TY - JOUR A1 - Agirrezabal-Telleria, Iker A1 - Guo, Y. A1 - Hemmann, Felix A1 - Arias, P. L. A1 - Kemnitz, E. T1 - Dehydration of xylose and glucose to furan derivatives using bifunctional partially hydroxylated MgF2 catalysts and N2-stripping N2 - The current furfural production yield is low due to the use of non-selective homogeneous catalysts and expensive separation. In this work, partially hydroxylated MgF2 catalysts, synthesized using different water contents, were screened during xylose dehydration in water–toluene at 160 °C. The different Lewis/Brønsted ratios on the MgF2 catalysts showed that under-coordinated Mg can isomerize xylose to xylulose, whilst the surface OH-groups were responsible for the dehydration reactions. The presence of glucose as a co-carbohydrate reduced the furfural selectivity from 86 to 81%, whilst it also led to high 5-hydroxymethylfurfural selectivity. The tests catalyzed by MgF2 in combination with simultaneous N2-stripping showed that a furfural selectivity of 87% could be achieved using low xylose loadings. Moreover, the catalysts regenerated by H2O2 showed high activity during the dehydration tests in water–toluene at 160 °C. KW - Bifunctional MgF2 KW - Lewis/Bronsted KW - Carbohydrates KW - Furan derivatives KW - N2-stripping PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-305441 DO - https://doi.org/10.1039/c4cy00129j SN - 2044-4753 SN - 2044-4761 VL - 4 IS - 5 SP - 1357 EP - 1368 PB - RSC Publ. CY - Cambridge AN - OPUS4-30544 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stoch, P. A1 - Szczerba, Wojciech A1 - Bodnar, W. A1 - Ciecinska, M. A1 - Stoch, A. A1 - Burkel, E. T1 - Structural properties of iron-phosphate glasses: spectroscopic studies and ab initio simulations N2 - Vitrification is the most effective method for the immobilization of hazardous waste by incorporating toxic elements into a glass structure. Iron phosphate glasses are presently being considered as matrices for the storage of radioactive waste, even of those which cannot be vitrified using conventional borosilicate waste glass. In this study, a structural model of 60P2O5–40Fe2O3 glass is proposed. The model is based on the crystal structure of FePO4 which is composed of [FeO4][PO4] tetrahedral rings. The rings are optimized using the DFT method and the obtained theoretical FTIR and Raman spectra are being compared with their experimental counterparts. Moreover, the proposed model is in very good agreement with X-ray absorption fine structure spectroscopy (XANES/EXAFS) and Mössbauer spectroscopy measurements. According to the calculations the Fe3+ is in tetrahedral and five-fold coordination. The maximal predicted load of waste constituents into the glass without rebuilding of the structure is 30 mol%. Below this content, waste constituents balance the charge of [FeO4]- tetrahedra which leads to their strong bonding to the glass resulting in an increase of the chemical durability, transformation and melting temperatures and density. KW - Glass KW - Iron KW - DFT simulations KW - Mössbauer spectroscopy KW - XANES/EXAFS KW - FTIR spectroscopy KW - Raman spectroscopy KW - Coordination PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-317351 DO - https://doi.org/10.1039/c4cp03113j SN - 1463-9076 SN - 1463-9084 VL - 16 IS - 37 SP - 19917 EP - 19927 PB - The Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-31735 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krause, Christina A1 - Zorn, R. A1 - Emmerling, Franziska A1 - Falkenhagen, Jana A1 - Frick, B. A1 - Huber, P. A1 - Schönhals, Andreas T1 - Vibrational density of states of triphenylene based discotic liquid crystals: dependence on the length of the alkyl chain N2 - The vibrational density of states of a series of homologous triphenylene-based discotic liquid crystals HATn (n = 5, 6, 8, 10, 12) depending on the length of the aliphatic side chain is investigated by means of inelastic neutron scattering. All studied materials have a plastic crystalline phase at low temperatures, followed by a hexagonally ordered liquid crystalline phase at higher temperatures and a quasi isotropic phase at the highest temperatures. The X-ray scattering pattern for the plastic crystalline phase of all materials shows a sharp Bragg reflection corresponding to the intercolumnar distance in the lower q-range and a peak at circa 17 nm-1 related to intracolumnar distances between the cores perpendicular to the columns as well as a broad amorphous halo related to the disordered structure of the methylene groups in the side chains in the higher q-range. The intercolumnar distance increases linearly with increasing chain length for the hexagonal columnar ordered liquid crystalline phase. A similar behaviour is assumed for the plastic crystalline phase. Besides n = 8 all materials under study exhibit a Boson peak. With increasing chain length, the frequency of the Boson peak decreases and its intensity increases. This can be explained by a self-organized confinement model. The peaks for n = 10, 12 are much narrower than for n = 5, 6 which might imply the transformation from a rigid system to a softer one with increasing chain length. Moreover the results can also be discussed in the framework of a transition from an uncorrelated to a correlated disorder with increasing n where n = 8 might be speculatively considered as a transitional state. KW - X-ray scattering KW - Neutron scattering KW - Differential scanning calorimetry PY - 2014 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-304789 DO - https://doi.org/10.1039/c3cp55303e SN - 1463-9076 SN - 1463-9084 VL - 16 IS - 16 SP - 7324 EP - 7333 PB - The Royal Soc. of Chemistry CY - Cambridge AN - OPUS4-30478 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wollschläger, Nicole A1 - Tasdemir, Z. A1 - Häusler, Ines A1 - Leblebici, Y. A1 - Österle, Werner A1 - Alaca, B. E. T1 - Determination of the elastic behavior of silicon nanowires within a scanning electron microscope N2 - Three-point bending tests were performed on double-anchored, <110> silicon nanowire samples inside a scanning electron microscope (SEM) via a micromanipulator equipped with a piezo-resistive force sensor. Representing the upper and lower boundaries achievable in a consistent manner, silicon nanowires with widths of 35 nm and 74 nm and a height of 168 nm were fabricated. The nanowires were obtained monolithically along with their 10-m-tall supports through a top-down fabrication approach involving a series of etching processes. Hence, no interface compliance was introduced between supports and nanowires. Exact nanowire dimensions and cross-sectional features were determined by transmission electron microscopy (TEM) following sample preparation through focused ion beam (FIB) machining. Conducting the experiments inside an SEM chamber further raised the opportunity of the direct observation of any deviation from ideal loading conditions such as twisting, which was taken into consideration in simulations. Measured force-displacement behavior was observed to exhibit close resemblance to simulation results obtained by finite element modeling, when the bulk value of 169 GPa was taken as the modulus of elasticity for <110> silicon. Hence, test results show neither any size effect nor evidence of residual stresses for the considered nanoscale objects. The increased effect of the native oxide with reduced nanowire dimensions was captured as well. Thus this very simple in-situ testing method was found to be an alternative to elaborate AFM measurements on geometrically formidable nanostructures. The results demonstrate the applicability of the developed fabrication approach to the incorporation of silicon nanowires in functional micromechanical devices. KW - Silicon nanowire KW - Elastic behavior KW - Scanning electron microscope KW - Mechanical properties PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-370383 DO - https://doi.org/10.1155/2016/4905838 VL - 2016 SP - Article 4905838, 1 EP - 6 PB - Hindawi Publishing Corporation AN - OPUS4-37038 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Olejko, Lydia A1 - Bald, Ilko T1 - FRET efficiency and antenna effect in multi-color DNA origami-based light harvesting systems N2 - Artificial light harvesting complexes find applications in artificial photosynthesis, photovoltaics and light harvesting chemical sensors. They are used to enhance the absorption of light of a reaction center which is often represented by a single acceptor. Here, we present different light harvesting systems on DNA origami structures and analyze systematically the light harvesting efficiency. By changing the number and arrangement of different fluorophores (FAM as donor, Cy3 as transmitter and Cy5 as acceptor molecules) the light harvesting efficiency is optimized to create a broadband absorption and to improve the antenna effect 1 (including two energy transfer steps) from 0.02 to 1.58, and the antenna effect 2 (including a single energy transfer step) from 0.04 to 8.7, i.e. the fluorescence emission of the acceptor is significantly higher when the light-harvesting antenna is excited at lower wavelength compared to direct excitation of the acceptor. The channeling of photo energy to the acceptor proceeds by Förster Resonance Energy Transfer (FRET) and we carefully analyze also the FRET efficiency of the different light harvesting systems. Accordingly, the antenna effect can be tuned by modifying the stoichiometry of donor, transmitter and acceptor dyes, whereas the FRET efficiency is mainly governed by the spectroscopic properties of dyes and their distances. KW - DNA origami KW - Light-harvesting KW - FRET KW - Antenna effect PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-405867 UR - http://pubs.rsc.org/en/content/articlelanding/2017/ra/c7ra02114c#!divAbstract DO - https://doi.org/10.1039/C7RA02114C VL - 7 IS - 39 SP - 23924 EP - 23934 PB - The Royal Soc. of Chemistry AN - OPUS4-40586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Österle, Werner A1 - Nikonov, A. Y. A1 - Dmitriev, A. I. ED - Krzanowski, J. T1 - MD sliding simulations of amorphous tribofilms consisting of either SiO2 or carbon N2 - The sliding behaviors of two simplified tribofilms with amorphous structure consisting either of SiO₂ molecules or C atoms were simulated by molecular dynamics modeling. The objective was to identify mechanisms explaining the experimentally observed lubricating properties of the two amorphous films. The impacts of layer thickness, normal pressure, temperature and different substrate materials were studied systematically, while the sliding velocity was kept constant at 30 m/s. While the layer thickness was not critical, all the other parameters showed special effects under certain conditions. Normal pressure impeded void formation and could even eliminate voids if applied at high temperature. Stick-slip sliding was changed to smooth sliding at high temperature due to void healing. Considering the carbon film, high friction forces and shearing of the entire film was observed with diamond substrates, whereas interface sliding at low friction forces and an amorphous layer of iron mixed with carbon was observed if the supporting substrates consisted of α-Fe. Both films show a decrease of friction forces and smooth sliding behavior at elevated temperature, corresponding well to the tribological behavior of and advanced nanocomposite sliding against a steel disc under severe stressing conditions when high flash temperatures can be expected. KW - dry friction KW - amorphous silica film KW - amorphous carbon film KW - sliding simulation KW - molecular dynamics PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-379367 DO - https://doi.org/10.3390/lubricants4030024 VL - 4 IS - 24 PB - MDPI CY - Basel, Switzerland AN - OPUS4-37936 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klykov, Oleg A1 - Weller, Michael G. T1 - Quantification of N-hydroxysuccinimide and N-hydroxysulfosuccinimide by hydrophilic interaction chromatography (HILIC) N2 - N-Hydroxysuccinimide (NHS) esters are the most important activated esters used in many different bioconjugation techniques, such as protein labelling by fluorescent dyes and enzymes, surface activation of chromatographic supports, microbeads, nanoparticles, and microarray slides, and also in the chemical synthesis of peptides. Usually, reactions with NHS esters are very reliable and of high yield, however, the compounds are sensitive to air moisture and water traces in solvents. Therefore, the quantification of NHS would be a very helpful approach to identify reagent impurities or degradation of stored NHS esters. No robust and sensitive method for the detection of NHS (or the more hydrophilic sulfo-NHS) has been reported yet. Here, a chromatographic method based on HILIC conditions and UV detection is presented, reaching a detection limit of about 1 mg L-1, which should be sensitive enough for most of the applications mentioned above. Exemplarily, the hydrolytic degradation of a biotin-NHS ester and a purity check of a fluorescent dye NHS ester are shown. An important advantage of this approach is its universality, since not the structurally variable ester compound is monitored, but the constant degradation product NHS or sulfo-NHS, which avoids the necessity to optimize the separation conditions and facilitates calibration considerably. KW - NHS KW - Sulfo-NHS KW - NHS-Ester KW - Qualitätskontrolle KW - Reinheitsbestimmung KW - HPLC PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-337833 DO - https://doi.org/10.1039/c5ay00042d SN - 1759-9660 SN - 1759-9679 VL - 7 IS - 15 SP - 6443 EP - 6448 PB - RSC Publ. CY - Cambridge AN - OPUS4-33783 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Carl, Peter A1 - Schneider, Rudolf T1 - Optimization and evaluation of a hapten microarray using chemometric methods N2 - The demands for the assessment of water quality are increasing steadily, making it necessary to routinely monitor multiple contaminants in water samples. For this application a hapten microarray was developed. In order to reach the required low detection limits a design of experiments (DoE) approach was used to optimize the assay performance. Here we show that a Box-Behnken design plan is an adequate choice for the straightforward exploration of hapten microarray assay parameters. For both read-out systems studied (fluorophore-labelled detection antibodies or enzymatic signal development followed by reflectometric scan, respectively), it was possible to significantly extend the measurement ranges. Furthermore, it could be shown that multivariate data analysis, here partial least squares regression (PLS), can improve the prediction accuracy of 'unknown' samples when used as calibration model, compared to classical, univariate data evaluation methods. KW - Koffein KW - Caffeine KW - Proteine microarray KW - Design of experiments KW - Multivariate data analysis KW - Partial least squares regression KW - Small molecule detection KW - Microarray KW - Immunoarray KW - Immunoassay KW - ELISA KW - Chemometrie KW - Chemometrics PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-344672 DO - https://doi.org/10.1016/j.proeng.2015.08.684 SN - 1877-7058 VL - 120 SP - 501 EP - 506 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-34467 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Siebler, Daniel A1 - Rohwetter, Philipp A1 - Brusenbach, R. A1 - Plath, R. T1 - Optical-only detection of partial discharge with fluorescent polymer optical fiber sensors N2 - This paper reflects recent progress in the field of fluorescent polymer optical fiber sensors (F-POF) for partial discharge (PD) detection in high voltage (HV) cable accessories using optical-only PD detection by coincidence single photon counting. In experiments with artificial PD sources these sensors show the ability to detect optical emissions from picocoulomb-level PDs in a real-scale model of a translucent high voltage cable accessory. False positives (caused by detector noise) are efficiently suppressedwhile maintaining sufficient sensitivity,even when the sensor is located in an unfavorable position. T2 - EUROSENSORS 2015 CY - Freiburg, Germany DA - 06.09.2015 KW - Partial discharge KW - Silicone rubber KW - High voltage cable accessories KW - Polymer optical fiber POF KW - Fluorescence KW - Coincidence PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-337881 DO - https://doi.org/10.1016/j.proeng.2015.08.711 SN - 1877-7058 VL - 120 SP - 845 EP - 848 PB - Elsevier Ltd. CY - Amsterdam AN - OPUS4-33788 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Mähner, D. A1 - Sodeikat, Ch. A1 - Maack, Stefan T1 - ZfPBau-Verfahren an Elementwänden – Fallbeispiele und vergleichende Untersuchungen N2 - Die zerstörungsfreien Prüfverfahren konnten ihre Fähigkeit bei der Untersuchung von Elementwänden in einzelnen Fallstudien erbringen. Aufbauend auf den Kenntnissen aus der Praxis und auf Testreihen im Rahmen von Laboruntersuchungen wurde ein erster Ringversuch geplant und durchgeführt. Im Rahmen dieses Ringversuchs wurden verschiedene Strukturdefekte und Einbauteile in Elementwände eingebaut. Die Messung der Wände erfolgte anschließend durch mehrere Messteams mit unterschiedlichen zerstörungsfreien Prüfverfahren. Zum Einsatz kamen hierbei das Ultraschall-Echo- und das Impact-Echo-Verfahren sowie das Impuls-Radar-Verfahren. Zur Verbesserung der Vergleichbarkeit zwischen den unterschiedlichen Prüfverfahren wurde auf die Elementwände ein einheitliches Messraster aufgebracht. Für eine möglichst objektive Messung der Wände erhielten die Messteams vor den Messungen keine Details zu den Strukturdefekten oder Einbauteilen. Die Prüfaufgabe bestand darin, die Wände mit dem jeweiligen Prüfverfahren zu untersuchen. Anschließend wurden die Ergebnisse der Messteams zentral gesammelt und ausgewertet. Anhand der zentralen Auswertung sollten Aussagen zu den eingebauten Inhomogenitäten ableitet werden. Hierdurch kann zum einen die Leistungsfähigkeit der Prüfverfahren an unterschiedlichsten Inhomogenitäten getestet werden, zum anderen können die Ergebnisse und somit die Prüfverfahren untereinander verglichen werden. Zu diesen in der Praxis immer häufiger vorkommenden Fragestellungen können grundsätzliche Aussagen zum Einsatz von zerstörungsfreien Prüfungen bei Elementwänden gewonnen werden. Über die Ergebnisse dieses Ringversuches wird nachfolgend berichtet. T2 - Fachtagung Bauwerksdiagnose - Praktische Anwendungen Zerstörungsfreier Prüfungen und Zukunftsaufgaben CY - Berlin, Germany DA - 25.02.2016 KW - Beton KW - Zerstörungsfreie Prüfung im Bauwesen KW - Elementwände KW - WU-Bauwerke PY - 2016 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-388331 UR - http://www.bauwerksdiagnose2016.de/Portals/bwd2016/BB/vortrag%2010.pdf SP - 1 EP - 22 PB - Deutsche Gesellschaft für zerstörungsfreie Prüfung e.V. CY - Berlin AN - OPUS4-38833 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -