact laboratory X-ray spectroscopy systems is possible. A permanent laboratory-based setup offers the advantages of low cost and easy accessibility and, therefore, more flexibility in the preparation and scheduling of measurements. Herein, we report a laboratory X-ray setup allowing simultaneous XES and XAS measurements. The double von Hamos spectrometer performances are demonstrated by concurrent K beta XES and K-edge XAS measurements done for 3d elements.

  • 2.
    Forsgard, Niklas
    et al.
    Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Physical and Analytical Chemistry.
    Sjöberg, Per
    Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Physical and Analytical Chemistry.
    Bylund, Dan
    Andersson, Marit
    Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Physical and Analytical Chemistry.
    Pettersson, Jean
    Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Physical and Analytical Chemistry.
    Screening and identification of aluminium-containing biomolecules by column-switched LC-ICP-MS and LC-ESI-MS/MS2007In: Journal of Analytical Atomic Spectrometry, ISSN 0267-9477, E-ISSN 1364-5544, Vol. 22, no 11, p. 1397-1402Article in journal (Refereed)
    Abstract [en]

    Column-switching liquid chromatography followed by low resolution ICP-MS was evaluated as a tool for speciation analysis of aluminium-containing biomolecules. The strategy was applied on siderophores, small organic molecules (Mr < 1500) which normally act as strong iron chelators. The drawbacks normally encounterd with aluminium detection using low resolution ICP-MS are the formation of polyatomic ions causing isobaric overlaps and space-charge effects. When adding a carbon rich solvent, such as methanol or acetonitrile, the 13C14N+, 12C15N+ and 12C14N1H+ with the same mass as 27Al+ will form in the plasma. The nitrogen is either entrained from the surrounding atmosphere or added with the constituents in the mobile phase. These disadvantages were successfully counteracted by the use of nitrogen free organic modifier in the mobile phase and the use of cool plasma conditions. Detection limits for standard solutions of aluminium-chelated ferrichrome in sub-nanomolar range were obtained by monitoring the aluminium-27 isotope. The combined use of LC-ICP-MS and LC-ESI-MS/MS was also evaluated as a tool to identify unknown metal complexes, here siderophores, in field soil solution samples. Two aluminium-chelated siderophores, Al-desferrichrom and Al-desferricrocin, were identified and quantified. Both aluminium-siderophore complexes were present in the low nanomolar range (1.1 and 0.7 nM, respectively).

  • 3.
    Forsgård, Niklas
    et al.
    Uppsala University, Disciplinary Domain of Science and Technology, Technology, Department of Engineering Sciences, Ion Physics.
    Salehpour, Mehran
    Uppsala University, Disciplinary Domain of Science and Technology, Technology, Department of Engineering Sciences, Ion Physics.
    Possnert, Göran
    Uppsala University, Disciplinary Domain of Science and Technology, Technology, Department of Engineering Sciences, Ion Physics.
    Accelerator mass spectrometry in the attomolar concentration range for C-14-labeled biologically active compounds in complex matrixes2010In: Journal of Analytical Atomic Spectrometry, ISSN 0267-9477, E-ISSN 1364-5544, Vol. 25, no 1, p. 74-78Article in journal (Refereed)
    Abstract [en]

    Accelerator mass spectrometry (AMS) is an ultra-sensitive analytical method suitable for detection of sub-nanomolar concentrations of labeled biological substances such as pharmaceutical drugs in body fluids. A limiting factor in extending the concentration measurements to the sub-picomolar range is the natural C-14 content in living tissues. This can be circumvented by separating the labeled drug from the tissue matrix with, for example, liquid chromatography. The analysis of drugs and their metabolites or endogenous compounds in biological fluids by liquid chromatography is usually complicated and the sample preparation step remains the most serious problem both with regard to losses and degradation of the analyte, and also automation of the analysis. In this article a method for detection and quantification of extremely low concentrations of C-14-labeled biomolecules in biological fluids by AMS is described. The use of a column switched chromatographic system incorporating a restricted-access media (RAM) column allowed the direct injection of untreated human plasma samples, which reduces the total time of analysis and makes automation of the sample preparation step possible. As the separated total drug amount is in the attogram to femtogram region, it is not possible to use a standard AMS sample preparation method, where mg sizes are required. We have utilized a sensitive carbon carrier method where a C-14-deficient compound is added to the HPLC fractions and the composite sample is prepared and analysed by AMS. The method shows remarkable sensitivity, low background values and good linearity, allowing the detection and quantification of a pharmaceutical drug in human plasma in the low femtomolar and down to the attomolar concentration range.

  • 4.
    Korvela, Marcus
    et al.
    Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - BMC, Analytical Chemistry.
    Andersson, Marit
    Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - BMC, Analytical Chemistry.
    Pettersson, Jean
    Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - BMC, Analytical Chemistry.
    Internal standards in inductively coupled plasma mass spectrometry using kinetic energy discrimination and dynamic reaction cells2018In: Journal of Analytical Atomic Spectrometry, ISSN 0267-9477, E-ISSN 1364-5544, Vol. 33, no 10, p. 1770-1776Article in journal (Refereed)
    Abstract [en]

    ICP-MS is a sensitive element analysis technique used for analyzing several different sample types. This can result in difficult matrixes which can affect both physical parameters and create overlaps of analyte elements. Some of the possible overlaps can be reduced by the use of reaction and/or collision cells, while the use of internal standards can help with reducing the physical interferences caused by a matrix. While both internal standardization and the use of cells have been studied separately, their effects on each other have not been investigated earlier. In this study ICP-MS was used to analyze Mg-24, Al-27, Ti-47, Ti-49, V-51, Cr-52, Cr-53, Mn-55, Fe-57, Co-59, Ni-60, Ni-61, Ni-62, Cu-63, Cu-65, Zn-66, Zn-67, As-75, Se-78, Se-82, Cd-111, and Pb-208 with Be-9, Y-89, Ga-69, Rh-103, In-115, Ir-193, and Tl-205 as internal standards with high concentrations of either HNO3, PBS-buffer, or Triton X-100 as the matrix, in reaction-, collision- and standard-cell modes. This was done to investigate which internal standards would compensate matrix effects in different cell modes. All internal standards, except Be, compensated fairly well (relative sensitivity RSD < 10%) even for severe matrix effects for most elements regardless of similarity in mass in the different cell modes. For Zn, As and Se no proper internal standard could be found, of the ones investigated.

  • 5. Kvashnina, Kristina O.
    et al.
    Butorin, Sergei M.
    Uppsala University, Disciplinary Domain of Science and Technology, Physics, Department of Physics and Astronomy, Soft X-Ray Physics.
    Glatzel, Pieter
    Direct study of the f-electron configuration in lanthanide systems2011In: Journal of Analytical Atomic Spectrometry, ISSN 0267-9477, E-ISSN 1364-5544, Vol. 26, no 6, p. 1265-1272Article in journal (Refereed)
    Abstract [en]

    The valence shell electron configurations within a few electron volts above the Fermi level in cerium, ytterbium, europium and samarium compounds were probed by resonant X-ray emission spectroscopy (RXES) at the L-3 absorption pre-edge. The rare earth systems show distinct spectral signatures depending on the f-electron configuration. The high energy resolution experimental results reported here are well reproduced by atomic multiplet calculations confirming the localized character of the 4f electrons. The magnitude of the electron-electron interactions within the 4f shell and between 3d and 4f electrons is analyzed. The present technique is a powerful tool for the study of the 4f valence electron configuration that, unlike L-3 absorption spectroscopy at the main edge, is little influenced by valence electron relaxation following core hole creation.

  • 6.
    Vegelius, Johan
    et al.
    Uppsala University, Disciplinary Domain of Science and Technology, Physics, Department of Physics and Astronomy, Soft X-Ray Physics.
    Kvashnina, Kristina
    Klintenberg, Mattias
    Uppsala University, Disciplinary Domain of Science and Technology, Physics, Department of Physics and Astronomy, Materials Theory.
    Soroka, Inna
    Butorin, Sergei
    Uppsala University, Disciplinary Domain of Science and Technology, Physics, Department of Physics and Astronomy, Soft X-Ray Physics.
    Cu Kβ2,5 X-ray emission spectroscopy as a tool for characterization of monovalent copper compounds2012In: Journal of Analytical Atomic Spectrometry, ISSN 0267-9477, E-ISSN 1364-5544, Vol. 27, no 11, p. 1882-1888Article in journal (Refereed)
    Abstract [en]

    Cu Kβ 2,5 X-ray emission and resonant inelastic X-ray scattering measurements were performed on monovalent and divalent copper compounds. The data were compared with the results of local-density- approximation calculations. The methods were found to be efficient tools for studies of Cu 4p states in the valence band and for distinguishing between different monovalent copper compounds. This is of particular importance for the debate concerning copper corrosion in oxygen-free water.

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