TY - GEN A1 - Bienwald, Frank T1 - Optimierung der Aminosäureanalytik aromatischer Aminosäuren mittels HPLC N2 - Ausgehend von dem in der Literatur beschriebenen Verfahren zur Bestimmung aromatischer Aminosäuren konnte eine Analysemethode zur Proteinbestimmung über die optische Detektion von Tyrosin und Phenylalanin nach chromatographischer Trennung der Protein-Hydrolysate entwickelt werden, die gegenüber dem Verfahren aus der Literatur erhebliche Vorteile besitzt. Der Einsatz von Rundbodenvials stellt eine Neuerung und kostengünstige Alternative zu der konventionellen Hydrolyse in Vakuumhydrolyseröhrchen wie auch zu den Mikrowellenvials der Mikrowellenhydrolyse dar, die das Potential für Miniaturisierungen der Proben hat und sich zudem für große Probendurchsätze eignet. Anstelle der Mikrowellenheizungen wurde ein konventionelles Ölbad als Heizquelle verwendet. Somit ergibt sich eine Verbesserung auch darin, dass diese Methode geringere Geräteinvestitionen erfordert. Wie die Ergebnisse nahelegen, sind sowohl Salzsäure als auch Bromwasserstoffsäure geeignete Reagenzien, die bei der sauren Hydrolyse von Proteinen verwendet werden können. Mit Hilfe antioxidativer Zusätze können Nebenreaktionen erfolgreich vermieden werden. Hier haben sich L-Cystein und Oxalsäure als wirkungsvolle Additive herausgestellt. Wichtige Verbesserungen betreffen vor allem die Zeitersparnis bei der Hydrolyse, die Aufarbeitung der Hydrolysate und die chromatographischen Separationen. Erstere konnte gegenüber der konventionellen Methode von 22 Stunden auf 45 Minuten reduziert werden. Die chromatographische Trennung wurde so weit optimiert, dass die Laufzeit von 64 auf 35 Minuten verkürzt werden konnte. Zudem konnte auf das zeitraubende und kontaminationsanfällige Eindampfen der Hydrolysate verzichtet werden. Während der Aufarbeitung der Hydrolysate konnten die Menge eingesetzter Chemikalien reduziert und damit mögliche Störungen während der optischen Detektion verringert werden. Letztere wurde zum einen durch das Einbeziehen der UV-Absorption bei 260 nm erweitert, sodass eine Alternative zur Absorption bei 215 nm vorliegt, die ebenere Basislinien im Chromatogramm ermöglicht. Zum anderen wurde gezeigt, dass mit Hilfe der Fluoreszenz die Empfindlichkeit der Methode gegenüber der UV-Absorption erheblich verbessert werden kann. Anhand der Probe eines Birkenpollenextraktes ließ sich die Anwendbarkeit der optimierten Methode auf Realproben demonstrieren. KW - Aromatische Aminosäuren KW - Aromatic amino acid analysis KW - AAAA KW - Phenylalanine KW - Tyrosine KW - Hydrochloric acid KW - Hydrobromic acid KW - HCl KW - HBr KW - Chromatographie KW - Reversed-phase KW - Hydrolysis KW - AdvanceBio Peptide Map KW - PRP-C18 PY - 2017 SP - 1 EP - 71 PB - Humboldt-Universität zu Berlin CY - Berlin AN - OPUS4-54650 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nolze, Gert A1 - Hielscher, R. A1 - Winkelmann, Aimo T1 - Electron backscatter diffraction beyond the mainstream N2 - We present special applications of electron backscatter diffraction (EBSD) which aim to overcome some of the limitations of this technique as it is currently applied in the scanning electron microscope. We stress that the raw EBSD signal carries additional information which is useful beyond the conventional orientation determination. The background signal underlying the backscattered Kikuchi diffraction (BKD) patterns reflects the chemical composition and surface topography but also contains channeling-in information which is used for qualitative real-time orientation imaging using various backscattered electron signals. A significantly improved orientation precision can be achieved when dynamically simulated pattern are matched to the experimental BKD patterns. The breaking of Friedel’s rule makes it possible to obtain orientation mappings with respect to the point-group symmetries. Finally, we discuss the determination of lattice parameters from individual BKD patterns. Subgrain structure in a single quartz grain. The increased noise level in the left map reflects the lower precision of a standard orientation determination using band detection by the Hough transform. The right map results from the same experimental raw data after orientation refinement using a pattern matching approach. The colors correspond an adapted inverse pole figure color key with a maximum angular deviation of about 2° from the mean orientation. KW - Electron backscatter diffraction PY - 2017 U6 - https://doi.org/10.1002/crat.201600252 SN - Online 1521-4079 VL - 52 IS - 1 SP - Special Issue - Article Number: UNSP 1600252, 1 EP - 24 PB - WILEY-VCH AN - OPUS4-37935 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mady, A. H. A1 - Baynosa, M. L. A1 - Tuma, Dirk A1 - Shim, J.-J. T1 - Facile microwave-assisted green synthesis of Ag-ZnFe2O4@rGO nanocomposites for efficient removal of organic dyes under UV- and visible-light irradiation N2 - Nanocomposites of Ag-ZnFe2O4@reduced graphene oxide (rGO) were synthesized using a one-pot microwave-assisted self-assembly method. The morphology and structure of the Ag-ZnFe2O4@rGO nanocomposites were characterized. The nanocomposites formed with 15.2 wt% rGO showed excellent adsorption properties and high photocatalytic activity for the degradation of methylene blue (MB), rhodamine B (RhB), and methyl orange (MO). The synergistic interactions between Ag, ZnFe2O4, and rGO decreased the aggregation of the nanoparticles (NPs) and increased the surface area, resulting in better absorption in both UV and visible light. Such a structure was helpful for separating the photoexcited electron-hole pairs and accelerating electron transfer. Electrochemical impedance spectroscopy (EIS) revealed a smaller resistance in the solid-state interface layer and charge transfer on the composite surface than that of the bare ZnFe2O4 NPs and ZnFe2O4@rGO nanocomposite. The Ag-ZnFe2O4@rGO nanocomposite could be recovered easily by a magnet and reused five times with no significant decrease in photocatalytic activity. The as-prepared Ag-ZnFe2O4@rGO nanocomposite catalyst could be applied to the removal of hard-to-degrade waste materials owing to its high efficiency in both UV and visible light and its excellent reusability. KW - nanoparticles KW - microwave synthesis KW - photocatalysis PY - 2017 U6 - https://doi.org/10.1016/j.apcatb.2016.10.033 SN - 0926-3373 SN - 1873-3883 VL - 203 SP - 416 EP - 427 PB - Elsevier B. V. CY - Amsterdam AN - OPUS4-37962 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Cappella, Brunero T1 - Force-distance curves on lubricant films: An approach to the characterization of the shape of the AFM tip N2 - Force-distance curves have been acquired with an atomic force microscope on perfluorpolyether films. It is shown that curves acquired on films of different thickness, at different rates and with different dwell times can be overlapped by rescaling the time or distance axis.When the time or distance axis is rescaled,the force depends only on the surface tension of perfluorpolyether and on geometrical properties of thetip (aperture and perimeter of the tip at a given distance from the apex). Hence, curves acquired with thesame tip overlap. By comparing curves acquired at different rates the dynamics of tip-wetting can be investigated. Fur-thermore, rescaled force-distance curves have been matched with the perimeter of cross sections ofthe tip, i.e. with the perimeter of the three-phase contact line. Such measurements pave the way for anon-destructive investigation of the tip shape. KW - Lubricant films KW - Surface tension KW - Atomic force microscopy KW - Force-distance curves KW - AFM tip shape PY - 2017 U6 - https://doi.org/10.1016/j.micron.2016.11.006 SN - 0968-4328 VL - 93 SP - 20 EP - 28 AN - OPUS4-38391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bonse, Jörn A1 - Höhm, S. A1 - Kirner, Sabrina V. A1 - Rosenfeld, A. A1 - Krüger, Jörg T1 - Laser-induced periodic surface structures — a scientific evergreen N2 - Laser-induced periodic surface structures (LIPSS, ripples) are a universal phenomenon and can be generated on almost any material upon irradiation with linearly polarized radiation. With the availability of ultrashort laser pulses, LIPSS have gained an increasing attraction during the past decade, since these structures can be generated in a simple single-step process, which allows a surface nanostructuring for tailoring optical, mechanical, and chemical surface properties. In this study, the current state in the field of LIPSS is reviewed. Their formation mechanisms are analyzed in ultrafast time-resolved scattering, diffraction, and polarization constrained double-pulse experiments. These experiments allow us to address the question whether the LIPSS are seeded via ultrafast energy deposition mechanisms acting during the absorption of optical radiation or via self-organization after the irradiation process. Relevant control parameters of LIPSS are identified, and technological applications featuring surface functionalization in the fields of optics, fluidics, medicine, and tribology are discussed. KW - Laser ablation KW - Nanostructures KW - Surface functionalization KW - Surface texture KW - Laser-induced periodic surface structures (LIPSS) PY - 2017 U6 - https://doi.org/10.1109/JSTQE.2016.2614183 SN - 1077-260X SN - 1558-4542 VL - 23 IS - 3 SP - 9000615 PB - IEEE AN - OPUS4-38633 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rabe, Sebastian A1 - Schartel, Bernhard T1 - The rapid mass calorimeter: Understanding reduced-scale fire test results N2 - The effects of reducing specimen size on the fire behavior of polymeric materials were investigated by means of the rapid mass calorimeter, a high-throughput Screening instrument. Results from the rapid mass calorimeter were compared with those from the cone calorimeter. Correlation coefficients between the different measures of each method and between the two methods are discussed to elucidate the differences and similarities in the two methods. Materials with characteristic heat release rate (HRR) curves in the cone calorimeter were evaluated in detail. The rapid mass calorimeter produces valuable and interpretable results with HRR curve characteristics similar to cone calorimeter results. Compared to cone calorimeter measurements, material savings of 96% are achieved, while maintaining the Advantages of a macroscopic fire test. KW - Rapid mass calorimeter KW - High throughput KW - Cone calorimeter KW - Flame retardancy PY - 2017 U6 - https://doi.org/10.1016/j.polymertesting.2016.11.027 SN - 0142-9418 VL - 57 SP - 165 EP - 174 PB - Elsevier AN - OPUS4-38739 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Gawlitza, Kornelia A1 - Wan, Wei A1 - Wagner, Sabine A1 - Rurack, Knut ED - Tiwari, Ashutosh ED - Uzun, Lokman T1 - Fluorescent Molecularly Imprinted Polymers N2 - An ideal sensor system is a combination of a selective receptor, an effective transducer, and a sensitive detector. To utilize molecularly imprinted polymers (MIPs) as responsive recognition phases in sensors, the employment of fluorescent molecules or nanoparticles (NPs) that show prominent changes in their spectroscopic properties after binding of the target molecule in the MIP’s cavity is particularly attractive. Such fluorescent MIPs (fMIPs) act through target-induced quenching, enhancement, or spectral shifts of the fluorescence. This contribution introduces different strategies of incorporation of fluorescent dyes, probes, and NPs into fMIPs. In addition, various sensing mechanisms are reviewed, and depending on the application of the sensor, the different deployable formats, their advantages, drawbacks, and impact will be presented and discussed. KW - Dyes KW - Fluorescence KW - Molecular imprinted polymers KW - Quantum dots KW - Sensors PY - 2017 SN - 978-1-119-33629-7 SP - 89 EP - 128 PB - Scrivener Publishing, WILEY CY - Beverly, MA ET - 1 AN - OPUS4-38798 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Hahn, Oliver ED - Gonella, Julia ED - Weis, Friederike ED - Rauch, Christoph T1 - Scientific investigation of carbon inks – an analytical challenge N2 - The investigation of physical properties and chemical composition generates data important for answering art-historical questions. Due to technological developments, technical diagnostics in art and culture are in ever-greater demand in such fields of transdisciplinary research. Based on one example, a collar drawing from the Berlin Diez albums, the present paper aims to give some insights into the multi-instrumental approach in the material analysis of cultural artefacts. The same methods were also applied to other drawings from the Diez Albums. KW - Archaeometry KW - X-ray fluorescence KW - Visible spectrophotometry KW - Non-destructive analysis PY - 2017 SN - 9789004323483 U6 - https://doi.org/10.1163/9789004323483_016 VL - 11 SP - 427 EP - 438 PB - Brill CY - Leiden AN - OPUS4-38818 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leng, Jing A1 - Kang, N. A1 - Wang, D.-Y. A1 - Wurm, Andreas A1 - Schick, C. A1 - Schönhals, Andreas T1 - Crystallization behavior of nanocomposites based on poly(L-lactide) and MgAl layered double hydroxides - Unbiased determination of the rigid amorphous phases due to the crystals and the nanofiller N2 - Semicrystalline polymers have to be described by a three phase model consisting of a mobile amorphous (MAF), a crystalline (CF), and a rigid amorphous fraction (RAF). For nanocomposites based on a semicrystalline polymer the RAF is due to both the crystallites (RAFcrystal) and the filler (RAFfiller). Polymer nanocomposite based on poly(L-lactide) and MgAl layered double hydroxide nanofiller were prepared. Due to the low crystallization rate of PLA ist crystallization can be suppressed by a high enough cooling rate, and the RAF is due only to the nanofiller. The MAF, CF, and RAF were estimated by Temperature Modulated DSC. For the first time CF, MAF, RAFcrystal, and RAFfiller could be estimated. It was found, that RAFfiller increases linearly with the concentration of the nanofiller for this system. Furthermore, RAFcrystal is only slightly influenced by the presence of the nanofiller. KW - Polymer based nanocomposites PY - 2017 U6 - https://doi.org/10.1016/j.polymer.2016.11.065 SN - 0032-3861 SN - 1873-2291 VL - 108 SP - 257 EP - 264 PB - Elesevier AN - OPUS4-39052 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Häusler, Ines A1 - Moeck, P. A1 - Volz, K. A1 - Neumann, W. T1 - Orientation relationships of Mn0.75Ga0.25As crystallites on and within GaAs determined by scanning nano beam electron diffraction N2 - Mn0.75Ga0.25As crystallites, partially embedded on and fully embedded within a single crystalline matrix of GaAs formed during metal organic vapor phase epitaxy (MOVPE) of Mn-rich (Mn,Ga)As on (001) oriented GaAs wafers. Phase and orientation analysis of these crystallites were performed with scanning nano beam electron diffraction (SNBED). The investigation of plan-view specimens using a liquid nitrogen cooling stage enabled the phase and orientation analysis of partially embedded ferromagnetic a-phase particles. In all specimens the following two orientation relationships (O) between the a-phase particles and the GaAs matrix were determined: O1: [1-2.0] Mn0.75Ga0.25As || [110] GaAs and [10.2] Mn0.75Ga0.25As || [-110] GaAs O2: [10.2] Mn0.75Ga0.25As || [110] GaAs and [1-2.0] Mn0.75Ga0.25As || [-110] GaAs. The study of cross-sectional specimens enabled the analysis of fully embedded crystallites. It could be unambiguously detected that a fully embedded crystallite has the structure of the atomically ordered monoclinic β' phase. The β' phase crystallite consists of two domains which are related in twin positions to each other. The orientation relations of the different particles are illustrated by color coded stereographic projections. KW - (Mn,Ga)As crystallites KW - Scanning nano beam electron diffraction KW - Crystal phase determination KW - Orientation mapping KW - STEM/TEM imaging PY - 2017 U6 - https://doi.org/10.1002/crat.201600261 SN - 1521-4079 SN - 0232-1300 VL - 52 IS - 1, Special Issue: Anniversary Issue: 50 Years of Crystal Research & Technology SP - 138 EP - 145 PB - Wiley AN - OPUS4-38939 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -