TY - JOUR A1 - Simon, Sebastian A1 - Selleng, C. A1 - Meng, Birgit T1 - Prompt phase analyses of ultrahigh-performance concrete JF - Journal of Materials in Civil Engineering N2 - Powder X-ray diffraction is a time-consuming and challenging task, especially for preparation of sensitive phases like ettringite and calcium-silicate-hydrate (C-S-H) phases. Fine-grained ultrahigh-performance concrete (UHPC) with an average grain size <100 μm could be investigated directly without time-consuming milling. As a proof of concept, small UHPC cylinders with plain surfaces were investigated with a newly designed sample holder. The comparison with conventionally prepared powder shows the feasibility of fast qualitative phase analysis using this approach. As a great benefit, a depth-dependent analysis, as well as a comparison of surface layers and core material, was carried out. KW - Ultrahigh-performance concrete (UHPC) KW - X-ray diffraction (XRD) KW - Sample holder KW - Fast measurement KW - Spatial analyses PY - 2018 DO - https://doi.org/10.1061/(ASCE)MT.1943-5533.0002163 SN - 1943-5533 SN - 0899-1561 VL - 30 IS - 3 SP - 06018001, 1 EP - 06018001, 5 PB - American Society of Civil Engineers CY - Reston, VA, USA AN - OPUS4-43879 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Simon, Sebastian A1 - Gluth, Gregor A1 - Peys, A. A1 - Onisei, S. A1 - Banerjee, D. A1 - Pontikes, Y. T1 - The fate of iron during the alkali-activation of synthetic (CaO-)FeOx-SiO2 slags: An Fe K-edge XANES study JF - Journal of the American Ceramic Society N2 - Slags from the nonferrous metals industry have great potential to be used as feedstocks for the production of alkali-activated materials. Until now, however, only very limited information has been available about the structural characteristics of these materials. In the work presented herein, synthetic slags in the CaO–FeOx–SiO2 system, representing typical compositions of Fe-rich slags, and inorganic polymers (IPs) produced from the synthetic slags by activation with alkali Silicate solutions have been studied by means of X-ray absorption near-edge structure (XANES) spectroscopy at the Fe K-edge. The iron in the slags was largely Fe2+, with an average coordination number of approximately 5 for the iron in the amorphous fraction. The increase in average oxidation number after alkali-activation was conceptualized as the consequence of slag dissolution and IP precipitation, and employed to calculate the degrees of reaction of the slags. The degree of reaction of the slags increased with increasing amorphous fraction. The iron in the IPs had an average coordination number of approximately 5; thus, IPs produced from the Fe-rich slags studied here are not Fe-analogs of aluminosilicate geopolymers, but differ significantly in terms of structure from the latter. KW - Alkali-activated slag KW - Inorganic polymers KW - Iron speciation KW - Nonferrous slag KW - X-ray absorption near-edge structure KW - X-ray absorption spectroscopy PY - 2018 DO - https://doi.org/10.1111/jace.15354 SN - 1551-2916 SN - 0002-7820 VL - 101 IS - 5 SP - 2107 EP - 2118 PB - John Wiley & Sons, Inc. AN - OPUS4-43880 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Seuthe, T. A1 - Grehn, M. A1 - Eberstein, M. A1 - Rosenfeld, A. A1 - Mermillod-Blondin, A. T1 - Time-resolved microscopy of fs-laser-induced heat flows in glasses JF - Applied Physics A N2 - Time-resolved phase-contrast microscopy is employed to visualize spatio-temporal thermal transients induced by tight focusing of a single Ti:sapphire fs-laser pulse into a solid dielectric sample. This method relies on the coupling of the refractive index change and the sample temperature through the thermo-optic coefficient dn/dT. The thermal transients are studied on a timescale ranging from 10 ns up to 0.1 ms after laser excitation. Beyond providing direct insights into the laser–matter interaction, analyzing the results obtained also enables quantifying the local thermal diffusivity of the sample on a micrometer scale. Studies conducted in different solid dielectrics, namely amorphous fused silica (a-SiO2), a commercial borosilicate glass (BO33, Schott), and a custom alkaline earth silicate glass (NaSi66), illustrate the applicability of this approach to the investigation of various glassy materials. KW - Femtosecond laser KW - Phase-contrast microscopy KW - Heat diffusion KW - Glasses PY - 2018 DO - https://doi.org/10.1007/s00339-017-1465-5 SN - 0947-8396 SN - 1432-0630 VL - 124 IS - 1 SP - 60, 1 EP - 6 PB - Springer-Verlag AN - OPUS4-43739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lasri, J. A1 - Chulvi, Katherine A1 - Eltayeb, N. E. T1 - Crystal structures of (E)-1-naphthaldehyde oxime and (E)-phenanthrene-9-carbaldehyde oxime JF - Acta crystallographica, Section E, Crystallographic communications N2 - The aldoximes C11H9NO (I) and C15H11NO (II), synthesized in ca 90%yield, by treatment of 1-naphthaldehyde or phenanthrene-9-carbaldehyde, respectively, with hydroxylamine hydrochloride and sodium carbonate, have been characterized by IR, 1H, 13C and DEPT-135 NMR spectroscopies, and also by singlecrystal X-ray diffraction analysis. The molecules of (I) and (II) are conformationally similar, with the aldoxime substituent groups lying outside the planes of the naphthalene or phenanthrene rings, forming dihedral angles with them of 23.9 (4) and 27.9 (6)°, respectively. The crystal structures of both (I) and (II) are similar with a single intermolecular O—H...N hydrogenbonding interaction, giving rise to the formation of one-dimensional polymeric chains extending along the 21 (b) screw axes in each. KW - Crystal structure KW - Aromatic aldehydes KW - E-aldoximes KW - Hydrogen bonding PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-443351 DO - https://doi.org/10.1107/S2056989018002116 SN - 2056-9890 VL - 74 SP - 332 EP - 336 PB - International Union of Crystallography CY - Chester AN - OPUS4-44335 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Tumanova, N. A1 - Tumanov, N. A1 - Robeyns, K. A1 - Fischer, Franziska A1 - Fusaro, L. A1 - Morelle, F. A1 - Ban, V. A1 - Hautier, G. A1 - Filinchuk, Y. A1 - Wouters, J. A1 - Leyssens, T. A1 - Emmerling, Franziska T1 - Opening Pandora’s Box: Chirality, Polymorphism, and Stoichiometric Diversity in Flurbiprofen/Proline Cocrystals JF - Crystal Growth & Design N2 - Proline has been widely used for various cocrystallization applications, including pharmaceutical cocrystals. Combining enantiopure and racemic flurbiprofen and proline, we discovered 18 new crystal structures. Liquid-assisted grinding proved highly efficient to explore all the variety of crystal forms. A unique combination of stateof-the-art characterization techniques, comprising variable temperature in situ X-ray diffraction and in situ ball-milling, along with other physicochemical methods and density functional theory calculations, was indispensable for identifying all the phases. Analyzing the results of in situ ball-milling, we established a stepwise mechanism for the formation of several 1:1 cocrystals via an intermediate 2:1 phase. The nature of the solvent in liquidassisted grinding was found to significantly affect the reaction rate and, in some cases, the reaction pathway. KW - Mechanochemistry KW - Polymorphs KW - In situ PY - 2018 UR - https://pubs.acs.org/doi/abs/10.1021/acs.cgd.7b01436 DO - https://doi.org/10.1021/acs.cgd.7b01436 VL - 18 IS - 2 SP - 954 EP - 961 PB - American Chemical Society AN - OPUS4-44365 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Medina, A. A1 - Ol, M. V. A1 - Greenblatt, D. A1 - Müller-Vahl, H. A1 - Strangfeld, Christoph T1 - High-Amplitude Surge of a Pitching Airfoil: Complementary Wind- and Water-Tunnel Measurements JF - AIAA Journal N2 - RECENT interest in gust response, rotorcraft forward flight and wind energy, among other applications, has focused on streamwise oscillations of nominally two-dimensional airfoils in attached and separated flows. The airfoil may be simultaneously held at constant incidence or execute some maneuver, such as pitch. The relative freestream is spatially uniform but temporally unsteady, and this can be accomplished in a ground-test facility in two ways. The first method is to vary the output of the prime mover, such as the rotational speed of the impeller or the blower driving a wind tunnel, or (alternatively) to vary the pressure drop in the tunnel, thereby varying the flow speed in the test section, despite nominally constant primemover revolutions per minute. The second method is used to keep the tunnel’s operating speed constant, as well as to move the test article in the streamwise direction, fore and aft (for example, via an electric linear motor), such that the relative freestream speed felt by the test article varies according to some waveform. Typically, the latter approach is chosen in water tunnels, where there is too much tunnel-circuit inertia to vary the flow speed directly but where the usually low tunnel test section flow speeds enable large excursions in the relative freestream by oscillation of the test article. In fact, outright reverse flow is possible by moving the test article in the laboratory frame at a higher speed than the water-tunnel flow speed. In either case, a sinusoidal relative-speed waveform is the most intuitively realizable, and this can be combined with similar oscillations in the airfoil incidence angle or other kinematics. Although the two methods of realizing streamwise oscillations are mechanically distinct, experimental comparisons between an oscillating test article in a water tunnel and a stationary test article in a wind tunnel with a louvermechanismhave demonstrated agreement in themeasured lift and drag histories. Such experimentswere performed by Granlund et al. for a 10% freestream amplitude oscillation and fixed airfoil incidence, comparing a free-surface water tunnel and a closed-circuit wind tunnel. After buoyancy was subtracted from the wind-tunnel data (resulting from the louver pressure drop) and the model inertia subtracted from the water-tunnel data (resulting from acceleration of the test article), the remaining lift and drag histories matched well at the low freestream oscillation amplitude regime. The work of Granlund et al. was later extended to high-advance-ratio streamwise oscillations of 50% amplitude by Greenblatt et al., where the aerodynamic histories of the water-tunnel and wind-tunnel facilities were compared in combined pitch and freestreamoscillations (governed by relative pitch phase), pure pitch oscillations, and purely freestream oscillations. Agreement between the two facilities’ data for fixed-incidence streamwise oscillations was reasonably good, and in fact, better than agreement in just the static lift and drag, evidently owing to differences in blockage and model-support systems. Additionally, Greenblatt et al. determined there was no strong coupling between simultaneous freestream oscillations and pitch oscillations on resultant lift and moment coefficients. KW - Wind energy KW - Dynamic stall KW - Deep stall KW - Airfoil surging KW - Airfoil pitching PY - 2018 DO - https://doi.org/10.2514/1.J056408 SN - 0001-1452 SN - 1533-385X VL - 56 IS - 4 SP - 1703 EP - 1709 PB - American Institute of Aeronautics and Astronautics AN - OPUS4-43994 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ruhe, L. A1 - Ickert, Stefanie A1 - Beck, S. A1 - Linscheid, M. W. T1 - A new strategy for metal labeling of glycan structures in antibodies JF - Anal. Bioanal. Chem. N2 - Quantitative analysis of complex proteins is a challenging task in modern bioanalytical chemistry. Commonly available isotope labels are still suffering from limitations and drawbacks, whereas new metal labels open numerous possibilities in mass spectrometric analyses. In this work, we have developed a newmetal labeling strategy to tag glycan structures of proteins, more particularly antibodies. The oligosaccharide glycans were selectively trimmed to the last N-acetylglucosamine to which an artificial azide containing galactose residue was bound. This azide can be used for subsequent cycloaddition of an alkyne. Therefore, we developed a lanthanide-containing macrocyclic reagent to selectively connect to this azido galactose. In summary, the glycan structures of an antibody can be labeled with a metal functionality using this approach. Furthermore, the functionality of the antibodies can be fully maintained by labeling the Fc glycans instead of using labeling reagents that target amino or thiol groups. This approach enables the possibility of using elemental, besides molecular mass spectrometry, for quantitative analyses or imaging experiments of antibodies in complex biological samples. KW - Antibody KW - Metal labeling KW - Glycans KW - DOTA KW - Lanthanide PY - 2018 DO - https://doi.org/10.1007/s00216-017-0683-1 SN - 1618-2650 SN - 1618-2642 VL - 410 IS - 1 SP - 21 EP - 25 PB - Springer AN - OPUS4-44000 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Zscherpel, Uwe A1 - Ewert, Uwe ED - Russo, Paolo T1 - Handbook of X-ray imaging: Physics and technology T2 - Series in Medical Physics and Biomedical Engineering N2 - Industrial Radiology is used for volumetric inspection of industrial objects. By penetration of these objects (typically weldments, pipes or castings) with X-ray or Gamma radiation the 3D-volume is projected onto a 2D image detector. The X-ray film is the oldest radiographic image detector and still in wide use in industry. The industrial X-ray film systems used today differ from these used in medicine. Medical film systems are described well in the literature, but industrial film systems not. So we start with a description of the properties and standards for industrial film systems. The requirements on image quality are defined by several standards and can be verified with different image quality indicators (IQIs). They describe the ability of the human being to detect small and low contrast indications in a noisy image background. The essential parameters for digital industrial radiology are described. Since about 30 years electronic image detectors are gradually replacing the industrial film. These detectors are based on storage phosphor imaging plates in combination with Laser scanners (“Computed Radiography”, CR) or a variety of different digital detector arrays (DDA). Typical applications of CR and DDAs are discussed as well as new possibilities by digital image processing, which is enabled by the computer based image handling, processing and analysis. KW - Industrial radiology KW - Industrial radiography KW - NDT films KW - Computed radiography KW - Digital detector arrays PY - 2018 SN - 978-1-4987-4152-1 SP - Chapter 30, 595 EP - 617 PB - CRC Press CY - Boca Raton, FL, USA AN - OPUS4-44026 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kothavale, S. A1 - Jadhav, A. G. A1 - Scholz, Norman A1 - Nirmalananthan-Budau, Nithiya A1 - Behnke, Thomas A1 - Resch-Genger, Ute A1 - Sekar, N. T1 - Corrigendum to "Deep red emitting triphenylamine based coumarin-rhodamine hybrids with large stokes shift and viscosity sensing: Synthesis, photophysical properties and DFT studies of their spirocyclic and open forms" [Dyes Pigments 137 (2017) 329-341] JF - Dyes and pigments N2 - We designed and synthesized triphenylamine based and coumarin fused rhodamine hybrid dyes and characterized using 1H, 13C NMR and HR-LCMS analysis. Both the newly synthesized hybrid dyes were found to show red shifted absorption as well as emissions and large Stokes shift (40e68 nm) as compared to the small Stokes shift (25e30 nm) of reported dyes Rhodamine B and 101. Photophysical properties of these dyes were studied in different solvents and according to the solvents acidity or basicity they preferred to remain in their spirocyclic or open form in different ratio. We studied the spirocyclic as well as open form derivatives of these dyes for their viscosity sensitivity in three different mixture of solvents i.e. polar-protic [EtOH-PEG 400], polar-aprotic [toluene-PEG 400] and non-polaraprotic [toluene-paraffin]. They are found to show very high viscosity sensitivity in polar-protic mixture of solvents [EtOH-PEG 400] and hence concluded that both polarity as well as viscosity factor worked together for the higher emission enhancement rather than only viscosity factor. As these dyes showed very high viscosity sensitivity in their spirocyclic as well as open form, they can be utilized as viscosity sensors in visible as well as deep red region. We also correlated our experimental finding theoretically by using Density Functional theory computations. KW - Dye KW - Fluorescence KW - Synthesis KW - Quantum yield KW - Lifetime KW - Coumarin KW - Rhodamine KW - Probe KW - Viscosity PY - 2018 DO - https://doi.org/10.1016/j.dyepig.2017.06.021 SN - 0143-7208 SN - 1873-3743 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. VL - 149 SP - 929 PB - Elsevier CY - Amsterdam AN - OPUS4-44038 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Griepentrog, Michael A1 - Hertwig, Andreas A1 - Weise, Matthias T1 - White light interference microscopy, ellipsometry, and instrumented indentation testing as reference procedures N2 - The paper addresses “WHITE LIGHT INTERFERENCE MICROSCOPY, ELLIPSOMETRY, AND INSTRUMENTED INDENTATION TESTING AS REFERENCE PROCEDURES“ and is subdivided in the following sections: 1. Measurement vs. testing vs. reference procedures, 2. White light interference microscopy (WLIM) for determination of step height h, 3. Spectroscopic ellipsometry (SE) for determination of layer thickness d and 4. Instrumented indentation testing (IIT) for determination of indentation hardness HIT. The following points are discussed in more detail: methodology of measurement and testing, uncertainty budgets for direct (WLIM), model-based (SE) and formula-based (IIT) reference procedures by means of specific examples. It is shown that standardization efforts are connected to reference procedures. T2 - Referenzverfahren CY - BAM, Berlin, Germany DA - 21.02.2018 KW - Reference procedures KW - Uncertainty budgets KW - White light interference microscopy KW - Spectroscopic ellipsometry KW - Instrumented indentation testing PY - 2018 AN - OPUS4-44256 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Hoffmann, Katrin A1 - Wegmann, Marc A1 - Hannemann, M. A1 - Somma, V. A1 - Jochum, T. A1 - Niehaus, J. A1 - Roggenbuck, D. T1 - Automated determination of genotoxicity of nanoparticles with DNA-based optical assays - The NANOGENOTOX project N2 - The overall interest in nanotoxicity, triggered by the increasing use of nanomaterials in the material and life sciences, and the synthesis of an ever increasing number of new functional nanoparticles calls for standardized test procedures1,2 and for efficient approaches to screen the potential genotoxicity of these materials. Aiming at the development of fast and easy to use, automated microscopic methods for the determination of the genotoxicity of different types of nanoparticles, we assess the potential of the fluorometric γH2AX assay for this purpose. This assay, which can be run on an automated microscopic detection system, relies on the detection of DNA double strand breaks as a sign for genotoxicity3. Here, we provide first results obtained with broadly used nanomaterials like CdSe/CdS and InP/ZnS quantum dots as well as iron oxide, gold, and polymer particles of different surface chemistry with previously tested colloidal stability and different cell lines like Hep-2 and 8E11 cells, which reveal a dependence of the genotoxicity on the chemical composition as well as the surface chemistry of these nanomaterials. These studies will be also used to establish nanomaterials as positive and negative genotoxicity controls or standards for assay performance validation for users of this fluorometric genotoxicity assay. In the future, after proper validation, this microscopic platform technology will be expanded to other typical toxicity assays. T2 - SPIE 2018 CY - San Francisco, USA DA - 27.01.2018 KW - Nanoparticle KW - Fluorescence KW - Surface chemistry KW - Size KW - Assay KW - Microscopy KW - Nanotoxicity KW - Toxicity KW - Automation KW - Calibration KW - Standard PY - 2018 AN - OPUS4-44186 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Swaraj, Sufal A1 - Müller, Anja A1 - Sparnacci, Katia A1 - Unger, Wolfgang T1 - Core-shell nanoparticles investigated with scanning transmission X-ray microscopy N2 - A scanning transmission x-ray microscopy (STXM) based methodology is introduced for determining the dimensions (shell thickness, core and total diameter) of core-shell nanoparticles which exhibit a strong x-ray absorption contrast and a sharp interface between core and shell material. A low radiation dosage during data acquisition and, therefore, less x-ray beam induced damage of the sample is achieved by recording STXM images only at two predetermined energies of maximum absorption contrast instead of recording a stack of images across the whole absorption edge. A model core-shell nanoparticle, polytetrafluoroethylene (PTFE) cores with polystyrene (PS) shell, investigated at the HERMES beamline is presented for demonstration. This STXM based methodology yields particle dimensions in good agreement with the scanning electron microscopy (SEM) results (deviation equal or less than 10%). Extension of this methodology to core-shell nanoparticles with inorganic core and organic shell will also be presented and the challenges encountered will be highlighted. T2 - 13th SOLEIL Users' Meeting CY - Saint-Aubin, France DA - 18.01.2018 KW - STXM KW - SEM KW - PTFE KW - PS KW - Core-shell nanoparticles KW - Polymers PY - 2018 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-43883 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Hertwig, Andreas A1 - Winkler, J. T1 - Preliminary work item (PWI) 23131 on standardization of ellipsometry N2 - The paper addresses the PRELIMINARY WORK ITEM (PWI) 23131 ON STANDARDIZATION OF ELLIPSOMETRY and the following points are discussed in more detail: Historical background of ellipsometry, Technical/industrial importance of ellipsometry and Standardization activities on ellipsometry. T2 - ISO TC 107 and JWG 4 meeting CY - Levi, Finland DA - 23.01.2018 KW - Standardization KW - Ellipsometrie KW - Modelling KW - Accreditation PY - 2018 AN - OPUS4-43959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute ED - Wang, Cui ED - Otto, S. ED - Dorn, M. ED - Kreidt, E. ED - Lebon, J. ED - Srsan, L. ED - di Martino-Fumo, P. ED - Gerhards, M. ED - Seitz, M. ED - Heinze, K. T1 - Deuterated Molecular Ruby with Record Luminescence Quantum Yield JF - GDCh N2 - The recently reported luminescent chromium(III) complex 13+ ([Cr(ddpd)2]3+; ddpd=N,N’-dimethyl-N,N’-dipyridine-2-yl-pyridine-2,6-diamine) shows exceptionally strong near-IR emission at 775 nm in water under ambient conditions (F=11%) with a microsecond lifetime as the ligand design in 13+ effectively eliminates non-radiative decay pathways, such as photosubstitution, back-intersystem crossing, and trigonal twists. In the absence of energy acceptors, such as dioxygen, the remaining decay pathways are energy transfer to high energy solvent and ligand oscillators, namely OH and CH stretching vibrations. Selective deuteration of the solvents and the ddpd ligands probes the efficiency of these oscillators in the excited state deactivation. Addressing these energytransfer pathways in the first and second coordination sphere furnishes a record 30% quantum yield and a 2.3 millisecond lifetime for a metal complex with an earth-abundant metal ion in solution at room temperature. KW - Fluorescence KW - Quantum yield KW - Ligand design KW - Cr(III) KW - Complex KW - Oxygen sensor KW - NIR KW - Fluorescence lifetime PY - 2018 DO - https://doi.org/10.1002/ange.201711350 SN - 1521-3773 VL - 57 IS - 4 SP - 1112 EP - 1116 PB - Wiley-VCH Verlag & Co. KGaA CY - Weinheim AN - OPUS4-44045 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Taparli, Ugur Alp A1 - Griesche, Axel A1 - Kannengießer, Thomas A1 - Jacobsen, Lars A1 - Michalik, Katarzyna A1 - Mory, David T1 - In situ laser-induced breakdown spectroscopy measurements in stainless steels during TIG welding N2 - Chemical composition of the welding seam and HAZ has significant effect on weld quality. Current inspection methods for weld seams measure and investigate post factum and cannot prevent weld defects. Element burn-off may significantly affect solidification leading to embrittlement or cracking Control of weld chemical compositions insures a controlled solidification and resistance to related weld defects. A prototype of a LIBS controlled welding process is presented. T2 - Forschungsseminar Universität Magdeburg CY - Magdeburg, Germany DA - 17.01.2018 KW - LIBS KW - TIG-Welding KW - Chemical compositions KW - In situ measurements PY - 2018 AN - OPUS4-43830 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zorn, R. A1 - Yin, Huajie A1 - Lohstroh, W. A1 - Harrison, W. A1 - Budd, P.M. A1 - Pauw, Brian Richard A1 - Böhning, Martin A1 - Schönhals, Andreas T1 - Anomalies in the low frequency vibrational density of states for a polymer with intrinsic microporosity - the Boson peak of PIM-1 JF - Physical Chemistry Chemical Physics N2 - Polymers with intrinsic microporosity are promising candidates for the active separation layer in gas separation membranes. Here, the vibrational density of states (VDOS) for PIM-1, the prototypical polymer with intrinsic microporosity, is investigated by means of inelastic neutron scattering. The results are compared to data measured for a more conventional high-performance polyimide used in gas separation membranes (Matrimid). The measured data show the characteristic low frequency excess contribution to VDOS above the Debye sound wave level, generally known as the Boson peak in glass-forming materials. In comparison to the Boson peak of Matrimid, that of PIM-1 is shifted to lower frequencies. This shift is discussed considering the microporous, sponge-like structure of PIM-1 as providing a higher compressibility at the molecular scale than for conventional polymers. For an annealed PIM-1 sample, the Boson peak shifts to higher frequencies in comparison to the un-annealed sample. These changes in the VDOS of the annealed PIM-1 sample are related to changes in the microporous structure as confirmed by X-ray scattering. KW - Polymers KW - Boson peak KW - Neutron scattering KW - Physical aging KW - Polymer of intrinsic microporosity PY - 2018 DO - https://doi.org/10.1039/C7CP07141H SN - 1463-9076 SN - 1463-9084 VL - 20 IS - 3 SP - 1355 EP - 1363 PB - The Royal Society of Chemistry AN - OPUS4-43808 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Falkenhagen, Jana T1 - Characterization of co (polyamide)s N2 - Charactrization of Co(polyamide)s Molar mass distribution; Functionalization; supression of end group effects in favor of sequence distribution analysis; Evidence of of randomization with increasing reaction time T2 - Polyamide Meeting, DSM CY - Sittard, The Netherlands DA - 20.04.2018 KW - Liquid chromatography KW - Mass spectrometry of polymers PY - 2018 AN - OPUS4-44747 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - THES A1 - Sobol, Oded T1 - Hydrogen assisted cracking and transport studied by ToF-SIMS and data fusion with HR-SEM T2 - BAM-Dissertationsreihe N2 - For almost 150 years it is known that hydrogen has a deleterious effect on the mechanical properties of metallic components. Nowadays, the problem of hydrogen assisted degradation is highly relevant in energy related fields due to the massive use of steel as a structural component in these applications and its sensitivity to hydrogen. Since the discovery of hydrogen assisted cracking (HAC), researchers studied intensively and suggested possible explanations and mechanisms in order to define how hydrogen is affecting the material. In general, it is considered that hydrogen changes the mechanical properties more in terms of ductility (deformation capacities) than in strength (load capacities). Hydrogen concentration is one of three crucial factors in the degradation process, together with the microstructure of the material and the internal/external mechanical load. The relatively high concentration of hydrogen resulting in this loss of ductility can originate during production or before service (e.g. welding processes) and during service (i.e. catholically protected systems to eliminate corrosion processes in sour environments). In parallel to the theoretical work, tremendous efforts were, and are still, invested in searching for a proper method to elucidate, map and quantify the hydrogen in the microstructure, which is the basis for this work. For steels, the focus is mainly on the observations of diffusion processes and the interaction of hydrogen with the microstructure in regions with high local stresses/strains (for example around evolving cracks). The challenge for reaching this goal arises from the fact that accurate indication of hydrogen by means of position, unlike heavier atoms, can be made only by mass spectrometry or by interaction with another element (e.g. silver decoration, special coating and resonant nuclear reaction by nitrogen). In addition to this, the difficulty recording the hydrogen behavior while it rapidly diffuses through the material, leaving only the unpredicted failure, should be taken into account. Although using powerful characterization methods, models and computational simulations, the key to defining the mechanisms behind HAC is still under debate and not fully understood. The relationship between material and hydrogen is determined by three factors, i.e., the material structure and microstructure – determining the physical properties, the mechanical load applied on the material and the hydrogen concentration. It is well known that in order to have a complete definition of HAC these three factors must be examined locally with the minimal scale and the maximal resolution reachable. The major gap is the lack in such a characterization method or a technique by which one has the ability to detect and observe the hydrogen in the metallic microstructure. The commonly used techniques nowadays are capable of characterization of the microstructure without the ability to observe the hydrogen distribution. Global hydrogen concentration and localized hydrogen observation are possible by some techniques which are incapable of indicating a change in the structure or microstructure therefore a comprehensive overview can be gained only by combining several methods. In the presented research, secondary ion mass spectrometry (SIMS) was adopted as the main tool to detect and locally map the hydrogen distribution in two types of duplex stainless steel grades: EN 1.4462 (standard 2205 duplex stainless steel) and EN 1.4162 (2101 lean duplex stainless steel). The term duplex stainless steel (DSS) refers to the austenitic-ferritic microstructure of the steel where the combination of physical and mechanical properties of the two phases is achieved. The DSS was selected as a case study for this work due to the wide use of this grade in many energy and the lack of knowledge on hydrogen behavior in two-phase containing microstructures. ToFSIMS was exploited in-situ and ex-situ in three experimental approaches during or following an electrochemical charging procedure. This type of hydrogen charging was selected as it simulated a procedure of cathodic protection of most sub-water oil and gas extraction and delivery systems. The experimental procedures were: 1. Ex-situ charging followed by ToF-SIMS imaging for basic understanding of hydrogen distribution. 2. Ex-situ charging followed by in-situ mechanical loading to obtain information on hydrogen behavior around a propagating crack. 3. In-situ permeation of hydrogen through a steel membrane inside the ToF-SIMS to obtain information on diffusion behavior of hydrogen in a two-phase microstructure. The comprehensive view of the effect of hydrogen on steel was gained by using supplementary methods, such as high resolution scanning electron microscopy (HR-SEM), focused ion beam (FIB) and electron back-scattered diffraction (EBSD). The state of the art in this work lies in applying both: in-situ experimental approaches and data treatment of the ToF-SIMS raw data. The data treatment includes the combination of data from several sources (data fusion). The results for the ex-situ charging followed by static sample imaging and data fusion showed that when the analyzed surface is directly exposed to the electrolyte the degradation is pronounced differently in the ferrite, austenite and interface. The degradation mechanisms in the ferrite and austenite were reflected by the formation of cracks on the surface of both, where a high concentration of hydrogen was obtained. This result supports the assumption that hydrogen is attracted to highly deformed regions. The advantage of using in-situ charging/permeation in comparison to ex-situ charging is that the effect of hydrogen on the ferrite and austenite phases when the hydrogen is evolving from within the microstructure is realized, in comparison to when the analyzed surface is initially exposed directly to the electrolyte. In both experiments the ferrite was observed as a fast diffusion path for the hydrogen. The faster diffusion of hydrogen through the ferrite is expected due to the higher diffusion coefficient, however, a direct proof for the diffusion sequence in this scale was never shown. Most significant results were achieved by the ‘core’ experiments of this research. These experiments included the design of a novel dynamic mechanical loading device to apply an external load during SIMS imaging of a hydrogen precharged-notched sample. For the first time it was shown that plastic deformation induced by applying a mechanical load is resulting in a redistribution of hydrogen locally around the notch. T3 - BAM Dissertationsreihe - 160 KW - Duplex stainless steels KW - Hydrogen assisted cracking KW - Time-of-Flight secondary ion mass spectrometry KW - Data fusion PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-447331 SN - 1613-4249 VL - 160 SP - I EP - 180 PB - Bundesanstalt für Materialforschung und -prüfung (BAM) CY - Berlin AN - OPUS4-44733 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steger, Simon A1 - Hahn, Oliver T1 - Development of a methodical approach for in-situ analysis of modern reverse paintings on glass N2 - The technique of painting on the reverse side of glass was rediscovered by artists in the early 20th century and gained great popularity, especially in Germany. In contrast to other paint techniques (e.g. panel and mural painting), the paint layers are applied in reverse succession starting with the foremost paint layer and ending with the primer (backmost layer). The paintings are viewed in reflected light, thus revealing an impressive gloss, luminosity and depth of colour. Scientific investigation of the material provides important information for appropriate conservation concepts. Transport of the precious and fragile objects to the lab is often not feasible. Therefore, in-situ, non-invasive analysis is necessary to analyse colorants and binders. However, some analytical problems need to be considered: due to the reverse paint stratigraphy in reverse paintings on glass, the measured layer is always the backmost one. The analytical possibilities are extremely reduced, when the back is covered by a metal foil (or by paper, carton etc.). However, measurements through the glass (using Raman and VIS) can still yield information on the colourants of the front layer. When the paint layer is accessible, we start our procedure using X-ray fluorescence (Tracer III-SD, Bruker AXS Microanalysis GmbH, 40 kV, 15 μA) and VIS reflectance spectroscopy (SPM 100, Gretag-Imaging AG). Both techniques provide first information on the inorganic colourants. Raman measurements (i-Raman®Plus, Bwtek inc., 785 nm, 50× objective, resolution 4 cm-1) are then carried out to clarify uncertain XRF measurements and to identify synthetic organic pigments (SOP). Diffuse Reflection-Infrared-Fourier-Transform Spectroscopy (DRIFTS; ExoScan, Agilent GmbH, 4000–650 cm-1, 500 scans, spectral resolution 4 cm-1) is used for the classification of the binders. Moreover, it may help to identify SOP, when fluorescence dominates the Raman signal. This analytical sequence yields the best results, when time is the limiting factor. We present two in-situ studies of the paintings “Kreuzabnahme” (1914-15) by Carlo Mense and “Stadt am Morgen” (1921) by Walter Dexel. The painting “Kreuzabnahme” is an outstanding piece in Mense’s ɶuvre, because the glass plate was painted on both sides (Fig. 1). The results of the back-side show mainly inorganic pigments: basic lead white, talc, red and brown ochre, cinnabar, chrome yellow, viridian, ultramarine blue, Prussian blue and bone black. The classification of binding media using DRIFTS yields positive results for drying oil. Acrylic resin could be identified in two areas, resulting from a previous restauration treatment. For the front side painting, Mense used basic lead white, cinnabar, chrome yellow and umbra as pigments and oil as binder. Measurements of the abstract painting “Stadt am Morgen” by Walter Dexel show zinc white, basic lead white, chalk, cinnabar, red lead, strontium yellow, cadmium yellow, cobalt blue, Prussian blue, ultramarine blue, brown ochre and bone black as pigments. Moreover, synthetic alizarin (PR83) was identified as dark red colorant. The results of DRIFTS classify oil as binding media. We conclude that, the use of complementary spectroscopic methods yields the best results for in-situ analysis of reverse paintings on glass. T2 - 3rd International Conference on Innovation in Art Research and Technology CY - Parma, Italy DA - 26.03.2018 KW - Modern painting KW - Non invasive analysis KW - Raman spectroscopy PY - 2018 AN - OPUS4-44780 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heinrich, Thomas A1 - Sparnacci, K. A1 - Unger, Wolfgang A1 - Schneider, Markus A1 - Müller, Anja T1 - Chemical Analysis of Core-Shell Nanoparticles using ToF-SIMS and XPS N2 - The analysis of nanomaterials is current an important task - especially in case of risk assessment, as the properties of these material class are not well understood currently. The rather high surface area of these objects renders their interactions significantly different to their corresponding bulk. Thus, the surfaces chemical composition has to be investigated to get a better understanding and prediction of the nanomaterials' behavior. ToF-SIMS has proven as a powerful tool to determine said chemical composition. Its superior surface sensitivity allows us to study mainly the utmost atomic layer and therefore gives us an idea of the interactions involved. Here, we show first result from the validation of the method for the analysis of polystyrene and gold nanoparticles. ToF-SIMS will be compared to other methods like XPS, T-SEM or REM. Furthermore, principle component analysis (PCA) will be used to detect the influence of different sample preparation performed by an innovative microfluidic device. ToF-SIMS imaging is desired to be implemented for single particle detection as well. T2 - DPG-Frühjahrstagung der Sektion Kondensierte Materie gemeinsam mit der EPS CY - Berlin, Germany DA - 11.03.2018 KW - XPS KW - ToF-SIMS KW - Nanoparticles PY - 2018 N1 - Geburtsname von Müller, Anja: Hermanns, A. - Birth name of Müller, Anja: Hermanns, A. AN - OPUS4-44790 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Schumacher, David A1 - Meyendorf, N. A1 - Hakim, I. A1 - Ewert, Uwe ED - Chimenti, D. E. ED - Bond, L. J. T1 - Defect recognition in CFRP components using various NDT methods within a smart manufacturing process T2 - AIP Conference Proceedings N2 - The manufacturing process of carbon fiber reinforced polymer (CFRP) components is gaining a more and more significant role when looking at the increasing amount of CFRPs used in industries today. The monitoring of the manufacturing process and hence the reliability of the manufactured products, is one of the major challenges we need to face in the near future. Common defects which arise during manufacturing process are e.g. porosity and voids which may lead to delaminations during operation and under load. To find irregularities and classify them as possible defects in an early stage of the manufacturing process is of high importance for the safety and reliability of the finished products, as well as of significant impact from an economical point of view. In this study we compare various NDT methods which were applied to similar CFRP laminate samples in order to detect and characterize regions of defective volume. Besides ultrasound, thermography and eddy current, different X-ray methods like radiography, laminography and computed tomography are used to investigate the samples. These methods are compared with the intention to evaluate their capability to reliably detect and characterize defective volume. Beyond the detection and evaluation of defects, we also investigate possibilities to combine various NDT methods within a smart manufacturing process in which the decision which method shall be applied is inherent within the process. Is it possible to design an in-line or at-line testing process which can recognize defects reliably and reduce testing time and costs? This study aims to show up opportunities of designing a smart NDT process synchronized to the production based on the concepts of smart production (Industry 4.0). A set of defective CFRP laminate samples and different NDT methods were used to demonstrate how effective defects are recognized and how communication between interconnected NDT sensors and the manufacturing process could be organized. T2 - 44TH ANNUAL REVIEW OF PROGRESS IN QUANTITATIVE NONDESTRUCTIVE EVALUATION CY - Provo, Utah, USA DA - 16.07.2017 KW - Carbon fiber reinforced polymers KW - Non-destructive testing KW - Smart industry (4.0) KW - Ultrasound KW - Laminography KW - Serial sectioning KW - Computed tompgraphy PY - 2018 SN - 978-0-7354-1644-4 DO - https://doi.org/10.1063/1.5031521 SN - 0094-243X VL - 1949 SP - UNSP 020024, 1 EP - 11 PB - AIP Publishing AN - OPUS4-44773 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nirmalananthan-Budau, Nithiya A1 - Moser, Marko A1 - Behnke, Thomas A1 - Geißler, Daniel A1 - Resch-Genger, Ute T1 - Multimodal cleavable reporters for the optical quantification of functional groups on nano- and microparticles N2 - Nano- and microparticles are of increasing importance for a wide range of applications in the material and life sciences. Examples are their use as carriers for dye molecules and drugs, multichromophoric reporters for signal enhancement strategies in optical assays, targeted probes for bioimaging, and biosensors. All these applications require surface functionalization of the particles with e.g., ligands (to tune the dispersibility and prevent unspecific interactions), crosslinkers, sensor dyes, or analyte recognition moieties like biomolecules, and subsequently, the knowledge of the chemical nature and total number of surface groups as well as the number of groups accessible for coupling reactions. Particularly attractive for the latter are sensitive and fast photometric or fluorometric assays, which can be read out with simple, inexpensive instrumentation. Here, we present a novel family of cleavable photometric and multimodal reporters for the quantification of conjugatable amino and carboxyl surface groups on nano- and microparticles. These probes allow for the determination of particle-bound labels, unbound reporters in the supernatant, and reporters cleaved off from the particle surface as well as the remaining thiol groups on the particles by photometry and inductively coupled optical emission spectrometry (32S ICP-OES).3 Comparison of the performance of these cleavable reporters with conventional labels, utilizing changes in intensity and/or colour of absorption and/or emission, underlines the analytical potential of this versatile concept which elegantly circumvents signal distortions by light scattering and encoding dyes, and enables straightforward validation by method comparison. T2 - INNANOPART Open day CY - London, UK DA - 24.04.2018 KW - Nanoparticle KW - Surface groups KW - Cleavable reporter PY - 2018 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-44828 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Moser, Marko A1 - Nirmalananthan-Budau, Nithiya A1 - Behnke, Thomas A1 - Geißler, Daniel A1 - Resch-Genger, Ute T1 - Multimodal cleavable reporters versus conventional labels for optical quantification of accessible amino and carboxy groups on nano- and microparticles JF - Analytical chemistry N2 - Many applications of nanometer- and micrometer-sized particles include their surface functionalization with linkers, sensor molecules, and analyte recognition moieties like (bio)ligands. This requires knowledge of the chemical nature and number of surface groups accessible for subsequent coupling reactions. Particularly attractive for the quantification of these groups are spectrophotometric and fluorometric assays, which can be read out with simple instrumentation. In this respect, we present here a novel Family of cleavable spectrophotometric and multimodal reporters for conjugatable amino and carboxyl surface groups on nano- and microparticles. This allows determination of particle-bound labels, unbound reporters in the supernatant, and reporters cleaved off from the particle surface, as well as the remaining thiol groups on particle, by spectrophotometry and inductively coupled optical emission spectrometry (32S ICP-OES). Comparison of the performance of these cleavable reporters with conductometry and conventional labels, utilizing changes in intensity or Color of absorption or emission, underlines the analytical potential of this versatile concept which elegantly circumvents Signal distortions by scattering and Encoding dyes and enables straightforward validation by method comparison. KW - Polymer particles KW - Cleavable reporter KW - Optical quantification KW - Validation PY - 2018 DO - https://doi.org/10.1021/acs.analchem.8b00666 SN - 1520-6882 SN - 0003-2700 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. VL - 90 IS - 9 SP - 5887 EP - 5895 PB - ACS Publ. CY - Washington, DC AN - OPUS4-44830 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weidner, Steffen A1 - Kricheldorf, H. A1 - Scheliga, F. T1 - Cyclic polylactides via ring-expansion polymerization N2 - We will report on a new kind of ring-expansion polymerization (REP) of cyclic esters based of three classes of catalysts. In contrast to REP described previously these new polymerizations are characterized by a self-extrusion of the catalysts resulting in cyclic homopolyesters as the only reaction product. These REP of L-lactide were performed in bulk at temperatures between 100 and 180°C without racemization. A simplified scheme of a REP catalyzed by BuCa or SnBi is presented below. With meso-lactide temperatures down to 60°C were realized. Depending on catalyst, time and temperature with equal quantities of even and odd-numbered cycles a strong predominance of either even or odd-numbered cycles was found. T2 - 255th ACS National Meeting CY - New Orleans, LA, USA DA - 18.03.2018 KW - MALDI-TOF MS KW - Poly(lactide) KW - Polymerisation KW - Catalysts PY - 2018 AN - OPUS4-44833 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geißler, Daniel A1 - Nirmalananthan-Budau, Nithiya A1 - Moser, Marko A1 - Resch-Genger, Ute T1 - Synthesis of polymeric nanobeads with different surface group densities and their charaterization using multimodal cleavable reporters and lanthanide tags N2 - Polymeric nanoparticles (NP) are of increasing importance for a wide range of applications in the material and life sciences, including their use as drug carriers, fluorescent sensors and multimodal reporters in a large variety of bioassays and bioimaging studies. Application-relevant properties of NP include their size (and size distribution), shape, optical properties, and ease of subsequent functionalization, e.g. with linkers, sensor molecules, and bioligands. In this respect, knowledge of the chemical nature, the total number of surface groups and the number of groups accessible for subsequent coupling reactions is mandatory.1 Commercially available polystyrene NP often contain different additives like stabilizers, radical starters and crosslinkers, which can influence the quantification of surface functionalities. Moreover, they often have unknown surface group densities that may vary from batch to batch, which complicates or even hampers their reliable use in many (bio)applications. To circumvent these issues, we synthesized amino- and carboxy-functionalized, monodisperse 100 nm polystyrene NP with three different, well-defined surface group densities. Using a recently developed approach for the quantification of functional groups on nano- and microparticles with cleavable reporters,2 we quantified the assessible functional groups on the self-synthesised PS particles via optical spectroscopy (photometry) and inductively coupled optical emission spectrometry (32S ICP-OES). In addition, we developed a fluorimetric approach for the quantification of surface functional groups on nanoparticles based on the labelling with luminescent lanthanide complexes (LLC). In contrast to common organic dyes, LLC are not prone to photo¬luminescence quenching arising from reabsorption or dye aggregation, and thus, enable a reliable fluorometric quantification of the assessible functional groups on NP surfaces. Moreover, lanthanide tags can be detected with high specificity and sensitivity with analytical techniques such as XPS and ICP-MS, which allow for the multimodal validation of the fluorometric quantification approach. T2 - RSC-NPL Symposium "Nanoparticle concentration – critical needs and state-of-the-art measurement" and EMPIR 14IND12 Innanopart Open Day CY - London, UK DA - 24.05.2018 KW - Nanoparticle KW - Functional group KW - Quantification PY - 2018 N1 - Geburtsname von Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. - Birth name of Nirmalananthan-Budau, Nithiya: Nirmalananthan, N. AN - OPUS4-44836 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan A1 - Mielke, Johannes A1 - Dohányosová, P. A1 - Müller, P. A1 - López-Vidal, S. T1 - Controlled deposition of nanoparticles by electrospray for improved analysis by imaging techniques N2 - Of many experimental techniques for measuring particle sizes and size distributions, electron microscopy (EM) is still considered as the gold standard, especially in the nano range (1–100 nm). Furthermore, high-resolution X-ray spectroscopy (EDX) in conjunction with EM can be applied to individual NPs. Preparation of an EM sample for generic particulate materials is a difficult task. Usually the particles in a suspension are deposited on a support. However, this procedure includes the drying of larger solvent amounts on the substrate itself, and this can affect the spatial distribution of the deposited particles. One possibility to overcome this is the use of an electrospray system, where the suspension of particles is sprayed onto the substrate in charged droplets that are so small that they either dry off on the substrate immediately without affecting the position of particles, or even already during their flight time to the substrate. Additionally, the charging of particles minimizes agglomeration and aggregation, maximizing the collection of the EM grids. The prototype of an electrospray deposition system from RAMEM under its trademark IONER (www.ioner.eu) was tested. Electrospray is theoretically described since a long time, but no dedicated commercial instruments are available for the preparation of TEM grids yet, apart from electrostatic deposition of aerosols.2 Several materials have been sprayed onto TEM grids and the resulting particle distributions were evaluated. Operation parameters such as the sample flow-rate, capillary – substrate distance, electric field strength and sampling period length have been optimized. It was found that the particles deposited by electrospray generally show a much more homogeneous spatial distribution on the substrate and a substantial increase of the number of single particles (suited to automatic analysis). T2 - RSC-NPL Symposium: Nanoparticle concentration – critical needs and state-of-the-art measurement CY - London, UK DA - 24.04.2018 KW - Electrospray deposition KW - Nanoparticles KW - Electron microscopy PY - 2018 AN - OPUS4-44802 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Hodoroaba, Vasile-Dan T1 - Lessons on measurement of nanoparticle size and shape learnt from NanoDefine N2 - The EC Recommendation on the definition of nanomaterial1, based solely on size of the constituent particles, foresees development of harmonised measurement methods ensuring ‘consistent results across materials and over time’. The EU/FP7 large research project NanoDefine (http://www.nanodefine.eu) has been exclusively dedicated to support the implementation of this EC Recommendation for the European Union’s legislation. For the first time, measurement techniques able to determine the size of nanoparticles have been evaluated systematically on a well-defined set of quality control materials (spherical, monodisperse) as well as industrial materials of complex shapes and considerable polydispersity. Particularly based on the analytical performance of the measurement techniques as tested on the challenging real-world particulate materials, it was possible to formulate recommendations for use of a new tiered approach consisting of screening and confirmatory techniques. Thus, a consistent framework of guidance for nanomaterial identification according to the EC Definition has been issued in form of the NanoDefiner e-tool (https://labs.inf.fh-dortmund.de/NanoDefiner), with a transparent decision flow scheme and an extensive user manual. Selected examples of analysis and classification as nano-/non-nanomaterials will be given, highlighting the limits of applicability of the available measurement techniques in dependence on sample properties. On some recent relevant developments in sample preparation – as a crucial part for an accurate analysis - will be also reported. T2 - RSC-NPL Symposium: Nanoparticle concentration – critical needs and state-of-the-art measurement CY - London, UK DA - 24.04.2018 KW - Nanoparticles KW - Nanomaterial KW - Particle size distribution KW - EU definition of nanomaterial PY - 2018 AN - OPUS4-44804 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Streeck, C. A1 - Wirth, Thomas A1 - Unger, Wolfgang A1 - Beckhoff, B. T1 - Qualifying calibration samples for advanced thin film materials characterisation JF - SPECTROSCOPY EUROPE N2 - In this article the question of the certification of calibration samples for the characterisation of advanced thin film materials is addressed within the framework of reliable process control or quality management purposes. Reference measurement techniques can be used in order to address the gap in appropriate certified reference materials (CRMs) for thin film analyses. They allow for qualifying out-of-production samples originating from an operating production line as calibration samples. As a template for this procedure, CIGS [Cu(In,Ga)Se2] layers, that are absorber layers for high efficiency thin-film solar cells, have been used for establishing and validating reference-free X-ray fluorescence (XRF) analysis and Auger-electron spectroscopy (AES) as reference measurement techniques. The focus was on determining the average mole fractions in the CIGS layers obtaining results traceable to the SI unit system. Reference-free XRF is physically traceable and is based upon radiometrically calibrated instrumentation and knowledge of atomic fundamental data. Sputter-assisted AES can be established as a chemically traceable method after careful calibration using a certified reference material (CRM) based on a total number counting method. KW - CIGS KW - X-ray fluorescence (XRF) KW - Auger-electron spectroscopy (AES) PY - 2018 UR - https://www.spectroscopyeurope.com/article/qualifying-calibration-samples-advanced-thin-film-materials-characterisation VL - 30 IS - 1 SP - 11 EP - 14 PB - John Wiley & Sons Ltd CY - Chichester, West Sussex PO19 8SQ, UK AN - OPUS4-44260 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nagli, L. A1 - Gaft, M. A1 - Raichlin, Y. A1 - Gornushkin, Igor B. T1 - Cascade generation in Al laser induced plasma JF - Optics Communications N2 - We found cascade IR generation in Al laser induced plasma. This generation includes doublet transitions 3s25s 2S1∕2→ 3s24p 2P1∕2,3∕2 → 3s24s 2S1∕2; corresponding to strong lines at 2110 and 2117 nm, and much weaker lines at 1312–1315 nm. The 3s25s2S 1∕2 starting IR generation level is directly pumped from the 3s23p 2P3∕2 ground level. The starting level for UV generation at 396.2 nm (transitions 3s24s 2S1∕2 → 4p 2P3∕2) is populated due to the fast collisional processes in the plasma plume. These differences led to different time and special dependences on the lasing in the IR and UV spectral range within the aluminum laser induced plasma. KW - Plasma diagnostics KW - Laser induced plasma KW - LIBS KW - Plasma modeling PY - 2018 DO - https://doi.org/10.1016/j.optcom.2018.01.041 VL - 415 SP - 127 EP - 129 PB - Elsevier B.V. AN - OPUS4-44274 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Makowski, Maike A1 - Werneburg, Martina A1 - Jung, Christian A1 - Haase, H. A1 - Koch, Matthias T1 - Non-invasive Cereal Analysis by GC-MS detection of Trichodiene as a Volatile Mycotoxin Biomarker N2 - Due to the increasing consumption of cereals worldwide, the monitoring of growth, storage and processing is becoming more and more crucial. Particularly when stored, infested grains breed fungal clusters (“hot spots”) in which mycotoxins greatly exceed allowed maximum levels. Because of their unpredictable presence, current sample drawing and procedures for mycotoxin analysis represent a complex challenge for operators, involving invasive and cost intensive steps. Therefore, new time- and labour-saving mycotoxin control methods including sampling and analysis steps are needed. A possible approach is the non-invasive analysis of the homogeneous gas phase above the crops, instead of analyzing random samples. However, this procedure requires microbial volatile organic compounds (MVOC´s) being released by the samples and representing the present mycotoxins. Previous investigations revealed trichodiene to be a precursor in trichothecenes biosynthesis – one of the largest mycotoxin groups with over 180 compounds. Due to its non-functionalized sesquiterpene structure, trichodiene has already been quantified using Headspace GC-MS methods (for instance]). Thereby, it can possibly be used as a biomarker for trichothecene contamination in foodstuff. However, further investigations are necessary. The correlation between trichodiene concentration in the gas phase and trichothecenes mass fraction in the sample must be examined closely to draw conclusions about the exact trichothecene content within samples. Realizing this idea, would widely extend the applicability of trichodiene and enormously simplify trichothecene quantification. Hence, this first step of an ongoing study aims to develop a laboratory reference method using trichodiene as volatile biomarker to quantify trichothecenes in cereals. Static headspace and SPME-enrichment coupled to gas chromatography with mass spectrometry (GC-MS) were employed. In a second step, this reference method is intended to validate new approaches for fast on-site screening of trichodiene in cereals. T2 - 10th World Mycotoxin Forum Conference CY - Amsterdam, The Netherlands DA - 11.03.2018 KW - Trichodiene KW - GC-MS KW - Mycotoxin Biomarker PY - 2018 AN - OPUS4-44508 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Makowski, Maike A1 - Jung, Christian A1 - Werneburg, Martina A1 - Haase, H. A1 - Koch, Matthias T1 - Non-invasive Cereal Analysis by GC-MS detection of Trichodiene as a Volatile Mycotoxin Biomarker N2 - Due to the increasing consumption of cereals worldwide, the monitoring of growth, storage and processing is becoming more and more crucial. Particularly when stored, infested grains breed fungal clusters (“hot spots”) in which mycotoxins greatly exceed allowed maximum levels. Because of their unpredictable presence, current sample drawing and procedures for mycotoxin analysis represent a complex challenge for operators, involving invasive and cost intensive steps. Therefore, new time- and labour-saving mycotoxin control methods including sampling and analysis steps are needed. A possible approach is the non-invasive analysis of the homogeneous gas phase above the crops, instead of analyzing random samples. However, this procedure requires microbial volatile organic compounds (MVOC´s) being released by the samples and representing the present mycotoxins. Previous investigations revealed trichodiene to be a precursor in trichothecenes biosynthesis – one of the largest mycotoxin groups with over 180 compounds. Due to its non-functionalized sesquiterpene structure, trichodiene has already been quantified using Headspace GC-MS methods (for instance). Thereby, it can possibly be used as a biomarker for trichothecene contamination in foodstuff. However, further investigations are necessary. The correlation between trichodiene concentration in the gas phase and trichothecenes mass fraction in the sample must be examined closely to draw conclusions about the exact trichothecene content within samples. Realizing this idea, would widely extend the applicability of trichodiene and enormously simplify trichothecene quantification. Hence, this first step of an ongoing study aims to develop a laboratory reference method using trichodiene as volatile biomarker to quantify trichothecenes in cereals. Static headspace and SPME-enrichment coupled to gas chromatography with mass spectrometry (GC-MS) were employed. In a second step, this reference method is intended to validate new approaches for fast on-site screening of trichodiene in cereals. T2 - 10th World Mycotoxin Forum Conference CY - Amsterdam, The Netherlands DA - 11.03.2018 KW - Trichodiene KW - GC-MS KW - Mycotoxin Biomarker PY - 2018 AN - OPUS4-44509 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Titschack, J. A1 - Baum, D. A1 - Matsuyama, K. A1 - Boos, K. A1 - Färber, C. A1 - Kahl, W.-A. A1 - Ehrig, Karsten A1 - Meinel, Dietmar A1 - Soriano, C. A1 - Stock, S.R. T1 - Ambient occlusion – A powerful algorithm to segment shell and skeletal intrapores in computed tomography data JF - Computers and Geosciences N2 - During the last decades, X-ray (micro-)computed tomography has gained increasing attention for the description of porous skeletal and shell structures of various organism groups. However, their quantitative analysis is often hampered by the difficulty to discriminate cavities and pores within the object from the surrounding region. Herein, we test the ambient occlusion (AO) algorithm and newly implemented optimisations for the segmentation of cavities (implemented in the software Amira). The segmentation accuracy is evaluated as a function of (i) changes in the ray length input variable, and (ii) the usage of AO (scalar) field and other AO-derived (scalar) fields. The results clearly indicate that the AO field itself outperforms all other AO-derived fields in terms of segmentation accuracy and robustness against variations in the ray length input variable. The newly implemented optimisations improved the AO field-based segmentation only slightly, while the segmentations based on the AOderived fields improved considerably. Additionally, we evaluated the potential of the AO field and AO-derived fields for the separation and classification of cavities as well as skeletal structures by comparing them with commonly used distance-map-based segmentations. For this, we tested the zooid separation within a bryozoan colony, the stereom classification of an ophiuroid tooth, the separation of bioerosion traces within a marble block and the calice (central cavity)-pore separation within a dendrophyllid coral. The obtained results clearly indicate that the ideal input field depends on the three-dimensional morphology of the object of interest. The segmentations based on the AO-derived fields often provided cavity separations and skeleton classifications that were superior to or impossible to obtain with commonly used distance-map-based segmentations. The combined usage of various AO-derived fields by supervised or unsupervised segmentation algorithms might provide a promising target for future research to further improve the results for this kind of high-end data segmentation and classification. Furthermore, the application of the developed segmentation algorithm is not restricted to X-ray (micro-)computed tomographic data but may potentially be useful for the segmentation of 3D volume data from other sources. KW - Micro-computed tomography KW - Pore segmentation KW - Skeletal classification KW - Image analysis PY - 2018 DO - https://doi.org/10.1016/j.cageo.2018.03.007 SN - 0098-3004 SN - 1873-7803 VL - 115 SP - 75 EP - 87 PB - Elsevier Ltd. AN - OPUS4-44511 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Gunella, F. A1 - Kunisch, E. A1 - Maenz, S. A1 - Horbert, V. A1 - Xin, L. A1 - Mika, J. A1 - Borowski, J. A1 - Bischoff, S. A1 - Schubert, H. A1 - Sachse, A. A1 - Illerhaus, Bernhard A1 - Günster, Jens A1 - Bossert, J. A1 - Jandt, K. D. A1 - Plöger, F. A1 - Kinne, R. W. A1 - Brinkmann, O. A1 - Bungartz, M. ED - Carragee, T1 - The GDF5 mutant BB-1 enhances the bone formation induced by an injectable, poly(l-lactide-co-glycolide) acid (PLGA) fiber-reinforced, brushite-forming cement in a sheep defect model of lumbar osteopenia T2 - The Spine Journal N2 - BACKGROUND CONTEXT: Targeted delivery of osteoinductive bone morphogenetic Proteins (eg, GDF5) in bioresorbable calcium phosphate cement (CPC), potentially suitable for vertebroplasty and kyphoplasty of osteoporotic vertebral fractures, may be required to counteract augmented local bone catabolism and to support complete bone regeneration. The biologically optimized GDF5 Mutant BB-1 may represent an attractive drug candidate for this purpose. PURPOSE: The aim of the current study was to test an injectable, poly (l-lactide-co-glycolide) acid (PLGA) fiber-reinforced, brushite-forming CPC containing low-dose BB-1 in a sheep lumbar osteopenia model. STUDY DESIGN/ SETTING: This is a prospective experimental animal study. METHODS: Bone defects (diameter 5 mm) were generated in aged, osteopenic female sheep and were filled with fiber-reinforced CPC alone (L4; CPC+fibers) or with CPC containing different dosages. KW - Bone morphogenetic protein; KW - Bone regeneration; KW - Micro-Computed-Tomography; KW - Calcium phosphate cement; KW - GDF-5 mutant; KW - Large animal model sheep; KW - Osteoporotic vertebral fracture PY - 2018 DO - https://doi.org/10.1016/j.spinee.2017.10.002 SN - 1529-9430 SN - 1878-1632 VL - 18 IS - 2 SP - 357 EP - 369 PB - Elsevier CY - New York AN - OPUS4-44561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maul, Ronald A1 - Borzekowski, Antje A1 - Drewitz, Tatjana A1 - Keller, Julia A1 - Pfeifer, Dietmar A1 - Kunte, Hans-Jörg A1 - Koch, Matthias A1 - Rohn, S. T1 - Biosynthesis of zearalenone conjugates by fungi N2 - Zearalenone (ZEN) and its sulfate and glucoside conjugates have been detected in (a broad variety of) food and feed commodities1. Both conjugated derivatives are formed as part of fungal or plant secondary metabolism and thus, belong to the group of modified mycotoxins2. After consumption of contaminated foodstuff, the conjugates can be hydrolyzed by human intestinal microbiota leading to liberation of ZEN that implies an underestimation of the true ZEN exposure. In order to include ZEN conjugates in routine analysis, as well as for toxicological investigation reliable standards are needed. The objective of the present study was to develop a simple and economic method for biosynthesis of ZEN conjugates. Preceding experiments on the biotransformation of ZEN by Rhizopus and Aspergillus species showed a mixed metabolite formation3. Therefore, these known ZEN conjugating fungal strains were screened for their potential to selectively synthesize the ZEN derivatives ZEN-14-sulfate (Z14S), ZEN-14-glucoside (Z14G) and ZEN-16-glucoside (Z16G). The screening was conducted by adding ZEN to liquid fungal cultures. Cultivation conditions and ZEN incubation time were varied. All media samples were analyzed for metabolite formation by HPLC-MS/MS. Z14S was exclusively formed by A. oryzae. Under optimized conditions a specific biosynthesis of Z14G by R. oryzae and Z16G by R. oligosporus was achieved. After liquid-liquid-extraction and preparative chromatographic cleanup 1H-NMR purities of ≥ 73% for Z14S, ≥ 82% for Z14G and ≥ 50% for Z16G were obtained. In addition, a consecutive biosynthesis was developed by first using Fusarium graminearum for ZEN biosynthesis on rice based liquid medium. After inactivation of Fusarium the subsequent conjugation reaction was conducted utilizing Aspergillus and Rhizopus species under the various optimized conditions. In this study an easy and cost-efficient biosynthesis for Z14S, Z14G and Z16G was developed. The developed biosynthesis could be also used for other metabolites like ZEL conjugates. Our results of the in vitro screening indicate also the formation of a ZEL-glucoside and α ZEL-sulfate as major metabolites by R. oryzae. In sum, under optimized cultivation conditions fungi can be easily utilized for a targeted and stereospecific synthesis of ZEN conjugates. T2 - 10th World Mycotoxin Forum Conference CY - Amsterdam, The Netherlands DA - 12.03.2018 KW - Mycotoxins KW - Food safety KW - Analytical standards PY - 2018 AN - OPUS4-44547 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Terborg, R. A1 - Hodoroaba, Vasile-Dan T1 - Analysis of the elemental composition and thickness of a Fe-Ni film on Si using Bruker ESPRIT and SAMx STRATAGem N2 - Quantitative analysis of a bulk sample requires that the composition of the sample is homogeneous over the analyzed volume. For inhomogenous samples the calculation of the matrix effects is not correct and this can lead to wrong results in the element concentrations. For samples containing a layer structure a different quantitative evaluation has to be applied. This can be provided with the standard-based analysis in ESPRIT in combination with the STRATAGem software. KW - Thin film analysis KW - SEM/EDX KW - EPMA KW - k-values PY - 2018 UR - https://www.bruker.com/products/x-ray-diffraction-and-elemental-analysis/eds-wds-ebsd-sem-micro-xrf-and-sem-micro-ct/quantax-eds-for-sem/applications/layer-analysis.html SP - 1 EP - 4 CY - Berlin AN - OPUS4-44594 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gottlieb, Cassian A1 - Günther, Tobias A1 - Wilsch, Gerd T1 - Impact of grain sizes on the quantitative concrete analysis using laser-induced breakdown spectroscopy JF - Spectrochimica Acta Part B: Atomic Spectroscopy N2 - In civil engineering concrete is the most used building material for making infrastructures like bridges and parking decks worldwide. It is as a porous and multiphase material made of aggregates with a defined grain size distribution, cement and water as well as different additives and admixtures depending on the application. Different grain sizes are important to ensure the needed density and compressive strength. The resulting porous cement matrix contains a mixture of flour grains (aggregates with a grain size below 125 lm) and cement particles (particle size≈50lm). Harmful species like chlorides may penetrate together with water through the capillary pore space and may trigger different damage processes. The damage assessment of concrete structures in Germany is estimated due to the quantification of harmful elements regarding to the cement content only. In the evaluation of concrete using LIBS a two-dimensional scanning is necessary to consider the heterogeneity caused by the aggregates. Therefore, a LIBS system operating with a low energy NdCr:YAG laser, a pulse energy of 3 mJ, a wavelength of 1064 nm, a pulse width of 1.5 ns and a Repetition rate of 100 Hz has been used. Different Czerny-Turner spectrometers with CCD detectors in the UV and NIR range have been used for the detection. Large aggregates (macro-heterogeneity) can be excluded from the evaluation, whereas small aggregates in the range of the laser spot size (flour grains) cannot be spatially resolved. In this work the micro heterogeneity caused by flour grains and their impact on the quantification with LIBS will be discussed. To analyze the effect of changing grain sizes and ratios, the ablation behavior has been determined and compared. Samples with defined grain sizes were made and analyzed using LIBS. The grain size distributions were analyzed with laser diffraction (LDA). KW - LIBS KW - Concrete KW - Micro heterogeneity KW - Grain sizes PY - 2018 DO - https://doi.org/10.1016/j.sab.2018.02.004 SN - 0584-8547 SN - 0038-6987 VL - 142 SP - 74 EP - 84 PB - Elsevier AN - OPUS4-44595 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heinen, S. A1 - Rackow, S. A1 - Cuellar-Camacho, J. L. A1 - Donskyi, Ievgen A1 - Unger, Wolfgang A1 - Weinhart, M. T1 - Transfer of functional thermoresponsive poly(glycidyl ether) coatings for cell sheet fabrication from gold to glass surfaces JF - Journal of Materials Chemistry B N2 - Thermoresponsive polymer coatings can facilitate cell sheet fabrication under mild conditions by promoting cell adhesion and proliferation at 37 1C. At lower temperatures the detachment of confluent cell sheets is triggered without enzymatic treatment. Thus, confluent cell sheets with intact extracellular matrix for regenerative medicine or tissue engineering applications become available. Herein, we applied the previously identified structural design parameters of functional, thermoresponsive poly(glycidyl ether) brushes on gold to the more application-relevant substrate glass via the self-assembly of a corresponding block copolymer (PGE-AA) with a short surface-reactive, amine-presenting anchor block. Both, physical and covalent immobilization on glass via either multivalent ionic interactions of the anchor block with bare glass or the coupling of the anchor block to a polydopamine (PDA) adhesion layer on glass resulted in stable coatings. Atomic force microscopy revealed a high degree of roughness of covalently attached coatings on the PDA adhesion layer, while physically attached coatings on bare glass were smooth and in the brush-like regime. Cell sheets of primary human dermal fibroblasts detached reliably (86%) and within 20 ± 10 min from physically tethered PGE-AA coatings on glass when prepared under cloud point grafting conditions. The presence of the laterally inhomogeneous PDA adhesion layer, however, hindered the spontaneous temperature-triggered cell detachment from covalently grafted PGE-AA, decreasing both detachment rate and reliability. Despite being only physically attached, self-assembled monolayer brushes of PGE-AA block copolymers on glass are functional and stable thermoresponsive coatings for application in cell sheet fabrication of human fibroblasts as determined by X-ray photoelectron spectroscopy. KW - X-ray photoelectron spectroscopy KW - Thermoresponsive poly(glycidyl ether) coatings KW - Cell sheet fabrication KW - Nm film thickness PY - 2018 DO - https://doi.org/10.1039/c7tb03263c SN - 2050-750X SN - 2050-7518 VL - 6 IS - 10 SP - 1489 EP - 1500 PB - The Royal Society of Chemistry AN - OPUS4-44600 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Plasma Fundamentals and Diagnostics N2 - This course will provide an introduction to plasma diagnostic techniques. The major focus of the course will be on the discussions of the practical procedures as well as the underlying physical principles for the measurements of plasma fundamental characteristics (e.g., temperatures, thermodynamic properties, and electron number density). Particular emphasis will be placed on inductively coupled plasma–atomic emission spectrometry, but other analytical plasmas will also be used as examples when appropriate. Selected examples on how one can manipulate the operating conditions of the plasma source, based on the results of plasma diagnostic measurements, to improve its performance used for spectrochemical analysis will also be covered. Topics to be covered include thermal equilibrium, line profiles, temperatures, electron densities, excitation processes, microreactions, pump and probe diagnostics, tomography, temporal and spatial resolution. Basis of plasma computer modeling will be presented. T2 - Winter Plasma Conference CY - Amelia Island, FL, USA DA - 08.01.2018 KW - Plasma diagnostics KW - Plasma physics PY - 2018 AN - OPUS4-44497 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit A1 - Schwibbert, Karin A1 - Dietrich, P. A1 - Thissen, A. A1 - Unger, Wolfgang T1 - Surface characterisation of biofilms by nearambient pressure X-ray photoelectron spectroscopy N2 - The XPS information depth of approximately 10 nm is in the same size range as the outer membrane of the gram-negative bacteria, which makes XPS a suitable tool for determining the elemental composition of the bacterial surface and monitor changes caused by outer stress like dehydration or exposure to antimicrobials. However, bacteria are inherently in a hydrated state, and therefore only compatible to ultra-high vacuum after extensive sample preparation, which may degrade the sample constituents. This issue is addressed by the development of near-ambient pressure (NAP)-XPS, which enables bacteria and biofilms to be characterised in their native wet state. Artificial biofilms, bacteria and biofilms of Escherichia coli have been characterised with the laboratory NAP-XPS instrument EnviroESCA from SPECS GmbH, at pressures ranging from high vacuum to 12 mbar, and in both humid and dry environment. By studying biological samples in their native wet state, new insight about composition and transport of drugs through cell membranes and the extracellular polymeric substance (EPS) of biofilms can be obtained. T2 - Royal Society of Chemistry Twitter Conference CY - Worldwide (online conference) DA - 06.03.2018 KW - Biofilms KW - E. coli KW - Alginate KW - NAP-XPS PY - 2018 AN - OPUS4-44498 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. A1 - Shabanov, Sergej V. T1 - Modeling chemical reactions in laser-induced plasmas at local thermodynamic equilibrium N2 - Laser induced plasma (LIP) is a dynamic, short living event which presents significant difficulty for modeling. In this report, a collisional-dominated chemical model developed earlier* is expanded by the inclusion of a new method for calculation of chemical reactions. The model consists of the coupled Navier-Stokes, state, radiative transfer, material transport, and chemical equations. The latter are written in terms of atomic and molecular partition functions rather than reaction rates. Typically, a solution of such the system of chemical equations is difficult for the entire range of plasma temperatures and densities because reaction constants may vary by hundreds orders of magnitude owing to extreme plasma conditions. No numerical solver of non-linear systems of equations handles this situation with ease. We resolve the problem by using a hierarchical approach. First, we rank the reactions according to their ascendancy. Second, we exploit either the contraction or Newton-Raphson algorithms to solve the system of chemical equations. We illustrate the approach by performing a series of calculations for reacting species Si, C, N, Ca, Cl and their molecules in laser induced plasmas. T2 - Winter Plasma Conference CY - Amelia Island, FL, USA DA - 08.01.2018 KW - Plasma physics KW - Plasma diagnostics PY - 2018 AN - OPUS4-44499 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit A1 - Schwibbert, Karin A1 - Dietrich, P. A1 - Thissen, A. A1 - Unger, Wolfgang T1 - Surface characterisation of bacteria and biofilms by NAP-XPS N2 - The XPS information depth of approximately 10 nm is in the same size range as the outer membrane of the gram-negative bacteria, which makes XPS a suitable tool for determining the elemental composition of the bacterial surface and monitor changes caused by outer stress like dehydration or exposure to antimicrobials. However, bacteria are inherently in a hydrated state, and therefore only compatible to ultra-high vacuum after extensive sample preparation, which may degrade the sample constituents. This issue is addressed by the development of near-ambient pressure (NAP)-XPS, which enables bacteria and biofilms to be characterised in their native wet state. Artificial biofilms, bacteria and biofilms of Escherichia coli have been characterised with the laboratory NAP-XPS instrument EnviroESCA from SPECS GmbH, at pressures ranging from high vacuum to 12 mbar, and in both humid and dry environment. By studying biological samples in their native wet state, new insight about composition and transport of drugs through cell membranes and the extracellular polymeric substance (EPS) of biofilms can be obtained. In this contribution, the latest progress on biofilm characterisation by NAP-XPS will be presented, and measurement capabilities and limitations will be discussed. T2 - Die Frühjahrstagung der Deutsche Physikalische Gesellschaft CY - Berlin, Germany DA - 12.03.2018 KW - Biofilms KW - E. coli KW - Alginate KW - NAP-XPS PY - 2018 AN - OPUS4-44500 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Szymoniak, Paulina A1 - Madkour, Sherif A1 - Schönhals, Andreas T1 - Dynamics of nanoscopically confined PVME in thin films of an asymmetric PVME/PS blend N2 - In recent years, substantial efforts have been devoted to investigating nanoscopic confinement of polymers, and its effect on glassy dynamics. Broadband Dielectric Spectroscopy (BDS) was used to study the dynamics of ultra-thin films of PVME/PS 50/50 wt% blend, employing a novel nano-structured capacitor sample arrangement. The investigated system shows a complex dynamic behavior. First, an α-relaxation, related to a bulk-like layer was found. Second, an α’-relaxation was observed, characteristic for dynamically asymmetric blends, where the out of equilibrium dynamics is attributed to weakly-cooperative PVME segments relaxing within a frozen environment of PS segments. Thirdly, for thinnest films, an Arrhenius-like process was dominant in the dielectric spectra, indicating localized fluctuations of the segments. Relaxation rates of this process resembled that of the degenerated α-relaxation of the adsorbed layer, found for pure PVME, thus it was assigned accordingly. For thinnest films, this process undergoes a further confinement, due to the topological constraints, introduced by PS. Such multiple confinement effect has not been reported for ultra-thin films of polymer blends, before this study. T2 - Spring Meeting of German Physical Society CY - Berlin, Germany DA - 12.03.2018 KW - Thin polymeric films PY - 2018 AN - OPUS4-44502 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rhode, Michael A1 - Mente, Tobias A1 - Steppan, E. A1 - Kannengießer, Thomas A1 - Steger, J. T1 - Hydrogen trapping in T24 Cr-Mo-V steel weld joints - microstructure effect vs. experimental influence on activation energy for diffusion JF - Welding in the World N2 - Hydrogen-assisted cracking is a critical combination of local microstructure, mechanical load and hydrogen concentration. Welded microstructures of low-alloyed creep-resistant Cr-Mo-V steels show different hydrogen trapping kinetics. This influences the adsorbed hydrogen concentration as well as the diffusion by moderate or strong trapping. A common approach to describe hydrogen traps is by their activation energy that is necessary to release hydrogen from the trap. In the present study, Cr-Mo-V steel T24 (7CrMoVTiB10-10) base material and TIG weld metal were investigated. Electrochemically hydrogen charged specimens were analyzed by thermal desorption analysis (TDA) with different linear heating rates. The results show two different effects. At first, the microstructure effect on trapping is evident in terms of higher hydrogen concentrations in the weld metal and increased activation energy for hydrogen release. Secondly, it is necessary to monitor the real specimen temperature. A comparison between the adjusted heating rate and the real specimen temperature shows that the calculated activation energy varies by factor two. Thus, the trap character in case of the base material changes to irreversible at decreased temperature. Hence, the effect of the experimental procedure must be considered as well if evaluating TDA results. Finally, realistic temperature assessment is mandatory for calculation of activation energy via TDA. KW - Creep-resistant steel KW - Hydrogen assisted cracking KW - Thermal desorption analysis KW - Welding KW - Microstructure KW - Diffusion PY - 2018 DO - https://doi.org/10.1007/s40194-017-0546-6 SN - 0043-2288 SN - 1878-6669 VL - 62 IS - 2 SP - 277 EP - 287 PB - Springer CY - Berlin, Heidelberg AN - OPUS4-44505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Coelho Lima, Isabela A1 - Grohmann, Maria A1 - Niederleithinger, Ernst T1 - Alternative imaging conditions for reverse-time migration N2 - Poster on the evaluation of several imaging conditions for reverse time migration, applied to ultrasonic echo data, tested with synthetic (simulated) dat and real data from a polyamide model. T2 - Jahrestagung der Deutschen geophysikalischen Gesellschaft CY - Leoben, Austria DA - 12.2.2018 KW - Ultrasound KW - Reverse time migration KW - Imaging condition KW - Concrete KW - Polyamide PY - 2018 AN - OPUS4-44583 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Ultrasound: From Imaging to Monitoring N2 - Review of ultrasonic echo imaging and ultrasonic monitoring techniques applied to concrete structures, especially bridges. Includes newest research results from BAM. T2 - Transport Research Board Annual Meeting, Workshop 1647 CY - Washington, DC, USA DA - 6.1.2018 KW - Ultrasound KW - Imaging KW - Monitoring KW - Concrete KW - Bridges PY - 2018 AN - OPUS4-44587 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Dietrich, P. A1 - Beblo-Vranesevic, K. A1 - Kjærvik, Marit A1 - Unger, Wolfgang A1 - Schwibbert, Karin A1 - Hardie, K. A1 - Brown, J. T1 - XPS surface analysis of bacterial samples N2 - This application note presents how EnviroESCA can be used to analyze bacterial samples under near ambient pressure conditions in various states of hydration using different levels of humidity. Such investigations of bacterial cell wall surfaces in their hydrated state are essential for studying biological interfaces at work. The use of innovative near-ambient pressure (NAP-)XPS instrumentation allows the detailed analysis of irregularly-surfaced biofilms. NAP-XPS enables the surface analysis of bacterial samples in their natural hydrated state without complex sample preparation techniques such as freeze-drying or fast-freezing, which are needed for XPS analysis in ultrahigh vacuum. KW - Near ambient pressure XPS KW - Biofilms PY - 2018 UR - http://www.enviroai.com/uploads/1/0/2/8/102861712/xps_surface_analysis_of_bacillus_subtilis_biofilms_final.pdf IS - Application Note #000399 SP - 1 EP - 5 CY - Berlin AN - OPUS4-44588 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saatz, Jessica A1 - Grunert, B. A1 - Jakubowski, Norbert T1 - Nanocrystals as labeling reagents for bioimaging of clinical cell assays N2 - Imaging of elemental distributions in single cell assays as well as tissue sections can be performed by laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS). This powerful technique offers precise spatially resolved measurements at the trace and ultratrace level and has been established as an excellent tool to answer analytical, biological and biomedical questions. To date, imaging mass cytometry is already able to simultaneously detect up to 40 cellular targets due to conjugation of isotopically pure lanthanides to affinity binders, e.g. antibodies. To further enhance the ability of multiparametric analysis to more than 100 analytes at once, we investigated lanthanide nanocrystals as new, highly sensitive metal tags for identification of targets in clinical cell assays and tissue samples. Multiparametric analysis will be possible by encoding the lanthanide composition of nanocrystals associated to the affinity binders. Nanocrystals showed remarkable potential for sensitive detection in MS due to high stability and signal amplification compared to e.g. polymer tags, carrying fewer metal atoms. Synthesis of functionalized lanthanide nanocrystals for further bioconjugation was performed with high reproducibility and monodisperse size distribution. For proof of principle, the uptake and distribution of these nanocrystals within the monolayered cell line A549 were investigated by mapping the intensities at subcellular resolution using LA-ICP-MS. It could be shown, that the cells were efficiently labeled with the nanocrystals and mostly accumulate near the nucleus. Additionally, the bioconjugation of the nanocrystals to antibodies and particularly the preservation of the antibody specificity was investigated using Dot Blot experiments. All in all, the results imply high sensitivity and the possibility of multiparametric analysis by doting various lanthanides into the nanocrystals. T2 - ESAS & CANAS 2018 CY - Berlin, Germany DA - 20.03.2018 KW - Bioimaging KW - Nanoparticle KW - Immuno-assay KW - Lanthanide PY - 2018 AN - OPUS4-44593 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Donskyi, Ievgen A1 - Drüke, M. A1 - Silberreis, K. A1 - Lauster, D. A1 - Ludwig, K. A1 - Kühne, C. A1 - Unger, Wolfgang A1 - Böttcher, C. A1 - Herrmann, A. A1 - Dernedde, J. A1 - Adeli, M. A1 - Haag, R. T1 - Interactions of fullerene-polyglycerol sulfates at viral and cellular interfaces JF - small N2 - Understanding the mechanism of interactions of nanomaterials at biointerfaces is a crucial issue to develop new antimicrobial vectors. In this work, a series of water-soluble fullerene-polyglycerol sulfates (FPS) with different fullerene/polymer weight ratios and varying numbers of polyglycerol sulfate branches are synthesized, characterized, and their interactions with two distinct surfaces displaying proteins involved in target cell recognition are investigated. The combination of polyanionic branches with a solvent exposed variable hydrophobic core in FPS proves to be superior to analogs possessing only one of these features in preventing interaction of vesicular Stomatitis virus coat glycoprotein (VSV-G) with baby hamster kidney cells serving as a model of host cell. Interference with L-selectin-ligand binding is dominated by the negative charge, which is studied by two assays: a competitive surface plasmon resonance (SPR)-based inhibition assay and the leukocyte cell (NALM-6) rolling on ligands under flow conditions. Due to possible intrinsic hydrophobic and electrostatic effects of synthesized compounds, pico- to nanomolar half maximal inhibitory concentrations (IC50) are achieved. With their highly antiviral and anti-inflammatory properties, together with good biocompatibility, FPS are promising candidates for the future development towards biomedical applications. KW - Fullerene-Polyglycerol Sulfates KW - Fullerene KW - Biointerfaces KW - XPS PY - 2018 DO - https://doi.org/10.1002/smll.201800189 SN - 1613-6829 SN - 1613-6810 VL - 14 IS - 17 SP - 1800189, 1 EP - 7 PB - WILEY-VCH Verlag GmbH & Co. KGaA CY - Weinheim AN - OPUS4-44573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Fischer, Daniel A1 - Hertwig, Andreas A1 - Hidde, Gundula A1 - Stockmann, Jörg M. A1 - Weise, Matthias T1 - Ellipsometric imaging of low-contrast surface modifications and depolarization contrast imaging (DCI) of particulate accumulations N2 - Imaging of surfaces regarding topographical, morphological, micro-structural, and chemical features is a key requirement for quality control for the identification of contaminated, degraded, damaged or deliberately modified surface areas vs. clean, virgin, undamaged or unmodified regions. As optical functions may represent any of these changes on the micro- and nano-scale, imaging ellipsometry (IE) is the technique of choice using either intensity, phase, or/and amplitude contrast for visualization of low-contrast surface modifications [1, 2]. Defects or surface and film features whether native or artificial, intended or unintended, avoidable or unavoidable as well as surface pattern are of interest for quality control. In contrast to microscopic techniques operated at normal incidence, ellipsometry as oblique-incidence technique provides improved contrast for vertically nano-scaled add-on or sub-off features such as ultra-thin transparent films, metallic island films, carbon-based thin films, laser modification or laser induced damage, dried stain, cleaning agent or polymeric residue. Two-sample reference techniques, i.e. referenced spectroscopic ellipsometry (RSE) may further increase sensitivity and decrease measurement time. In case of particulate accumulations depolarization contrast imaging (DCI) may improve the lateral resolution beyond the Abbe limit. This has been proven for silica spheres as reference in terms of single particles, particulate accumulations or particulate monolayers and layer stacks. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) were used for reference measurements of particle diameter, particle height, or particulate layer/accumulation thickness. It has been shown that single silica particles of 250 nm in diameter, i.e. at least a factor of 4 better than the lateral resolution limit as of now, can be visualized on even substrates. However, the ellipsometric measurement of particle diameters of this size needs further efforts interpretation. T2 - Workshop Ellipsometry 2018 CY - Chemnitz, Germaný DA - 19.03.2018 KW - Low-contrast surface modifications KW - Particulate distributions KW - Imaging ellipsometry(IE) KW - Depolarization contrast imaging (DCI) PY - 2018 AN - OPUS4-44548 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Eisenreich, F. A1 - Kathan, M. A1 - Dallmann, A. A1 - Ihrig, S. P. A1 - Schwaar, Timm A1 - Schmidt, B. M. A1 - Hecht, S. T1 - A photoswitchable catalyst system for remote-controlled (co)polymerization in situ JF - Nature Catalysis N2 - The fundamental properties of a polymeric material are ultimately governed by its structure, which mainly relies on monomercomposition and connection, topology, chain length, and polydispersity. Thus far, these structural characteristics are typicallyset ex situ by the specific polymerization procedure, eventually limiting the future design space for the creation of moresophisticated polymers. Herein, we report on a single photoswitchable catalyst system, which enables in situ remote controlover the ring-opening polymerization of l-lactide and further allows regulation of the incorporation of trimethylene carbonateand δ -valerolactone monomers in copolymerizations. By implementing a phenol moiety into a diarylethene-type structure,we exploit light-induced keto–enol tautomerism to switch the hydrogen-bonding-mediated monomer activation reversiblyON and OFF. This general and versatile principle allows for exquisite external modulation of ground-state catalysis of a livingpolymerization process in a closed system by ultraviolet and visible light and should thereby facilitate the generation of newpolymer structures. KW - Polymers PY - 2018 DO - https://doi.org/10.1038/s41929-018-0091-8 SN - 2520-1158 VL - 1 IS - 7 SP - 516 EP - 522 PB - Nature CY - London AN - OPUS4-45407 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Batzorig, L. A1 - Recknagel, Sebastian A1 - Scharf, Holger A1 - Oyuntungalag, U. A1 - Tegshjargal, E. A1 - Rausch, J. T1 - Certified reference material of total cyanide in soil/BAM-U 116/CGL 306 N2 - Due to their toxicity and widespread application for mining and industrial purposes, cyanides are ranking among the most important inorganic pollutants which should be tested and monitored not only in the aquatic environment, but also in soils and soil-like materials. Reference materials of soils with relevant contents of cyanide to ensure reliable test results of laboratories are rare today. New certified reference material (CRM) BAM-U116/CGL306 “Cyanide in soil” was produced within a framework of cooperation between Central Geological Laboratory (CGL) of Mongolia and Federal Institute for Materials Research and Testing (BAM) of Germany in 2013-2017. The CRM BAM-U116/CGL306 represents a mixture of a sandy soil collected from a contaminated former gasworks area in the Berlin region (Germany) and an unpolluted sandy soil from Nalaikh region (Mongolia). The bulk candidate material for this reference material was prepared at CGL CRM Laboratory exclusively destined to the preparation of reference materials and equipped with modern technical equipment. Homogeneity, stability and shelf life were studied in full compliance with ISO Guide 35. The CRM was evaluated as sufficiently homogeneous. Statistical evaluation of certification analysis was performed using software packages SoftCRM and ProLab Plus. Certified value of total cyanide of the CRM is 12.0 mg/kg and expanded uncertainty was assigned as 0.8 mg/kg. The intended purpose of this material is the verification of analytical results obtained for the mass fraction of total cyanide in soils and soil-like materials applying the standardized procedure ISO 11262:2011. As any reference material, it can also be used for routine performance checks (quality control charts) or validation studies. T2 - Geoanalysis 2018 CY - Sydney, Australia DA - 08.07.2018 KW - Certified reference material KW - Cyanide in soil KW - Total cyanide PY - 2018 AN - OPUS4-45417 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gornushkin, Igor B. A1 - Völker, Tobias A1 - Kazakov, Alexander Ya. T1 - Extension and investigation by numerical simulations of algorithm for calibration-free laser induced breakdown spectroscopy JF - Spectrochimica Acta Part B N2 - Accuracy of calibration-free (CF) methods in laser-induced breakdown spectroscopy (LIBS) depends on experimental conditions and instrumental parameters that must match a CF LIBS model. Here, the numerical study is performed to investigate effects of various factors, such as the optical density, plasma uniformity, line overlap, noise, spectral resolution, electron density and path length on the results of CF-LIBS analyses. The effects are examined one-by-one using synthetic spectra of steel slag samples that fully comply with the mathematical model of the method. Also, the algorithm includes several new features in comparison with previously proposed CF algorithms. In particular, it removes limits on the optical thickness of spectral lines that are used for the construction of the Saha-Boltzmann plot; it retrieves the absorption path length (Plasma diameter) directly from spectral lines; it uses the more realistic Voigt line profile function instead of the Lorentzian function; and it employs the pre-calculated and tabulated thin-to-thick line ratios instead of approximating functions for selfabsorption correction. KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics KW - Calibration free LIBS PY - 2018 DO - https://doi.org/10.1016/j.sab.2018.06.011 SN - 0584-8547 VL - 147 SP - 149 EP - 163 PB - Elsevier B.V. AN - OPUS4-45340 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Improved algorithm for calibration-free laser induced breakdown spectroscopy N2 - An improved algorithm for calibration-free laser induced breakdown spectroscopy (CF LIBS) is presented which includes several novel features in comparison with previously proposed similar algorithms. In particular, it allows using spectral lines with arbitrary optical thickness for the construction of Saha-Boltzmann plots, retrieves the absorption path length (plasma diameter) directly from a spectrum, replaces the Lorentzian line profile function by the Voigt function, and allows for self-absorption correction using pre-calculated and tabulated data rather than approximating functions. The tabulated data embody the solutions of the radiative transfer equation for numerous combinations of optical thicknesses and line widths. The algorithm is thoroughly verified with synthetic spectra. T2 - 14TH European Workshop on Laser Ablation 2018 (EWLA2018) CY - Pau, France DA - June 26 - 29, 2018 KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics KW - Calibration free LIBS PY - 2018 AN - OPUS4-45343 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gornushkin, Igor B. T1 - Laser induced plasma: Modeling, diagnostics, and applications N2 - Laser-induced plasmas are widely used in many areas of science and technology; examples include spectrochemical analysis, thin film deposition, material processing, and even jet propulsion. Several topics will be addressed. First, general phenomenology of laser-induced plasmas will be discussed. Then, a chemical model will be presented based on a coupled solution of Navier-Stokes, state, radiative transfer, material transport, and chemical (Guldberg-Waage) equations. Results of computer simulations for several chemical systems will be shown and compared to experimental observations obtained by optical imaging, spectroscopy, and tomography. The latter diagnostic tools will also be briefly discussed. Finally, a prospective application of laser-induced plasma and plasma modeling will be illustrated on the example of calibration-free MC LIBS (Monte Carlo Laser Induced Breakdown Spectroscopy), in which concentrations of elements in materials are found by fitting model-generated and experimental spectra. T2 - Invited talk at Yeshiva University, New York, USA CY - Yeshiva University, New York, USA DA - 4.24.2018 KW - Laser induced plasma KW - LIBS KW - Plasma modeling KW - Plasma diagnostics PY - 2018 AN - OPUS4-45344 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Strangfeld, Christoph A1 - Kruschwitz, Sabine T1 - Monitoring of the absolute water content in porous materials based on embedded humidity sensors JF - Journal of Construction and Building Materials N2 - Moisture transport monitoring may indicate the onset of deterioration in porous building materials Prior to damage occurring. Most moisture measurement systems provide only qualitative values, require extensive calibration, or are destructive. Thus, non-destructive and calibration-free monitoring Systems are required. Our approach of moisture monitoring is to embed sensors that measure the relative humidity. In our experiment, screed samples are monitored during the Hydration and evaporation process. Every test sample is equipped with 10 embedded sensors which measure the relative humidity across the sample thickness. Based on Hillerborg’s approach, the relative humidity is converted into the corresponding pore saturation. In our study, the free water is computed without knowledge of the Sorption isotherm. The free water in the pore system is predicted and validated. The predicted weight decrease corresponds conclusively to gravimetrically measured weights. The embedded sensors yield the absolute liquid water content and enable an experimental, non-destructive monitoring of liquid water in porous materials. KW - Moisture measurements KW - Porous materials KW - Embedded sensors KW - Partial pore saturation KW - Sorption isotherm PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-453476 DO - https://doi.org/10.1016/j.conbuildmat.2018.05.044 SN - 0950-0618 VL - 177 SP - 511 EP - 521 PB - Elsevier AN - OPUS4-45347 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lozano-Torres, B. A1 - Marcos, M. Dolores A1 - Pardo, T. A1 - Sancenón, F. A1 - Martínez-Mánez, Ramon A1 - Rurack, Knut T1 - Anilinopyridine–metal complexes for the selective chromogenic sensing of cyanide anion JF - Journal of Coordination Chemistry N2 - Probe 1, which contains an anilinopyridine chromophore and an azaoxa macrocyclic subunit, presented an absorption band centered at 340 nm in acetonitrile. Addition of Fe(III), Cr(III) and Hg(II) induced the growth of a new absorption band at 430 nm (with color change from colorless to yellow), whereas in the presence of Cu(II), Zn(II) and Pb(II), less marked changes were observed. The color changes observed upon addition of Fe(III), Cr(III) and Hg(II) were ascribed to the formation of 1:1 stoichiometry complexes with probe 1. Coordination of Fe(III), Cr(III) and Hg(II) with the pyridine fragment of 1 induced an enhancement of the charge transfer character accompanied with a marked bathochromic shift that was reflected in a color change from colorless to yellow. The strength of the interaction between probe 1 and Fe(III) cation was modulated upon interaction with anions. Of all the anions tested, only cyanide was able to induce the bleaching of the yellow 1·Fe(III) complex solution. This bleaching was ascribed to the formation of 1·Fe(III)-CN complex that restored, to some extent, the optical features of the free probe allowing the chromogenic sensing of cyanide. Besides, 1·Fe(III) complex was used to detect cyanide in acetonitrile-water 90:10 v/v mixtures with good recoveries. KW - Anilinopyridine KW - Charge Transfer KW - Iron Complex KW - Colorimetric Test KW - Cyanide PY - 2018 DO - https://doi.org/10.1080/00958972.2018.1434719 SN - 0095-8972 VL - 71 IS - 6 SP - 786 EP - 796 PB - Taylor & Francis Group CY - London AN - OPUS4-45398 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wagner, Sabine A1 - Zapata, Carlos A1 - Wan, Wei A1 - Gawlitza, Kornelia A1 - Weber, M. A1 - Rurack, Knut T1 - Role of Counterions in Molecularly Imprinted Polymers for Anionic Species JF - Langmuir N2 - Small-molecule oxoanions are often imprinted noncovalently as carboxylates into molecularly imprinted polymers (MIPs), requiring the use of an organic counterion. Popular species are either pentamethylpiperidine (PMP) as a protonatable cation or tetraalkylammonium (TXA) ions as permanent cations. The present work explores the influence of the TXA as a function of their alkyl chain length, from methyl to octyl, using UV/vis absorption, fluorescence titrations, and HPLC as well as MD simulations. Protected phenylalanines (Z-L/D-Phe) served as templates/analytes. While the influence of the counterion on the complex stability constants and anion-induced spectral changes shows a monotonous trend with increasing alkyl chain length at the prepolymerization stage, the cross-imprinting/rebinding studies showed a unique pattern that suggested the presence of adaptive cavities in the MIP matrix, related to the concept of induced fit of enzyme−substrate interaction. Larger cavities formed in the presence of larger counterions can take up pairs of Z-X-Phe and smaller TXA, eventually escaping spectroscopic detection. Correlation of the experimental data with the MD simulations revealed that counterion mobility, the relative distances between the three partners, and the hydrogen bond lifetimes are more decisive for the response features observed than actual distances between interacting atoms in a complex or the orientation of binding moieties. TBA has been found to yield the highest imprinting factor, also showing a unique dual behavior regarding the interaction with template and fluorescent monomer. Finally, interesting differences between both enantiomers have been observed in both theory and experiment, suggesting true control of enantioselectivity. The contribution concludes with suggestions for translating the findings into actual MIP development. KW - Anion receptors KW - Fluorescence sensing KW - Molecular dynamics simulations KW - Molecularly imprinted polymers KW - Rational design PY - 2018 DO - https://doi.org/10.1021/acs.langmuir.8b00500 SN - 0743-7463 VL - 34 IS - 23 SP - 6963 EP - 6975 PB - American Chemical Society CY - Washington, D.C. AN - OPUS4-45399 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Steger, Simon A1 - Hahn, Oliver T1 - In-situ Raman spectroscopic study of pigments used in modern reverse paintings on glass N2 - The technique of painting on the reverse side of glass was rediscovered by artists in the early 20th century. The artist group “Der Blaue Reiter” around Wassily Kandinsky and Franz Marc got in touch with this technique in 1908 and 1909. In the following years it gained great popularity, especially in Germany. Nevertheless, the technique has not received its due appreciation in art history. It was considered as stained glass. However, the paint layers are applied cold, hence this artistic technique doesn’t involve a firing step. Our multidisciplinary project investigates the art historic backgrounds, the painting techniques and materials of modern reverse paintings on glass. More than 1000 paintings from ~100 artists were discovered in the framework of our project. A selection of 60 paintings could be analyzed using non-invasive, in-situ methods such as Raman and VIS spectroscopy, Diffuse Reflectance Fourier Transform Infrared Spectroscopy (DRIFTS) and X-ray fluorescence (XRF). In this paper we want to point out the key role of Raman spectroscopy for our research. It offers the unique opportunity to measure paint layers from both sides. (front = through the glass; reverse = directly on the paint layer). T2 - XIII International GeoRaman Conference CY - Catania, Italy DA - 10.06.2018 KW - Raman spectroscopy KW - Reverse painting on glass KW - Non-invasive analysis PY - 2018 AN - OPUS4-45400 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit A1 - Dietrich, P. A1 - Thissen, A. A1 - Schwibbert, Karin A1 - Unger, Wolfgang T1 - Quantitative biocide profile measurements by calibrated NAP-XPS N2 - Progress update for the EMPIR-project MetVBadBugs- Quantitative measurement and imaging of drug-uptake by bacteria with antimicrobial resistance. T2 - MetVBadBugs 26 M project meeting CY - South Mimms, UK DA - 05.07.2018 KW - Biofilms KW - Alginate KW - Antibiotics KW - E. coli KW - XPS PY - 2018 AN - OPUS4-45402 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kjaervik, Marit A1 - Schwibbert, Karin A1 - Dietrich, P. A1 - Thissen, A. A1 - Unger, Wolfgang T1 - Surface characterisation of Escherichia coli under various conditions by near-ambient pressure XPS JF - Surface and Interface Analysis N2 - Bacteria are inherently in a hydrated state and therefore not compatible to ultra-high vacuum techniques such as XPS without prior sample preparation involving freeze drying or fast freezing. This has changed with the development of near-ambient pressure (NAP)-XPS, which makes it possible to characterise the bacterial surface with minimal sample preparation. This paper presents NAP-XPS measurements of Escherichia coli under various NAP conditions: at 11 mbar in a humid environment, at 2 mbar after drying in the chamber, pre-dried at 4 mbar, and at 1 mbar after overnight pumping at 10^−4 mbar. The high-resolution spectra of carbon, nitrogen, and oxygen are presented and found to be in general agreement with XPS measurements from freeze-dried and fast-frozen bacteria. However, it was found that the amount of carbon components associated with polysaccharides increases relative to aliphatic carbon during drying and increases further after overnight pumping. This implies that drying has an impact on the bacterial surface. T2 - European conference on applications of surface and interface analysis (ECASIA'17) CY - Montpellier, France DA - 24.09.2018 KW - Bacteria KW - E. coli KW - NAP-XPS PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-454047 DO - https://doi.org/10.1002/sia.6480 SN - 0142-2421 SN - 1096-9918 VL - 50 IS - 11 SP - 996 EP - 1000 PB - John Wiley & Sons CY - Hoboken, New Jersey, USA AN - OPUS4-45404 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Yildirim, Arda T1 - Liquid Crystals Forming a Columnar Mesophase: Structure, Dynamics and Electric Conductivity N2 - The molecular dynamics and ionic conductivity of ionic liquid crystals (ILCs) forming a columnar mesophase, two linear-shaped tetramethylated guanidinium triflates ILCs having different lengths of alkyl chains, were investigated by a combination of Broadband Dielectric Spectroscopy (BDS) and Specific Heat Spectroscopy (SHS). Three processes were detected by BDS; at low temperature γ-process, at higher temperatures α-process and at even higher temperatures conductivity. The γ-process indicates localized fluctuations, and the α-process designates cooperative fluctuations. Slightly different restrictions were found for conductivity processes of LC536 and LC537 due to the slightly different lengths of alky chains. The conductivity mechanisms in the plastic crystalline and the columnar mesophase have been revealed by BDS and different charge carriers were assigned for the different phases. Furthermore, the cooperative dynamics were also probed by SHS. The cooperative dynamics probed by the different techniques (BDS and SHS) compared, and assigned to the different restrictions on the cooperativity due to the difference in the sensitivity of the techniques. T2 - Seminar Vortrag Technische Universität Berlin CY - Berlin, Germany DA - 28.06.2018 KW - Columnar Liquid Crystals KW - Ionic Liquid Crystals PY - 2018 AN - OPUS4-45383 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Metz, Christian A1 - Franz, Philipp A1 - Maierhofer, Christiane A1 - Wachtendorf, Volker A1 - Fischer, C. T1 - Active thermography for quality assurance of 3D-printed polymer structures N2 - Active thermography with flash and halogen light excitation is used as a method for non-destructive testing of 3D-printed polymer components. Test specimens with artificial defects have been generated, using laser sintering and fused layer modeling. These test specimens have been investigated in different measurement configurations with both excitation methods. Afterwards, the different measurement conditions were compared regarding their capability to detect the defects. Furthermore, advanced analysis methods are used, to fully exploit the capabilities of these techniques. T2 - 14th Quantitative InfraRed Thermography Conference CY - Berlin, Germany DA - 25.06.2018 KW - Additive manufacturing KW - Active thermography KW - Artificial weathering PY - 2018 AN - OPUS4-45387 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Metz, Christian A1 - Franz, Philipp A1 - Fischer, C. A1 - Wachtendorf, Volker A1 - Maierhofer, Christiane T1 - Active thermography for quality assurance of 3D-printed polymer structures T2 - DGZfP-Proceedings BB 167 N2 - Additively manufactured test specimens made of polyamide 12 (PA 12) by Laser Sintering (LS) as well as of acrylnitril-butadien-styrol (ABS) by Fused Layer Modeling (FLM), were tested with active thermography. For this, two different excitation methods (flash and impulse excitation) were used and compared, regarding the suitability for the detection of constructed and imprinted defects. To increase the quality of the thermograms, data processing methods like thermal signal reconstruction (TSR) and Fourier-Transformation were applied. Furthermore, the long-term stability of the probes towards environmental stress, like UV-radiation, heat, water contact and frost is being investigated in the presented project with artificial weathering tests. T2 - 14th Quantitative InfraRed Thermography Conference CY - Berlin, Germany DA - 25.06.2018 KW - Additive manufacturing KW - Active thermography KW - Artificial weathering PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-453919 SP - Tu.3.A.2, 1 EP - 9 AN - OPUS4-45391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Illerhaus, Bernhard A1 - Kunisch, E. A1 - Kinne, R. W. T1 - Serial in situ compression of spongiosa cylinder observed by μCT, compared to simulated stress, strain, and movement T2 - Proceedings of 12th ECNDT, Gothenburg, Sweden N2 - Minimally invasive injection of calcium phosphate cement into bone defects in aged sheep vertebrae has been used as a model for the treatment of osteoporotic vertebral fractures. One of the therapeutic criteria is a compression test of non-treated or treated vertebral bodies. In the present study, an in situ compression test with a stepwise load increase was performed with small spongiosa cylinders from the vertebrae under continuous monitoring by μCT. This allows localization of bone cracks and the visualization of correct placement and form of the bone cylinder. In addition, the effects of an uneven load distribution on the sample due to an irregular shape and a subsequent underperformance of the test sample can be excluded by controlling its shape under increasing load. There was a good agreement between the measured data and those obtained by simulated load-dependent transformation on the basis of a digital volume correlation between consecutive compression tests on the bone surface under the assumption of homogeneous bone material. Mechanic simulation was executed by directly using structural voxel data, resulting in maps of Von Mise stresses and predicted displacements. T2 - 12th ECNDT CY - Gothenburg, Sweden DA - 11.6.2018 KW - Computed tomography KW - In-situ compression KW - Simulation PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-453317 SN - 978-91-639-6217-2 SP - 0162, 1 EP - 7 AN - OPUS4-45331 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Makowski, Maike A1 - Werneburg, M. A1 - Jung, Christian A1 - Haase, H. A1 - Koch, Matthias T1 - Non-invasive GC-MS Analysis of Trichodiene as Volatile Mycotoxin Biomarker in Cereals N2 - Due to the increasing consumption of cereals worldwide, monitoring of growth, storage and processing is becoming more crucial. Particularly when stored, infested grains breed fungal clusters (“hot spots”) in which mycotoxins greatly exceed allowed maximum levels. Because of their unpredictable presence, current sampling and procedures for mycotoxin analysis are complex and contain invasive and cost intensive steps. A possible approach to avoid sampling inaccuracies is the non-invasive analysis of the homogeneous gas phase above the crops, instead of analyzing random samples. However, this procedure requires microbial volatile organic compounds (MVOC´s) being released by the samples. Previous investigations revealed trichodiene to be a precursor in trichothecenes biosynthesis – one of the largest mycotoxin groups with more than 180 compounds. Due to its non-functionalized sesquiterpene structure, quantification of trichodiene using Headspace GC-MS methods is possible (e.g. [1]). Thereby, it could be used as biomarker for trichothecene contamination in foodstuff. However, further studies are necessary. The correlation between trichodiene concentration in the gas phase and trichothecenes mass fraction in the sample must be examined closely to draw conclusions about the trichothecene content in samples. Realizing this idea, would widely extend the applicability of trichodiene and enormously simplify trichothecene quantification. Hence, this first step of an ongoing study aims to develop a laboratory reference method using trichodiene as volatile biomarker to quantify trichothecenes in cereals. Static headspace and SPME-enrichment coupled to gas chromatography with mass spectrometry (GC-MS) were employed. In a second step, this reference method is intended to validate new approaches for fast on-site screening of trichodiene in cereals. T2 - 40th Mycotoxin Workshop CY - Munich, Germany DA - 11.06.2018 KW - Trichodiene KW - Gaschromatography-Mass Spectrometry KW - Mycotoxin Biomarker PY - 2018 AN - OPUS4-45314 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nutsch, A. A1 - Dill, S. A1 - Kamleitner, I. A1 - Sehorz, A. A1 - Schwarzenberger, M. A1 - Streeck, C. A1 - Beckhoff, B. A1 - Merz, H. A1 - Recknagel, Sebastian T1 - A Methodology to Obtain Traceability and Validation of Calibration Samples for Thin Metal Alloy Layers for X-Ray Fluorescence Tools N2 - Statistic process control as well as process capability demand for calibrated determination of layer thicknesses in various industries, e.g. automotive, aerospace, microelectronics manufacturing. Calibration requires well know and well characterized samples. A calibration laboratory accredited according to DIN EN ISO 17025 has the objective to distribute standards traceable to SI units to industrial laboratories for quality control of manufacturing of various products. Especially, the thickness determination of thin metallic coatings e.g. from galvanic processes or layer deposition using X-Ray Fluorescence can be significantly improved by customized calibration samples. This is essential as the measurement uncertainty directly correlates to the capability performing reliable control of processes with high yield. For calibration laboratories, the validation of results using round robins and the direct comparison to national metrology institutes is a prerequisite to demonstrate the competence to perform calibration services. In this paper a strategy to obtain traceability and validation for thin alloy layers as well as first results are presented. The combined use of the accredited method for determination of mass per area from measurement of mass and area combined with standard free X-Ray Fluorescence as well as chemical analysis of dissolved samples with thin layers is deployed for material systems as NixZn1-x as well as NixP1-x. The obtained results are compared to reference free X-Ray Fluorescence at the BESSY II laboratories of Physikalisch-Technische Bundesanstalt. An excellent agreement of the obtained measured values as mass per unit area and alloy concentrations from the different applied methods within the measurement uncertainty was observed for NixP1-x showing the successful performed traceability of the calibration samples to SI units in combination with a validation of results by national metrology institutes and the round robin approach. T2 - European Conference on X-Ray Spectrometry CY - Ljubljana, Slowenia DA - 24.06.2018 KW - Traceability KW - Thin metal alloy layers KW - X-ray fluorescence PY - 2018 AN - OPUS4-45317 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kakoulides, E. A1 - Stathoudaki, H. A1 - Alexopoulos, C. A1 - Philipp, Rosemarie T1 - Development of Certified Reference Materials for the calibration of breath analyzers N2 - IAPR participates in the EMPIR 16SRT02, entitled ‘Certified forensic alcohol reference materials - ALCOREF’ funded by EURAMET as an external funded partner. The Research in this project will address the needs for better enforcement of drink-driving legislation in several European countries, by building up long-term capacities for the production and certification of forensic alcohol reference materials, suitable for the calibration of evidential breath alcohol analyzers. The certification procedure includes characterization of the materials, assessment of homogeneity, stability, and uncertainty estimation. An interlaboratory comparison will be conducted to test the materials and capabilities developed. EMPIR 16SRT02-ALCOREF project is coordinated by BAM (DE). T2 - 7th National Metrology Congress CY - Athens, Greece DA - 11.05.2018 KW - Certified reference materials KW - Metrology institute KW - Calibration KW - Uncertainty PY - 2018 N1 - Sprache der Posterpräsentation: Griechisch AN - OPUS4-45321 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer A1 - Maierhofer, Christiane A1 - Heckel, Thomas A1 - Brackrock, Daniel A1 - Gower, M. A1 - Lodeiro, M. A1 - Baker, G. T1 - Quantitative comparison of different non-destructive techniques for the detection of artificial defects in GFRP T2 - Proceedings of the 12th ECNDT N2 - In order to test their suitability different non-destructive methods were performed to inspect a GFRP plate with artificial defects. These defects were manufactured by means of thin PTFE sheets inserted between two plies in three different depth. The inspection methods were microwave reflection, flash thermography and phased array ultrasonics, all applied to the same specimen. Selected results are shown for all methods demonstrating opportunities and limits of the particular inspection methods. The achieved detection limits and further application aspects are compared directly to provide a useful information for the planning of inspection tasks. T2 - ECNDT CY - Gothenburg, Sweden DA - 11.06.2018 KW - Fiber resisted polymers KW - Non-destructive testing KW - Thermographic testing KW - Ultrasonic testing PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-453728 SP - ECNDT-0247-2018 AN - OPUS4-45372 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krankenhagen, Rainer A1 - Ziegler, Mathias A1 - Maierhofer, Christiane ED - Maldague, X. T1 - Systematic errors in the evaluation of uncorrected data from thermographic lock-in measurements T2 - Proceedings of the 14th QIRT Conference 2018 N2 - Lock-in thermography (LT) is based on the correct evaluation of phase differences between the temperature oscillations at different surface regions of the object under test during periodic heating. Since the usual heating procedures contain a DC component, the actual heating pattern achieved is not harmonic. This causes systematic deviations when phase differences are determined by means of harmonic analysis, e.g. with FFT analysis. The resulting errors depend clearly on the ratio between DC and AC amplitude, which is demonstrated at simulated and experimentally recorded temperature transients. Further experimental LT data obtained by different oscillating energy inputs showed a variety of possible shapes of transients with different DC components. T2 - 14th QIRT Conference CY - Berlin, Germany DA - 26.06.2018 KW - NDT KW - Lock-in Thermography KW - FFT PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-453768 SP - 539 EP - 547 PB - QIRT Council AN - OPUS4-45376 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Würth, Christian A1 - Fischer, S. A1 - Grauel, Bettina A1 - Alivisatos, A. P. A1 - Resch-Genger, Ute T1 - Quantum Yields, Surface Quenching, and Passivation Efficiency for Ultrasmall Core/Shell Upconverting Nanoparticles N2 - We synthesized and characterized a set of ultrasmall hexagonal-phase NaGdF4: 20% Yb3+, 2% Er3+ upconversion nanoparticles with core diameters of 3.7 ± 0.5 nm. In order to assess passivation effects and the influence of possible core−shell intermixing and to identify optimum particle structures for combined imaging in the visible and near-infrared (vis−NIR: 410−850 nm) and short-wave infrared (SWIR: 1520 nm), NaYF4 shells of varying thicknesses (monolayer to 10 nm) were introduced and the influence of this parameter on the upconversion and downshifting photoluminescence of these particles was studied at different excitation power densities. This included excitation power-dependent emission spectra, slope factors, quantum yields, and excited state decay kinetics. These measurements revealed enhancement factors of the upconversion quantum yield of >10 000 in the low power region and an excitation power density-independent quantum yield of the downshifted emission at 1520 nm between 0.1 and 14%. The optimized shell thickness for combined vis and SWIR imaging was identified as 5 nm. Moreover, lifetimes and quantum yields can be continuously tuned by shell thickness which can be exploited for lifetime multiplexing and encoding. The fact that we did not observe a saturation of the upconversion quantum yield or the excited state decay kinetics with increasing shell thickness is ascribed to a strong intermixing of the active core with the inert shell during the shelling procedure. This indicates the potential of spectroscopic tools to detect cation intermixing. KW - Nanoparticle KW - Upconversion KW - Quenching PY - 2018 DO - https://doi.org/10.1021/jacs.8b01458 IS - 140 SP - 4922 EP - 4928 PB - American Chemical Society AN - OPUS4-45378 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Kotschate, Daniel T1 - New technologies for air-coupled ultrasonic transducers N2 - Air-coupled ultrasonic testing (ACUT) has experienced rapid growth within the last years. It is especially well suited to inspection of lightweight structures consisting of composite materials and adhesive joints. Uniform coupling and easy maintenance are its advantages compared to contact technique. However, the impedance mismatch between the transducer and air poses a major challenge to the development of ACUT transducers. Commercially available air-coupled transducers consist of a piezocomposite material and matching layers. Their fabrication is difficult in handling and their signal-to-noise ratio sometimes not sufficient for various testing requirements. However, there are several innovative approaches using other materials and other physical principles to transmit and receive an ultrasonic pulse. We present a review of the latest advances in research on air-coupled transducers for non-destructive testing, including previously unpublished results. We recognize two major directions as most promising: ferroelectrets and thermoacoustic transducers. Ferroelectrets are charged cellular polymers exhibiting piezoelectric properties. Their small acoustic impedance is matched to air better than matching layers applied in conventional air-coupled transducers. Applying bias voltage to a ferroelectret receiver is the latest development in this field, which increased the received signal by 12 to 15 dB. Thermoacoustic transducers use heat to initiate an ultrasonic wave, acting as transmitters. The working principle is known from nature as thunder and lightning: thermal energy of an electrically heated material, which can also be air, is converted into acoustic energy. Some thermoacoustic transmitters consist of a conductive layer with a thickness in the nanometer range deposited on a solid substrate. Another possibility is to use an electric spark. For the first time, measurements of the sound field of an electric spark up to 500 kHz were performed. Thermoacoustic transducers enable excitation of extremely broadband pulses while producing high pressure levels, which opens new possibilities for advanced signal processing. T2 - 12th European conference on Non-Destructive Testing CY - Gothenburg, Sweden DA - 11.06.2018 KW - Transducer KW - Air-coupled ultrasonic testing KW - Atmospheric pressure plasma KW - Cellular polypropylene KW - Ferroelectret PY - 2018 AN - OPUS4-45304 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate A1 - Kotschate, Daniel T1 - New technologies for air-coupled ultrasonic transducers T2 - 12th European conference on Non-Destructive Testing N2 - Air-coupled ultrasonic testing (ACUT) has experienced rapid growth within the last years. It is especially well suited to inspection of lightweight structures consisting of composite materials and adhesive joints. Uniform coupling and easy maintenance are its advantages compared to contact technique. However, the impedance mismatch between the transducer and air poses a major challenge to the development of ACUT transducers. Commercially available air-coupled transducers consist of a piezocomposite material and matching layers. Their fabrication is difficult in handling and their signal-to-noise ratio sometimes not sufficient for various testing requirements. However, there are several innovative approaches using other materials and other physical principles to transmit and receive an ultrasonic pulse. We present a review of the latest advances in research on air-coupled transducers for non-destructive testing, including previously unpublished results. We recognize two major directions as most promising: ferroelectrets and thermoacoustic transducers. Ferroelectrets are charged cellular polymers exhibiting piezoelectric properties. Their small acoustic impedance is matched to air better than matching layers applied in conventional air-coupled transducers. Applying bias voltage to a ferroelectret receiver is the latest development in this field, which increased the received signal by 12 to 15 dB. Thermoacoustic transducers use heat to initiate an ultrasonic wave, acting as transmitters. The working principle is known from nature as thunder and lightning: thermal energy of an electrically heated material, which can also be air, is converted into acoustic energy. Some thermoacoustic transmitters consist of a conductive layer with a thickness in the nanometer range deposited on a solid substrate. Another possibility is to use an electric spark. For the first time, measurements of the sound field of an electric spark up to 500 kHz were performed. Thermoacoustic transducers enable excitation of extremely broadband pulses while producing high pressure levels, which opens new possibilities for advanced signal processing. T2 - 12th European conference on Non-Destructive Testing CY - Gothenburg, Sweden DA - 11.06.2018 KW - Air-coupled ultrasonic testing KW - Atmospheric pressure plasma KW - Cellular polypropylene KW - Ferroelectret KW - Transducer PY - 2018 SP - ECNDT-0608-2018, 1 EP - 9 AN - OPUS4-45209 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Grager, J.-C. A1 - Kotschate, Daniel A1 - Gamper, J. A1 - Gaal, Mate A1 - Pinkert, K. A1 - Mooshofer, H. A1 - Goldammer, M. A1 - Grosse, C. U. T1 - Advances in air-coupled ultrasonic testing combining an optical microphone with novel transmitter concepts T2 - 12th European conference on Non-Destructive Testing N2 - Air-coupled ultrasound (ACU) is increasingly used for automated and contactless inspection of large-scale composite structures as well as for non-destructive testing (NDT) of water-sensitive or porous materials. The major challenge to overcome using ACU in NDT is the enormous loss of ultrasonic energy at each solid-air interface caused by the high acoustic impedance mismatch. Resonant low-frequency piezoceramic transducers are specially designed to achieve high sound pressure levels. For an expanded use of this technique, however, the spatial resolution needs to be increased. Recent studies of our collaborative research group demonstrated the successful application of a resonance-free, highly sensitive receiver that uses a Fabry-Pérot etalon instead of piezoceramic materials or membranes. However, to reach the full potential of this broadband small-aperture optical microphone, novel transmitter concepts have to be developed and evaluated for advanced NDT applications. Different types of transmitter were tested in combination with the optical microphone acting as receiver and they were compared to conventional piezoceramic transducers in through-transmission mode. Monolithic carbon fiber-reinforced plastics (CFRP) and CFRP sandwich structures containing different defect types were inspected. Presented results are processed as C-scan images and further evaluated for spatial resolution, signal-to-noise ratio and sensitivity of each measurement setup. Novel transmitter concepts, such as ferroelectret and thermoacoustic emitters, show promising findings with a considerably improved time and spatial resolution for ACU-NDT. T2 - 12th European conference on Non-Destructive Testing CY - Gothenburg, Sweden DA - 11.06.2018 KW - Air-coupled ultrasonic testing KW - Optical microphone KW - Thermoacoustic KW - Cellular polypropylene KW - Ferroelectret KW - Transducer PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-452114 SP - ECNDT-0166-2018, 1 EP - 10 AN - OPUS4-45211 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Strangfeld, Christoph T1 - Moisture testing and mapping N2 - Non-destructive testing of moisture in building materials T2 - NDT&E Advanced Training Workshop CY - Berlin, Germany DA - 27.06.2018 KW - Building materials KW - Concrete KW - Moisture measurement PY - 2018 AN - OPUS4-45348 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Niederleithinger, Ernst T1 - Buildings: Seismology and Strctural Health Monitoring N2 - Overview of seismological concepts unsed in nondestructive testing in civil engineering T2 - Fourth TIDES Advanced Training School CY - Prague, Czech Repubilc DA - 01.07.2018 KW - Geophysics KW - Seismology KW - Interferometry KW - Structural health monitoring KW - Nondestructive testing PY - 2018 AN - OPUS4-45361 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Meiling, T. T. A1 - Schürmann, Robin A1 - Vogel, Stefanie A1 - Ebel, Kenny A1 - Nicolas, C. A1 - Milosavljević, A. R. A1 - Bald, Ilko T1 - Photophysics and chemistry of nitrogen-doped carbon nanodots with high photoluminescence quantum yield JF - The Journal of Physical Chemistry C N2 - Fluorescent carbon nanodots (CNDs) are very promising nanomaterials for a broad range of applications because of their high photostability, presumed selective luminescence, and low cost at which they can be produced. In this respect, CNDs are superior to well-established semiconductor quantum dots and organic dyes. However, reported synthesis protocols for CNDs typically lead to low photoluminescence quantum yield (PLQY) and low reproducibility, resulting in a poor understanding of the CND chemistry and photophysics. Here, we report a one-step synthesis of nitrogen-doped carbon nanodots (N-CNDs) from various carboxylic acids, Tris, and ethylenediaminetetraacetic acid resulting in high PLQY of up to 90%. The reaction conditions in terms of starting materials, temperature, and reaction time are carefully optimized and their influence on the photophysical properties is characterized. We find that citric acid-derived N-CNDs can result in a very high PLQY of 90%, but they do not Show selective luminescence. By contrast, acetic acid-derived N-CNDs show selective luminescence but a PLQY of 50%. The chemical composition of the surface and core of these two selected N-CND types is characterized among others by high-Resolution synchrotron X-ray photoelectron spectroscopy using single isolated N-CND clusters. The results indicate that photoexcitation occurs in the N-CND core, whereas the emission properties are determined by the N-CND surface groups. KW - Carbon nanodots KW - Fluorescence KW - Synchrotron XPS PY - 2018 DO - https://doi.org/10.1021/acs.jpcc.8b00748 SN - 1932-7447 VL - 122 IS - 18 SP - 10217 EP - 10230 PB - American Chemical Society CY - Washington, DC AN - OPUS4-45426 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ziegler, Mathias A1 - Thiel, Erik A1 - Studemund, T. T1 - Thermography using a 1D laser array – From planar to structured heating JF - Materials Testing N2 - In the field of optically excited thermography, flash lamps (impulse shaped planar heating) and halogen lamps (modulated planar heating) have become established for the specific regimes of impulse and lock-in thermography. Flying-spot laser thermography is implemented by means of a rasterized focused laser, e. g. for crack detection (continuous wave operation) and photothermal material characterization (high-frequency modulated). The availability of novel technologies, i. e. fast and high-resolution IR cameras, brilliant innovative light sources and high-performance data acquisition and processing technology will enable a paradigm shift from stand-alone photothermal and thermographic techniques to uniform quantitative measurement and testing technology that is faster and more precise. Similar to an LED array, but with irradiance two orders of magnitude higher, a new type of brilliant laser source, i. e. the VCSEL array (vertical-cavity surface-emitting laser), is now available. This novel optical energy source eliminates the strong limitation to the temporal dynamics of established light sources and at the same time is spectrally clearly separated from the detection wavelength. It combines the fast temporal behavior of a diode laser with the high optical irradiance and the wide illumination area of flash lamps. In addition, heating can also be carried out in a structured manner, because individual areas of the VCSEL array can be controlled independently of each other. This new degree of freedom enables the development of completely new thermographic NDT methods. KW - Thermography KW - Laser thermography KW - Laser KW - Lock-in KW - VCSEL KW - Thermal wave KW - Photothermal PY - 2018 UR - https://www.hanser-elibrary.com/doi/abs/10.3139/120.111209 DO - https://doi.org/10.3139/120.111209 SN - 0025-5300 VL - 60 IS - 7-8 SP - 749 EP - 757 PB - Carl Hanser Verlag CY - München AN - OPUS4-45482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Bonnerot, Olivier A1 - Bosch, S. A1 - Rabin, Ira A1 - Hahn, Oliver T1 - Scientific service project Z02 at the CSMC: Material-science methods of reconstructing the history of manuscripts N2 - Z02 is one of the three technically supporting projects at the CSMC. In collaboration with Z01 and Z03, it aims at bridging the gap between humanities and natural sciences and technology. To that purpose, we set up a laboratory with a range of high-end instruments, most of them mobile, allowing thorough non-destructive analysis of manuscripts. In addition to working on constantly improving the laboratory and the methods of analysis, a substantial part of our activities is dedicated to service, by supporting different research projects conducted at the center. In this talk, we will present our equipment and the possibilities offered by the different techniques available regarding the different kinds of missions: typology and classification of inks, provenance studies, recovery of faded inscriptions and palimpsests, reconstruction of the history of manuscripts, authentication and dating. We will give a brief overview of our past and ongoing activities in the frame of the second phase of the CSMC. Finally, a selection of three projects will be presented in greater detail to highlight the possibilities of our laboratory and the diversity of missions which can be carried out: - Support of project C08 on East Frankish manuscripts containing collections of formulae - Identifying color materials applied in Muhammad Juki's Shahnamah with non-invasive combined methods - Checking for the presence of metals in the Herculaneum papyri T2 - 3rd International Conference on Natural Sciences and Technology in Manuscript Analysis CY - Hamburg, Germany DA - 13.06.2018 KW - CSMC KW - Manuscript KW - Ink KW - Pigment PY - 2018 AN - OPUS4-45504 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kjaervik, Marit A1 - Dietrich, P. A1 - Thissen, A. A1 - Schwibbert, Karin T1 - Surface characterisation of biological samples by near-ambient pressure XPS N2 - A presentation held for the seminar "Ausgewählte analytische Methoden der Physik" hosted by Prof. Birgit Kanngießer at TU Berlin. The first part focus on depth-dependent XPS-measurements (XPS, synchrotron HAXPES) to obtain a concentration profile of iodine in an artificial biofilm. In the second part, NAP-XPS measurements of various bacterial samples are presented. T2 - Forschungsseminar "Ausgewählte analytische Methoden der Physik", TU Berlin CY - Berlin, Germany DA - 17.07.2018 KW - Biofilms KW - Alginate KW - Agarose KW - HAXPES KW - NAP-XPS PY - 2018 AN - OPUS4-45505 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Puthiyaveettil, N. A1 - Ziegler, Mathias A1 - Myrach, Philipp A1 - Unnikrishnakurup, Sreedhar A1 - Krishnamurthy, C. V. A1 - Balasubramaniam, K. T1 - Numerical study of laser line thermography for crack detection at high temperature N2 - The detection of cracks before the failure is highly significant when it comes to safety-relevant structures. Crack detection in metallic samples at high surface temperature is one of the challenging situation in manufacturing industries. Laser thermography has already proved its detection capability of surface cracks in metallic samples at room temperature. In this work a continuous wave (CW) laser use to generate a laser, which is using to scan the metal surface with notch. The corresponding heat distribution on the surface monitored using infrared thermal (IR) camera. A simplified 3D model for laser thermography is developed and validated with experimental results. A dedicated image processing algorithm developed to improve the detectability of the cracks. To understand the dependency of surface temperature, laser power, laser scanning speed etc. in defect detection, we carried out parametric studies with our validated model. Here we report the capability of laser thermography in crack detection at elevated temperature. T2 - Conference QIRT 2018 CY - Berlin, Germany DA - 25.06.2018 KW - Thermography KW - Laser Thermography KW - Cracks PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-454441 DO - https://doi.org/10.21611/qirt.2018.076 AN - OPUS4-45444 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias A1 - Thiel, Erik A1 - Ahmadi, Samim T1 - Lock-in Thermography using High-Power Laser Sources N2 - Optical lock-in thermography is a completely contactless and very sensitive NDT technique. As an optical source of energy, incandescent lamps are most commonly used because they are relatively inexpensive and offer high irradiances at the test specimen. However, they are strongly restricted by their low modulation bandwidth with a maximum modulation frequency of only about 1 Hz. The use of high-power kilowatt-class laser sources, e.g. diode laser arrays, pushes this constraint beyond 100 Hz. This allows for the exploration of the near-surface region of metals and layer systems with better and more accurate penetration depth and depth resolution. Moreover, these lasers are virtually free of any additional thermal radiation that could interfere with the “true” thermal response emitted from the heated sample. In turn, they can be easily used in a one-sided test configuration. We present current activities with kilowatt-class high-power laser sources for advanced lock-in thermography and focus on the application of laser arrays that offer a very high irradiation strength over a large sample area beyond the mentioned advantages. T2 - 12th European Conference on Non-destructive Testing CY - Gothenburg, Sweden DA - 11.06.2018 KW - Thermography KW - Laser Thermography KW - Lock-in Thermography PY - 2018 AN - OPUS4-45445 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias A1 - Thiel, Erik A1 - Ahmadi, Samim T1 - Lock-in Thermography using High-Power Laser Sources T2 - Proceedings of the 12th European Conference on Non-destructive Testing 2018 N2 - Optical lock-in thermography is a completely contactless and very sensitive NDT technique. As an optical source of energy, incandescent lamps are most commonly used because they are relatively inexpensive and offer high irradiances at the test specimen. However, they are strongly restricted by their low modulation bandwidth with a maximum modulation frequency of only about 1 Hz. The use of high-power kilowattclass laser sources, e.g. diode laser arrays, pushes this constraint beyond 100 Hz. This allows for the exploration of the near-surface region of metals and layer systems with better and more accurate penetration depth and depth resolution. Moreover, these lasers are virtually free of any additional thermal radiation that could interfere with the “true” thermal response emitted from the heated sample. In turn, they can be easily used in a one-sided test configuration. We present current activities with kilowatt-class highpower laser sources for advanced lock-in thermography and focus on the application of laser arrays that offer a very high irradiation strength over a large sample area beyond the mentioned advantages. T2 - 12th European Conference on Non-destructive Testing CY - Gothenburg, Sweden DA - 11.06.2018 KW - Thermography KW - Laser Thermography KW - Lock-in Thermography PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-454466 UR - http://cdn.ecndt2018.com/wp-content/uploads/2018/05/ecndt-0139-2018.pdf SN - 978-91-639-6217-2 SP - ECNDT-0139-2018,1 EP - 7 AN - OPUS4-45446 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Ziegler, Mathias A1 - Thiel, Erik A1 - Ahmadi, Samim T1 - Lock-in Thermography using High-Power Laser Sources N2 - Optical lock-in thermography is a completely contactless and very sensitive NDT technique. As an optical source of energy, incandescent (i.e. halogen) lamps are most commonly used because they are relatively inexpensive and offer high irradiances at the test site. However, they are strongly restricted by their low modulation bandwidth with a maximum modulation frequency of only about 1 Hz. The use of high-power kilowatt-class laser sources, e.g. diode laser arrays, pushes this constraint beyond 100 Hz, see Fig.1. This allows for the exploration of the near-surface region of metals and layer systems with better and more accurate penetration depth and depth resolution. Moreover, these lasers are virtually free of any additional thermal radiation that could interfere with the “true” thermal response emitted from the heated sample. In turn, they can be easily used in a one-sided test configuration. Using the one-dimensional solution to the thermal heat diffusion equation together with the absorptance of the material which is illuminated with a harmonically modulated light source, we can calculate the temperature oscillation at the surface of a solid. As a second step, we calculate the corresponding oscillation of the total thermal emission using Stefan-Boltzmann law as a first order approximation and taking into account the emissivity of the material. Within this framework we can calculate the minimal irradiance of a light source necessary to provoke a measurable signal within a thermographic camera at a noise equivalent temperature difference (NETD) of 30 mK. In Fig. 2 this relationship is displayed for a wide spectrum of modulation frequencies and for a number of different light sources scaled to the same electrical input power and illumination area. Using this figure, it is now easily possible to analyze the range of materials to be tested using lock-in thermography, since only the materials (dotted lines) below the irradiance-vs-frequency curves (solid lines) are heated in excess of the camera’s NETD. This figure clearly shows that laser sources considerably increase the application range of lock-in thermography, since especially for metals with a high reflectance and high thermal diffusivity a high irradiance is vitally important to allow for lock-in texting. We present current activities with kilowatt-class high-power laser sources for advanced lock-in thermography and focus on the application of laser arrays that offer a very high irradiation strength over a large sample area beyond the mentioned advantages. T2 - Conference QIRT 2018 CY - Berlin, Germany DA - 25.06.2018 KW - Thermography KW - Laser Thermography KW - Lock-in Thermography PY - 2018 AN - OPUS4-45449 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Burgholzer, P. A1 - Berer, T. A1 - Ziegler, Mathias A1 - Thiel, Erik A1 - Ahmadi, Samim A1 - Gruber, J. A1 - Mayr, G. A1 - Hendorfer, G. T1 - Blind structured illumination as excitation for super-resolution photothermal radiometry T2 - Proceedings of the 14th QIRT Conference 2018 N2 - Using an infrared camera for radiometric imaging allows the contactless temperature measurement of multiple surface pixels simultaneously. From the measured surface data, a sub-surface structure, embedded inside a sample or tissue, can be reconstructed and imaged when heated by an excitation light pulse. The main drawback in radiometric imaging is the degradation of the spatial resolution with increasing depth, which results in blurred images for deeper lying structures. We circumvent this degradation with blind structured illumination, combined with a non-linear joint sparsity reconstruction algorithm. The ground-breaking concept of super-resolution can be transferred from optics to thermographic imaging. T2 - Conference QIRT 2018 CY - Berlin, Germany DA - 25.06.2018 KW - Thermography KW - Laser thermography KW - Super resolution PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-454506 SN - 978-3-940283-94-8 DO - https://doi.org/10.1080/17686733.2019.1655247 SP - We.3.A.2, 1 EP - 7 AN - OPUS4-45450 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kage, Daniel A1 - Fischer, Linn A1 - Hoffmann, Katrin A1 - Thiele, T. A1 - Schedler, U. A1 - Resch-Genger, Ute T1 - Close spectroscopic look at dye-stained polymer microbeads JF - The Journal of Physical Chemistry C N2 - Dye-stained micrometer-sized polymer beads are important tools in the life sciences with applications in biomedical, biochemical, and clinical research. Here, bead-based assays are increasingly used, for example, in DNA sequencing and the detection of autoimmune diseases or pathogenic microorganisms. Moreover, stained beads are employed as calibration tools for fluorescence microscopy and flow cytometry methods with increasing complexity. To address the requirements concerning the relevant fluorescence features, the spectroscopic properties of representative polymer beads with diameters ranging from about 1 to 10 μm stained with varying concentrations of rhodamine 6G were systematically assessed. The observed dependence of the spectral properties, fluorescence decay kinetics, and fluorescence quantum yields on bead size and dye loading concentration is attributed to different fluorescence characteristics of fluorophores located in the particle core and near-surface dye molecules. Supported by the fluorescence anisotropy measurements, the origin of the observed alteration of fluorescence features is ascribed to a combination of excitation energy transfer and polarity-related effects that are especially pronounced at the interface of the bead and the surrounding medium. The results of our studies underline the need to carefully control and optimize all Parameters that can affect the fluorescence properties of the dye-stained beads. KW - Fluorophore KW - Polymer particles KW - Photophysics KW - Life sciences KW - Standards PY - 2018 DO - https://doi.org/10.1021/acs.jpcc.8b02546 SN - 1932-7447 VL - 122 IS - 24 SP - 12782 EP - 12791 PB - ACS Publications CY - Washington, DC AN - OPUS4-45453 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Lisec, Jan A1 - Jaeger, C. ED - Antonio, C. T1 - Statistical and Multivariate Analysis of MS-Based Plant Metabolomics Data T2 - Plant Metabolomics: Methods and Protocols N2 - Raw data from metabolomics experiments are initially subjected to peak identification and signal deconvolution to generate raw data matrices m × n, where m are samples and n are metabolites. We describe here simple statistical procedures on such multivariate data matrices, all provided as functions in the programming environment R, useful to normalize data, detect biomarkers, and perform sample classification. KW - Mass-Spectrometry KW - Multivariate Statistics PY - 2018 SN - 978-1-4939-7819-9 SN - 978-1-4939-7818-2 DO - https://doi.org/10.1007/978-1-4939-7819-9_20 SN - 1064-3745 SN - 1940-6029 VL - 1778 SP - Chapter 20, 285 EP - 296 PB - Springer-Verlag AN - OPUS4-45492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lisec, Jan A1 - Hoffmann, F. A1 - Jaeger, C. A1 - Bhattacharya, A. A1 - Schmitt, C. A. T1 - Nontargeted Identification of Tracer Incorporation in High- Resolution Mass Spectrometry JF - Analytical Chemistry N2 - “Fluxomics” refers to the systematic analysis of metabolic fluxes in a biological system and may uncover novel dynamic properties of metabolism that remain undetected in conventional metabolomic approaches. In labeling experiments, tracer molecules are used to track changes in the isotopologue distribution of metabolites, which allows one to estimate fluxes in the metabolic network. Because unidentified compounds cannot be mapped on pathways, they are often neglected in labeling experiments. However, using recent developments in de novo annotation may allow to harvest the information present in these compounds if they can be identified. Here, we present a novel tool (HiResTEC) to detect tracer incorporation in high-resolution mass spectrometry data sets. The software automatically extracts a comprehensive, nonredundant list of all compounds showing more than 1% tracer incorporation in a nontargeted fashion. We explain and show in an example data set how mass precision and other filter heuristics, calculated on the raw data, can efficiently be used to reduce redundancy and noninformative signals by 95%. Ultimately, this allows to quickly investigate any labeling experiment for a complete set of labeled compounds (here 149) with acceptable false positive rates. We further re-evaluate a published data set from liquid chromatography-electrospray ionization (LC-ESI) to demonstrate broad applicability of our tool and emphasize importance of quality control (QC) tests. HiResTEC is provided as a package in the open source software framework R and is freely available on CRAN. KW - Fluxomics KW - R package KW - Mass-Spectrometry PY - 2018 DO - https://doi.org/10.1021/acs.analchem.8b00356 VL - 90 IS - 12 SP - 7253 EP - 7260 PB - ACS Publications AN - OPUS4-45493 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kruschwitz, Sabine A1 - Ebell, Gino A1 - Shen, J. T1 - Towards Data Based Corrosion Analysis of Concrete with Supervised Machine Learning T2 - Structural Materials Technology (SMT 2018) and the International Symposium Non-Destructive Testing in Civil Engineering N2 - Half-Cell-Potential Mapping (HP) is the most popular non-destructive testing (NDT) method for the detection of active corrosion in reinforced concrete. HP is influenced by parameters such as moisture and chloride gradients in the component. The sensitivity to the spatially small, but dangerous pitting is low. In this study we show how additional measurement information can be used with multi-sensor data fusion to improve the detection performance and to automate data evaluation. The fusion is based on supervised machine learning (SML). SML are methods that recognize relationships in (sensor) data based on given labels. We use SML to distinguish "defective" and "intact" labeled areas in our dataset. It consists of 18 measurement - each contains HP, ground radar, microwave moisture and Wenner resistance data. Exact labels for changing environmental conditions were available in a laboratory study on a reinforced concrete slab, which deteriorated controlled and accelerated. The deterioration progress was monitored continuously and corrosion was generated targeted at a predefined location. The detection results are quantified and statistically evaluated. The SML results shows a significant improvement over the best single method (HP). T2 - NDE/NDT for Highway and Bridges: Structural Materials Technology (SMT 2018) and the International Symposium Non-Destructive Testing in Civil Engineering (NDT-CE 2018) CY - New Brunswick, NJ, USA DA - 27.08.2018 KW - Data fusion KW - Half-cell potential mapping KW - Data based decision making KW - Non-destuctive corrosion testing of concrete KW - Supervised machine learning PY - 2018 SP - 1 EP - 7 AN - OPUS4-45512 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Rühle, Bastian A1 - Resch-Genger, Ute A1 - Kembuan, C A1 - Graf, C T1 - Gold-shell coated NaYF4:Er3+, Yb3+ nanoparticles for the enhancement of fluorescence emission N2 - In the present work, we aim to explore how far the UCNP emission intensity can be enhanced by the aid of plasmonic interactions using a gold shell. The distance between the UCNP core and the gold shell is varied by adding a silica spacer of different thicknesses. The synthetic conditions for obtaining UCNP@SiO2@Au core-shell nanoparticles with precisely tuneable silica shell thicknesses were investigated. A gold shell on the UCNP@SiO2 nanoparticles is expected to give rise to a noticeable enhancement of particle brightness and fluorescence, given that the thicknesses of the silica shell and the gold coating can be controlled and fine-tuned. First single particle studies revealing shortening of the Er3+ lifetimes suggest that plasmonic enhancement occurs. T2 - 2nd Conference and Spring School on Properties, Design and Applications of Upconversion Nanomaterials CY - Valencia, Spain DA - 02.04.2018 KW - Upconversion nanoparticles KW - Silica coating KW - Plasmonic enhancement PY - 2018 AN - OPUS4-44958 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schumacher, David A1 - Sharma, R. A1 - Grager, J.-C. A1 - Schrapp, M. T1 - Scatter and beam hardening reduction in industrial computed tomography using photon counting detectors JF - Measurement Science and Technology N2 - Photon counting detectors (PCD) offer new possibilities for x-ray micro computed tomography (CT) in the field of non-destructive testing. For large and/or dense objects with high atomic numbers the problem of scattered radiation and beam hardening severely influences the image quality. This work shows that using an energy discriminating PCD based on CdTe allows to address these problems by intrinsically reducing both the influence of scattering and beam hardening. Based on 2D-radiographic measurements it is shown that by energy thresholding the influence of scattered radiation can be reduced by up to in case of a PCD compared to a conventional energy-integrating detector (EID). To demonstrate the capabilities of a PCD in reducing beam hardening, cupping artefacts are analyzed quantitatively. The PCD results show that the higher the energy threshold is set, the lower the cupping effect emerges. But since numerous beam hardening correction algorithms exist, the results of the PCD are compared to EID results corrected by common techniques. Nevertheless, the highest energy thresholds yield lower cupping artefacts than any of the applied correction algorithms. As an example of a potential industrial CT application, a turbine blade is investigated by CT. The inner structure of the turbine blade allows for comparing the image quality between PCD and EID in terms of absolute contrast, as well as normalized signal-to-noise and contrast-to-noise ratio. Where the absolute contrast can be improved by raising the energy thresholds of the PCD, it is found that due to lower statistics the normalized contrast-to-noise-ratio could not be improved compared to the EID. These results might change to the contrary when discarding pre-filtering of the x-ray spectra and thus allowing more low-energy photons to reach the detectors. Despite still being in the early phase in technological progress, PCDs already allow to improve CT image quality compared to conventional detectors in terms of scatter and beam hardening reduction. KW - X-ray computed tomography KW - Photon counting detector KW - CdTe sensor KW - Non-destructive testing KW - Beam hardening KW - Scattered radiation PY - 2018 UR - http://iopscience.iop.org/article/10.1088/1361-6501/aabef7/meta DO - https://doi.org/10.1088/1361-6501/aabef7 SN - 1361-6501 VL - 29 IS - 7 SP - 075101, 1 EP - 12 PB - IOP Publishing CY - Bristol, UK AN - OPUS4-44959 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Resch-Genger, Ute A1 - Wuerth, Christian A1 - Kraft, Marco A1 - Kaiser, Martin A1 - Radunz, Sebastian A1 - Muhr, V. A1 - Hirsch, Th. A1 - Soukka, T. A1 - Homann, C. A1 - Haase, M. T1 - Luminescence efficiency of upconversion – Quantification of size, particle architecture and dopant concentration effects for different excitation power densities N2 - Lanthanide-based upconversion nanoparticles (UCNPs)like hexagonal beta-NaYF4 UCNPs doped with Yb3+ and Er3+, which efficiently convert 976 nm light to ultraviolet, visible, and near infrared photons, offer new strategies for luminescence-based sensing and imaging. The properties of their upconversion (UC) luminescence (UCL) are, however, strongly influenced by particle size, concentration and spatial arrangement of dopant ions, surface chemistry, microenvironment, and excitation power density (P). We present here comprehensive studies of the influence of UCNP size and particle architecture for Yb3+ and Er3+ co-doped NaYF4 nanoparticles and energy transfer processes in these materials, which underline the importance of quantitative luminescence measurements for mechanistic insights and the determination of application-relevant matrix- and P-dependent optimum dopand concentrations. T2 - 2nd Conference and Spring School CY - Valencia, Spain DA - 04.04.2018 KW - Upconverting nanoparticles KW - Size KW - Energy transfer KW - Fluorescence KW - Absolute fluorescence quantum yield KW - Fluorescence decay kinetics KW - Power density dependence PY - 2018 AN - OPUS4-44960 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Resch-Genger, Ute A1 - Hoffmann, Katrin A1 - Abbandonato, Gerardo T1 - Determination of quantum yields of semiconductor nanocrystals at the single emitter level via fluorescence correlation spectroscopy JF - Nanoscale N2 - Comparing the photoluminescence (PL) properties of ensembles of nanocrystals like semiconductor quantum dots (QDs) with single particle studies is of increasing interest for many applications of These materials as reporters in bioimaging studies performed under very dilute conditions or even at the single particle level. Particularly relevant is here the PL quantum yield (ΦF), which determines the signal size together with the reporter’s molar extinction coefficient and is a direct measure for nanocrystal quality, especially for the inorganic surface passivation shell and its tightness, which can be correlated also with nanocrystal stability and the possible release of heavy metal ions. Exemplarily for red and green emitting CdTe nanocrystals, we present a method for the determination of ΦF of nanoparticle dispersions at ultralow concentration compared to cuvette measurements using fluorescence correlation spectroscopy (FCS), a single molecule method, and compared to molecular dyes with closely matching spectral properties and known ΦF. Our results underline the potential of this approach, provided that material-inherent limitations like ligand- and QD-specific aggregation affecting particle diffusion and QD drawbacks such as their complex and power-dependent blinking behavior are properly considered as shown here. KW - Semiconductor nanocrystal KW - Quantum dot KW - Quantum yield KW - Fluorescence correlation spectroscopy FCS KW - Single molecule PY - 2018 DO - https://doi.org/10.1039/c7nr09332b SN - 2040-3364 SN - 2040-3372 VL - 10 IS - 15 SP - 7147 EP - 7154 PB - Royal Society of Chemistry AN - OPUS4-44894 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Pelkner, Matthias A1 - Stegemann, Robert A1 - Sonntag, Nadja A1 - Pohl, Rainer A1 - Kreutzbruck, Marc T1 - Benefits of GMR sensors for high spatial resolution NDT applications T2 - AIP Conference Proceedings N2 - Magneto resistance sensors like GMR (giant magneto resistance) or TMR (tunnel magneto resistance) are widely used in industrial applications, examples are position measurement and read heads of hard disk drives. However, in case of non-destructive testing (NDT) applications these sensors, although their properties are outstanding like high spatial resolution, high field sensitivity, low cost and low energy consumption, never reached a technical transfer to an application beyond sci-entific scope. This paper deals with benefits of GMR/TMR sensors in terms of high spatial resolution testing for different NDT applica-tions. The first example demonstrates the preeminent advantages of MR-elements compared with conventional coils used in eddy current testing (ET). The probe comprises one-wire excitation with an array of MR elements. This led to a better spatial resolution in terms of neighboring defects. The second section concentrates on MFL-testing (magnetic flux leakage) with active field excitation during and before test-ing. The latter illustrated the capability of highly resolved crack detection of a crossed notch. This example is best suited to show the ability of tiny magnetic field sensors for magnetic material characterization of a sample surface. Another example is based on characterization of samples after tensile test. Here, no external field is applied. The magnetization is only changed due to external load and magnetostriction leading to a field signature which GMR sensors can resolve. This gives access to internal changes of the magnetization state of the sample under test. T2 - QNDE 2017 CY - Provo, Utah, USA DA - 16.07.2017 KW - GMR KW - Non-destructive testing KW - Sensor arrays KW - Spatial resolution PY - 2018 SN - 978-0-7354-1644-4 DO - https://doi.org/10.1063/1.5031535 SN - 0094-243X VL - 1949 SP - UNSP 040001, 1 EP - 10 AN - OPUS4-45050 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Saleh, Maysoon I. A1 - Kembuan, C A1 - Rühle, Bastian A1 - Graf, C A1 - Resch-Genger, Ute T1 - Gold-shell coated NaYF4:Er3+, Yb3+ nanoparticles for the enhancement of fluorescence emission N2 - In the present work, we aim to explore how far the UCNP emission intensity can be enhanced by the aid of plasmonic interactions using a gold shell. The distance between the UCNP core and the gold shell is varied by adding a silica spacer of different thicknesses. The synthetic conditions for obtaining UCNP@SiO2@Au core-shell nanoparticles with precisely tuneable silica shell thicknesses were investigated. A gold shell on the UCNP@SiO2 nanoparticles is expected to give rise to a noticeable enhancement of particle brightness and fluorescence, given that the thicknesses of the silica shell and the gold coating can be controlled and fine-tuned. First single particle studies revealing shortening of the Er3+ lifetimes suggest that plasmonic enhancement occurs. T2 - 2nd Conference and Spring School on Properties, Design and Applications of Upconversion Nanomaterials CY - Valencia, Spain DA - 02.04.2018 KW - Upconversion nanoparticles KW - Silica coating KW - Plasmonic enhancement PY - 2018 AN - OPUS4-44969 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Müller, Anja A1 - Swaraj, S. A1 - Sparnacci, K. A1 - Unger, Wolfgang T1 - Shell thickness determination for PTFE‐PS core‐shell nanoparticles using scanning transmission X‐ray microscopy (STXM) JF - Surface and Interface Analysis N2 - A scanning transmission X‐ray microscopy (STXM)‐based methodology is introduced for determining the dimensions (shell thickness, core and total diameter) of core‐shell nanoparticles, which exhibit a strong X‐ray absorption contrast and a well‐defined interface between core and shell material. A low radiation dosage during data acquisition and, therefore, less X‐ray beam‐induced damage of the sample is achieved by recording STXM images only at 2 predetermined energies of maximum Absorption contrast, instead of recording a stack of images across the whole absorption edge. A model core‐shell nanoparticle, polytetrafluoroethylene (PTFE) cores with polystyrene (PS) shell, is used for demonstration. Near‐edge X‐ray absorption fine structure spectroscopy confirms the significant difference in X‐ray absorption behavior between PTFE and PS. Additionally, because of the insolubility of styrene in PTFE a well‐defined interface between particle core and shell is expected. To validate the STXM results, both the naked PTFE cores as well as the complete core‐shell nanoparticles are examined by scanning electron microscopy (SEM). The introduced STXM‐based methodology yields particle dimensions in agreement with the SEM results and provides additional information such as the position of the particle core, which cannot be extracted from a SEM micrograph. T2 - European conference on applications of surface and interface analysis (ECASIA'17) CY - Montpellier, France DA - 24.09.2017 KW - Core-shell nanoparticles KW - Polymers KW - PS KW - PTFE KW - SEM KW - STXM PY - 2018 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-449700 DO - https://doi.org/10.1002/sia.6464 SN - 1096-9918 SN - 0142-2421 VL - 50 IS - 11 SP - 1077 EP - 1082 PB - John Wiley & Sons CY - Hoboken, New Jersey, USA AN - OPUS4-44970 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Baier, Jennifa A1 - Hidde, Gundula A1 - Sahre, Marion A1 - Weise, Matthias T1 - Particles in PVD-coatings: Imperfection or functional add-on feature? N2 - The application of PVD-coatings ranges from mechanical engineering, i.e. thicker tribological coatings, to precision optics, i.e. thinner optical coatings. For physical vapor deposition (PVD) technologies such as evaporation, sputtering, ion beam assisted/driven deposition, vacuum is a prerequisite for two reasons: at first process-related ones (evaporation source, plasma discharge, and mean free path) and at second coating-related ones (pure, perfect, and dense films). Usually, the goal is a homogenous coating of defined stoichiometry and micro-structure without any imperfection. However, the implementation of micro- or nano-particles may occur accidentally or delibe-rately. Independent of the particle origin, there are two fundamental rules regarding coating functionality: at first, the larger the particle diameter to coating thickness ratio the more affected the functionality of the coating, and at second, the larger the material contrast in terms of the functional feature of interest the more affected the coating performance. Hence, embedded particles have to be avoided for the majority of thin films by all means. The unintended implementation of particles usually results in a malfunction of the coating from the beginning or is at least considered as a weak point of the coating creating a time-dependent defect under service conditions. The intended implementation of particles on surfaces and in coatings may create add-on features, topographic ones and functional ones, however, the facts mentioned hold true. Examples of particle-initiated coating defects are demonstrated in dependence on the origin and the field of application. Strategies for deliberate attachment/embedding of particles on surfaces/in coatings are discussed regarding process compatibility and coating integrity. For industrial applications, both the validation of process compatibility of particle injection and the plasma resistance of particles under vacuum and plasma conditions have to be confirmed. Further points of interest are the homogeneity of particle distribution and the avoidance of particle agglomeration which is still a crucial point for dry dispersed particles. So far, technical applications are limited to PVD hybrid coatings, plasma dispersion coatings are still a challenge except for applications where homogeneity is not required as in case of product authentication. T2 - ICMCTF 2018, International Conference on Metallurgical Coatings and Thin Films CY - San Diego, CA, USA DA - 23.04.2018 KW - PVD-coatings KW - PVD-processes KW - Unintended particle generation KW - Particles as imperfections KW - Deliberate particle implementation KW - Particles as add-on features PY - 2018 AN - OPUS4-44973 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zauer, M. A1 - Prinz, Carsten A1 - Adolphs, J. A1 - Emmerling, Franziska A1 - Wagenführ, A. T1 - Sorption surfaces and energies of untreated and thermally modified wood evaluated by means of excess surface work (ESW) JF - Wood Science and Technology N2 - Water vapor sorption surface areas and sorption energies of untreated and thermally modified Norway spruce [Picea abies (L.) Karst.], sycamore maple (Acer pseudoplatanus L.) and European ash (Fraxinus excelcior L.) were investigated by means of dynamic vapor sorption (DVS) measurements and excess surface work (ESW) evaluation method, respectively. Adsorption and desorption experiments in the hygroscopic range and desorption tests from water saturation were conducted. Thermodynamically, ESW is the sum of the surface free energy and the isothermal isobaric work of sorption. From the amount adsorbed in the first Minimum a specific surface area similar to the BET surface area can be obtained. The results show that untreated spruce has a significantly higher specific water vapor Sorption surface and sorption energy compared to both hardwoods maple and ash. Thermal modification of the woods leads to a significant reduction of water vapor Sorption surface and sorption energy. The determined surface area and energy are higher in desorption direction than in adsorption direction, whereby the highest values in Desorption direction from water saturation, especially for maple and ash, were obtained. The surface areas calculated by means of the ESW method are similar to the surface areas calculated by means of the BET method, particularly in adsorption direction. KW - Excess surface work KW - Dynamic vapor sorption KW - Wood KW - BET PY - 2018 DO - https://doi.org/10.1007/s00226-018-1021-2 SN - 1432-5225 SN - 0043-7719 VL - 52 IS - 4 SP - 957 EP - 969 PB - Springer CY - Berlin Heidelberg AN - OPUS4-44975 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Beck, Uwe A1 - Fischer, Daniel A1 - Hertwig, Andreas A1 - Mitzkus, Anja A1 - Sahre, Mario A1 - Weise, Matthias A1 - Köppe, Enrico A1 - Bartholmai, Matthias A1 - Basedau, Frank A1 - Hofmann, Detlef A1 - Schukar, Vivien A1 - Kormunda2, M. T1 - Multi-functional coatings for optical sensor applications: Surface plasmon resonance & magneto-optical coupling N2 - Multi-functional coatings are a key requirement for surface engineering. General demands are adhesion and long-term stability under service conditions. The modification of surfaces by means of PVD-, ECD- or hybrid processes allows an add-on functionalization of surfaces by a huge diversity of materials with both lateral and vertical micro-/nano-designs. This fact is a prerequisite for micro- and sensor-systems in lab-on-chip and sensor-on-chip technology. Two layer-based sensor principles are presented, i.e. surface plasmon resonance enhanced spectroscopic ellipsometry (SPREE) for detection of hazardous gases and magneto-optical sensors on smart-coated fiber Bragg gratings (FBG) for structural health monitoring (SHM). The interdependence of substrate features, coating properties, and layer design is discussed firstly for gas sensitivity and selectivity of SPREE-sensors and secondly for sensitivity and selectivity of magneto-strictive coatings to mechanical strain or external magnetic fields resulting in an optical displacement of the Bragg wavelength of FBG-sensors. Moreover, generic features such long-term stability, crucial process-related fabrication conditions, and effects of operational and environmental parameters are discussed with respect to the sensor performance. It has been shown that appropriate layer design and adapted selection of layer materials (SnOx/Au, Fe/Ni:SnOx/Au; Ni/NiFe-Cu-Cr) result in improved sensor parameters and may enable new sensor applications. T2 - SVC TechCon 2018 CY - Orlando, FL, USA DA - 05.05.2018 KW - Multi-functional coatings for sensors KW - Surface plasmon resonance enhanced ellipsometry (SPREE) KW - Gas monitoring KW - Magneto-optical coupling (MOC) KW - Structural health monitoring (SHM) PY - 2018 AN - OPUS4-44976 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Westwood, S. A1 - Josephs, R. A1 - Choteau, T. A1 - Daireaux, A. A1 - Stoppacher, N. A1 - Wielgosz, R. A1 - Davies, S. A1 - do Rego, E. A1 - Wollinger, W. A1 - Garrido, B. A1 - Fernandes, J. A1 - Lima, J. A1 - Oliveira, R. A1 - de Sena, R. A1 - Windust, A. A1 - Huang, T. A1 - Dai, X. A1 - Quan, C. A1 - He, H. A1 - Zhang, W. A1 - Wei, C. A1 - Li, N. A1 - Gao, D. A1 - Liu, Z. A1 - Lo, M. A1 - Wong, W. A1 - Pfeifer, Dietmar A1 - Koch, Matthias A1 - Dorgerloh, Ute A1 - Rothe, Robert A1 - Philipp, Rosemarie A1 - Hanari, N. A1 - Rezali, M. A1 - Arzate, C. A1 - Berenice, M. A1 - Caballero, V. A1 - Osuna, M. A1 - Krylov, A. A1 - Kharitonov, S. A1 - Lopushanskaya, E. A1 - Liu, Q. A1 - Lin, T. A1 - Fernandes-Whaley, M. A1 - Quinn, L. A1 - Nhlapo, N. A1 - Prevoo-Franzsen, D. A1 - Archer, M. A1 - Kim, B. A1 - Baek, S. A1 - Lee, S. A1 - Lee, J. A1 - Marbumrung, S. A1 - Kankaew, P. A1 - Chaorenpornpukdee, K. A1 - Chaipet, T. A1 - Shearman, K. A1 - Gören, A. A1 - Gündüz, S. A1 - Yilmaz, H. A1 - Un, I. A1 - Bilsel, G. A1 - Clarkson, C. A1 - Bedner, M. A1 - Camara, J. A1 - Lang, B. A1 - Lippa, K. A1 - Nelson, M. A1 - Toman, B. A1 - Yu, L. T1 - Mass fraction assignment of folic acid in a high purity material - CCQM-K55.d (Folic acid) Final Report JF - Metrologia N2 - The comparison required the assignment of the mass fraction of folic acid present as the main component in the comparison sample. Performance in the comparison is representative of a laboratory's measurement capability for the purity assignment of organic compounds of medium structural complexity [molecular weight range 300–500] and high polarity (pKOW < −2). Methods used by the eighteen participating NMIs or DIs were based on a mass balance (summation of impurities) or qNMR approach, or the combination of data obtained using both methods. The qNMR results tended to give slightly lower values for the content of folic acid, albeit with larger associated uncertainties, compared with the results obtained by mass balance procedures. Possible reasons for this divergence are discussed in the report, without reaching a definitive conclusion as to their origin. The comparison demonstrates that for a structurally complex polar organic compound containing a high water content and presenting a number of additional analytical challenges, the assignment of the mass fraction content property value of the main component can reasonably be achieved with an associated relative standard uncertainty in the assigned value of 0.5% KW - CCQM key comparison KW - Purity assessment KW - Folic acid PY - 2018 UR - https://www.bipm.org/utils/common/pdf/final_reports/QM/K55/CCQM-K55.d.pdf DO - https://doi.org/10.1088/0026-1394/55/1A/08013 VL - 55 IS - Technical Supplement, 2018 SP - 08013, 1 EP - 38 PB - Institute of Physics Publishing (IOP) ; Bureau International des Poids et Mesures AN - OPUS4-44999 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Büchele, Dominique A1 - Rühlmann, Madlen A1 - Schmid, Thomas A1 - Ostermann, Markus T1 - Comparison between uni- and multivariate data analysis for the determination of nutrients in soils using XRF N2 - Aim of the Federal Institute for Materials Research and Testing (BAM) in the frame of I4S - “Intelligence for Soil” is the characterization of an X-ray fluorescence (XRF) based sensor for robust online-application of arable land.Fast soil mapping for agricultural purpose allows the site-specific optimized introduction of plant essential nutrients like S, K, Ca, and Fe. This is important given that the distribution of minor and trace elements varies widely. The non-destructive and contactless XRF is suitable for rapid in-situ analysis on the field due to minimal sample preparation and simultaneous multi-element analysis. Soils are already considered as a complex matrix due to their wide range of elements in different contents, especially light elements with low atomic numbers (Z<19). Problems by measuring soil samples also arise from heterogeneity of the sample and matrix effects. Large grain size distribution causes strong inhomogeneity and matrix effects occur through physical properties related to high concentration of main components. Matrix-specific calibration strategies for determination of total major and minor plant essential nutrients are particularly important regarding these difficulties. For accurate calibration, data treatment and evaluation must also be considered. Empirical univariate and multivariate data analysis were compared regarding their analytical figures of merit. Using principal component analysis (PCA) it was possible to classify German soils in different groups as sand, clay and silt. A calibration curve was obtained by partial least squares regression (PLSR) and the elemental content of German soils was predicted. Elemental distribution maps for different German arable lands were created and the results compared to reference measurements. The correlation between predicted values and reference values were in good agreement for most major and minor nutrients. T2 - BonaRes Conference CY - Berlin, Germany DA - 26.02.2018 KW - PLSR KW - XRF KW - Soil KW - PCA PY - 2018 AN - OPUS4-45007 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -