TY - JOUR A1 - Heilmann, Maria A1 - Simões, R. G. A1 - Bernardes, C. E. S. A1 - Ramisch, Yen A1 - Bienert, Ralf A1 - Röllig, Matthias A1 - Emmerling, Franziska A1 - Minas da Piedade, M. E. T1 - Real-Time In situ XRD Study of Simvastatin Crystallization in Levitated Droplets N2 - Simvastatin (SV) is an important active pharmaceutical ingredient (API) for treatment of hyperlipidemias, which is known to exist in different crystalline and amorphous phases. It is, therefore, an interesting model to investigate how the outcome of evaporative crystallization in the contactless environment of an acoustically levitated droplet may be influenced by key experimental conditions, such as temperature, solvent properties (e.g., polarity and hygroscopicity), and dynamics of the evaporation process. Here, we describe a real-time and in situ study of simvastatin evaporative crystallization from droplets of three solvents that differ in volatility, polarity, and protic character (acetone, ethanol, and ethyl acetate). The droplet monitorization relied on synchrotron X-ray diffraction (XRD), Raman spectroscopy, imaging, and thermographic analysis. A pronounced solvent-dependent behavior was observed. In ethanol, a simvastatin amorphous gel-like material was produced, which showed no tendency for crystallization over time; in ethyl acetate, a glassy material was formed, which crystallized on storage over a two-week period to yield simvastatin form I; and in acetone, form I crystallized upon solvent evaporation without any evident presence of a stable amorphous intermediate. The XRD and Raman results further suggested that the persistent amorphous phase obtained from ethanol and the amorphous precrystallization intermediate formed in ethyl acetate were similar. Thermographic analysis indicated that the evaporation process was accompanied by a considerable temperature decrease of the droplet surface, whose magnitude and rate correlated with the solvent volatility (acetone > ethyl acetate > ethanol). The combined thermographic and XRD results also suggested that, as the cooling effect increased, so did the amount of residual water (most likely captured from the atmosphere) remaining in the droplet after the organic solvent was lost. Finally, the interpretation of the water fingerprint in the XRD time profiles was aided by molecular dynamics simulations, which also provided insights into the possible role of H2O as an antisolvent that facilitates simvastatin crystallization. KW - Simvastatin KW - In-situ KW - API KW - Crystallization PY - 2021 DO - https://doi.org/10.1021/acs.cgd.1c00509 SN - 1528-7483 VL - 21 IS - 8 SP - 4665 EP - 4673 PB - ACS Publications AN - OPUS4-53663 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Friedrich, Jörg A1 - Altmann, Korinna A1 - Wettmarshausen, Sascha A1 - Hidde, Gundula T1 - Coating of carbon fibers with adhesion-promoting thin polymer layers using plasma polymerization or electrospray ionization technique—A comparison N2 - Plasma polymers and electrospray-ionization (ESI) polymer layers are compared for most efficient adhesion promotion in carbon fiber-epoxy resin composites. The ultra-thin ESI layers (2–30 nm) of commercial poly(acrylic acid) and poly-(hydroxyethylmethacrylate) produce an significant increase of adhesion measured by single-fiber pull out tests. However, plasma Treatment has also advantages, such as simultaneous activation of the fiber substrate. Chemical structure and composition are rather far from the regular structure of commercial polymers as deposited by ESI processing. KW - Plasma polymers KW - Electrospray ionization polymers KW - Poly(acrylic acid) KW - Poly- (hydroxyethylmethacrylate) PY - 2017 DO - https://doi.org/10.1002/ppap.201600074 SN - 1612-8869 SN - 1612-8850 VL - 14 IS - 3 SP - e1600074-1 EP - 14 AN - OPUS4-40510 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nehls, Irene A1 - Hanebeck, Olaf A1 - Becker, Roland A1 - Emmerling, Franziska T1 - N-(beta-carboxyethyl)-alpha-isoleucine N2 - The title compound, {2-[(2-carbamoylethyl)amino]-3-methylpentanoic acid}, C9H18N2O3, is of interest with respect to its biological activity. It was formed during an addition reaction between acrylamide and the amino acid isoleucine. The crystal structure is a three-dimensional network built up by intermolecular N–H···O and O–H···N hydrogen bonds. KW - Acrylamid KW - Isoleucin KW - Derivatisierung PY - 2013 DO - https://doi.org/10.1107/S160053681205146X SN - 1600-5368 VL - 69 IS - Part 2 SP - o172-o173, sup-1 - sup-7 PB - Munksgaard CY - Copenhagen AN - OPUS4-27573 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peplinski, Burkhard A1 - Fitch, A.N. A1 - Evans, A. A1 - Ibberson, R.M. A1 - Többens, D.M. A1 - Cranswick, L.M.D. A1 - Dörfel, Ilona A1 - Emmerling, Franziska A1 - Matschat, Ralf T1 - Structural characterization of a coarse-grained transparent silicon carbide powder by a combination of powder diffraction techniques N2 - Diffraction of hard synchrotron radiation as well as constant-wavelength and time-of-flight neutron diffraction were used for the structural characterization of a silicon carbide powder having extremely low levels of chemical impurities, high perfection of the crystalline lattice and a grain size of up to 150 µm. The presence of three polytypes was ascertained and the ratios of their mass fractions were determined to be w15R : w6H = 0.002,3(8) and w4H : w6H = 0.000,6(2). KW - Silicon carbide KW - Polytypes KW - Phase quantification KW - Reference material PY - 2009 DO - https://doi.org/10.1524/zksu.2009.0009 SN - 0930-486X VL - 30 EPDIC 2008 SP - 61 EP - 66 PB - Oldenbourg CY - München AN - OPUS4-20561 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Polte, Jörg A1 - Ahner, T. T. A1 - Delißen, Friedmar A1 - Sokolov, S. A1 - Emmerling, Franziska A1 - Thünemann, Andreas A1 - Kraehnert, R. T1 - Mechanism of gold nanoparticle formation in the classical citrate synthesis method derived from coupled in situ XANES and SAXS evaluation PY - 2010 DO - https://doi.org/10.1021/ja906506j SN - 0002-7863 SN - 1520-5126 VL - 132 IS - 4 SP - 1296 EP - 1301 PB - American Chemical Society CY - Washington, DC AN - OPUS4-23048 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Zänker, Steffen A1 - Scholz, G. A1 - Heise, M. A1 - Kemnitz, E. A1 - Emmerling, Franziska T1 - New 2D layered structures with direct fluorine-metal bonds: MF(CH3COO) (M: Sr, Ba, Pb) N2 - New coordination polymers with 2D network structures with fluorine directly coordinated to the metal ion were prepared both via mechanochemical synthesis and fluorolytic sol–gel synthesis. Depending on the synthesis route, the samples show different particle sizes, according to SEM imaging. The crystal structures of barium acetate fluoride, strontium acetate fluoride, and lead acetate fluoride (BaFIJCH3COO), SrFIJCH3COO) and PbFIJCH3COO)) were solved from X-ray powder diffraction data. The structure solution is backed by the results from 19F MAS NMR, FT IR data, and thermal analysis. The calculated chemical shifts of the 19F MAS NMR spectra coincide well with the measured ones. It turns out that the grinding conditions have a remarkable influence on the mechanochemical synthesis and its products. Our systematic study also indicates a strong influence of the atomic radii of Ca, Sr, Ba, and Pb on the success of the syntheses. KW - Mechanochemistry KW - Coordination polymers PY - 2020 DO - https://doi.org/10.1039/d0ce00287a VL - 22 IS - 16 SP - 2772 EP - 2780 PB - Royal Society of Chemistry AN - OPUS4-50789 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Walther, M. A1 - Matterna, M. A1 - Juran, S. A1 - Fähnemann, S. A1 - Stephan, H. A1 - Kraus, Werner A1 - Emmerling, Franziska T1 - Imidazole-containing bispidine ligands: synthesis, structure and Cu(II) complexation N2 - The preparation and characterization of tris-pyridyl bispidine (3,7-diazabicyclo[3.3.1]nonane) derivatives with benzimidazole and imidazole donor groups at the N-3 position of the bispidine Skeleton and their copper(II) complexes are reported. The impact of the hetaryl substituents on the configurational isomerism of piperidones and their corresponding bispidones has been studied by NMR spectroscopy, revealing the exclusive appearance in the enol form for the piperidones in solution and the trans-configuration regarding the two pyridyl substituents, as well as the sole formation of the unsymmetric exo-endo isomers for the corresponding bispidones. Thus, the bispidones are preorganized ligands for building pentacoordinated complexes, confirmed by the preparation and characterization of the corresponding Cu(II) complexes. Of the di-pyridyl piperidones with benzimidazole and imidazole substituents, and of the Cu(II) complex of the benzimidazole-containing bispidone, Crystals have become available for the analysis by X-ray diffraction, showing that the piperidones form the enol tautomers also in the solid state. KW - Piperidone KW - Bispidine KW - Copper(II) KW - Configuration isomerism PY - 2011 SN - 0932-0776 SN - 0340-5087 SN - 0044-3174 VL - 66b SP - 721 EP - 728 PB - Verl. d. Zeitschrift für Naturforschung CY - Tübingen AN - OPUS4-24091 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peplinski, Burkhard A1 - Adam, Christian A1 - Adamczyk, Burkart A1 - Müller, Ralf A1 - Schadrack, Reinhard A1 - Michaelis, Matthias A1 - Emmerling, Franziska A1 - Reuther, H. A1 - Menzel, Michael T1 - Evidence of formation of the tridymite form of AlPO4 in some municipal sewage sludge ashes N2 - Evidence is provided that the tridymite component observed in the X-ray diffraction patterns of some sewage sludge ashes (SSAs) should not be interpreted as the tridymite modification of SiO2 but as the tridymite form of AlPO4. This proof is based on a combined X-ray Powder Diffraction (XRD), X-ray fluorescence (XRF) and Mossbauer spectroscopy investigation of two SSAs produced at two fluidized bed incineration facilities, located in different municipalities and operated differently. The structural and chemical characterization was carried out on the 'as received' SSA samples as well as on the residues of these two SSAs pretreated by leaching in citric acid. In addition, direct proof is presented that the tridymite form of AlPO4 does crystallize from X-ray amorphous precursors under conditions that mimic the huge heating rate and short retention time (just seconds at T ≈ 850 °C) typical for fluidized bed incinerators. KW - Aluminium phosphate KW - Ash KW - Fly ash KW - Incinerator ash KW - Sewage sludge ash KW - Tridymite form PY - 2013 DO - https://doi.org/10.1017/S0885715613000869 SN - 0885-7156 VL - 28 IS - S2 SP - S425 EP - S435 PB - JCPDS CY - Swarthmore, Pa. AN - OPUS4-29703 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Thünemann, Andreas A1 - Kegel, Jenny A1 - Polte, Jörg A1 - Emmerling, Franziska T1 - Superparamagnetic Maghemite Nanorods: Analysis by Coupling Field-Flow Fractionation and Small-Angle X-ray Scattering N2 - We report on the online coupling of asymmetrical flow field-flow fractionation (A4F) with small-angle X-ray scattering (SAXS) for the detection of nanoparticles. The A4F was used to fractionate superparamagnetic maghemite nanoparticles, which were prepared continuously with a micromixer. The outlet of the A4F was directly coupled to a flow capillary of a SAXSess instrument (Kratky type of camera). SAXS curves were recorded in a 1 s time interval. This was possible by using intense synchrotron radiation. The radii of gyration of the nanoparticles, as determined from Guinier plots, increased from 2 to 6 nm with increasing fractionation time of the A4F. A more detailed analysis of the scattering curves revealed that the particles were cylindrical in shape (nanorods), which we attributed to the micromixing preparation technique. The radii of the nanorods increased only slightly from 1.2 to 1.7 nm with increasing fractionation time, while the lengths increased strongly from 7.0 to 30.0 nm. The volume distribution of the nanorods was determined and described by Schultz-Zimm and log-normal distributions. Nanorod volumes increased from 45 to 263 nm³, corresponding to molar masses of 140 × 10³ to 820 × 10³ g mol-1. We propose A4F-SAXS coupling as a new method for analysis of nanoparticles of complex composition in solution. It allows precise online determination of the particle’s shape and size distributions. This method can be applied to mixtures of nanoparticles of arbitrary shapes and sizes (1-100 nm). Moreover, the total time needed for fractionation and online SAXS data recording is usually only 20 min. PY - 2008 DO - https://doi.org/10.1021/ac8004814 SN - 0003-2700 SN - 1520-6882 VL - 80 IS - 15 SP - 5905 EP - 5911 PB - American Chemical Society CY - Washington, DC AN - OPUS4-17813 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peplinski, Burkhard A1 - Adamczyk, Burkart A1 - Kley, Gerd A1 - Adam, Karin A1 - Emmerling, Franziska A1 - Simon, Franz-Georg T1 - New horizons of the structural characterization of stainless steel slags by X-ray powder diffraction KW - AOD slag KW - Metal recovery KW - Metallurgy KW - Rietveld method KW - Slags KW - Stainless steel slags KW - Quantitative phase analysis (QPA) PY - 2007 SN - 0930-486X VL - 26 SP - 61 EP - 66 PB - Oldenbourg CY - München AN - OPUS4-16666 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wolf, S. E. A1 - Müller, L. A1 - Barrea, R. A1 - Kampf, C.J. A1 - Leiterer, Jork A1 - Panne, Ulrich A1 - Hoffmann, T. A1 - Emmerling, Franziska A1 - Tremel, W. T1 - Carbonate-coordinated metal complexes precede the formation of liquid amorphous mineral emulsions of divalent metal carbonates N2 - During the mineralisation of metal carbonates MCO3 (M = Ca, Sr, Ba, Mn, Cd, Pb) liquid-like amorphous intermediates emerge. These intermediates that form via a liquid/liquid phase separation behave like a classical emulsion and are stabilized electrostatically. The occurrence of these intermediates is attributed to the formation of highly hydrated networks whose stability is mainly based on weak interactions and the variability of the metal-containing pre-critical clusters. Their existence and compositional freedom are evidenced by electrospray ionization mass spectrometry (ESI-MS). Liquid intermediates in non-classical crystallisation pathways seem to be more common than assumed. PY - 2011 DO - https://doi.org/10.1039/c0nr00761g SN - 2040-3364 SN - 2040-3372 IS - 3 SP - 1158 EP - 1165 PB - RSC Publ. CY - Cambridge AN - OPUS4-23355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Peplinski, Burkhard A1 - Adamczyk, Burkart A1 - Formanek, P. A1 - Meyer, Christian A1 - Krüger, O. A1 - Scharf, Holger A1 - Reinsch, Stefan A1 - Ostermann, Markus A1 - Nofz, Marianne A1 - Jäger, Christian A1 - Adam, Christian A1 - Emmerling, Franziska T1 - Nanocrystalline and stacking-disordered beta-cristobalite AlPO4 chemically stabilized at room temperature: synthesis, physical characterization, and X-ray powder diffraction data N2 - This paper reports the first successful synthesis and the structural characterization of nanocrystalline and stacking-disordered β-cristobalite AlPO4 that is chemically stabilized down to room temperature and free of crystalline impurity phases. Several batches of the title compound were synthesized and thoroughly characterized by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy, selected area electron diffraction, energy dispersive X-ray spectroscopy mapping in SEM, solid-state 31P nuclear magnetic resonance (31P-NMR) spectroscopy including the TRAPDOR method, differential thermal analysis (DTA), gas-sorption methods, optical Emission spectroscopy, X-ray fluorescence spectroscopy, and ion chromatography. Parameters that are critical for the synthesis were identified and optimized. The synthesis procedure yields reproducible results and is well documented. A high-quality XRD pattern of the title compound is presented, which was collected with monochromatic copper radiation at room temperature in a wide 2θ range of 5°–100°. KW - Stabilization of high-temperature phase at RT KW - Nanochrystalline AlPO4 KW - Beta-christobalite structure type KW - High-cristobalite form KW - Aluminium phosphate PY - 2017 DO - https://doi.org/10.1017/S0885715617000537 SN - 1945-7413 SN - 0885-7156 VL - 32 IS - S1 SP - S193 EP - S200 PB - JCPDS-ICDD CY - Cambridge AN - OPUS4-42235 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Klimakow, Maria A1 - Leiterer, Jork A1 - Kneipp, Janina A1 - Rössler, E. A1 - Panne, Ulrich A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Combined synchrotron XRD/Raman measurements: In situ identification of polymorphic transitions during crystallization processes N2 - A combination of two analytical methods, time-resolved X-ray diffraction (XRD) and Raman spectroscopy, is presented as a novel tool for crystallization studies. An acoustic levitator was employed as sample environment. This setup enables the acquisition of XRD and Raman data in situ simultaneously within a 20 s period and hence permits investigation of polymorphic phase transitions during the crystallization process in different solvents (methanol, ethanol, acetone, dichloromethane, acetonitrile). These real time measurements allow the determination of the phase content from the onset of the first crystalline molecular assemblies to the stable system. To evaluate the capability of this approach, the setup was applied to elucidate the crystallization process of the polymorphic compound nifedipine. The results indicate the existence of solvent-dependent transient phases during the crystallization process. The quality of the data allowed the assignment of the lattice constants of the hitherto unknown crystal structure of the β-polymorph. KW - Synchrotron radiation KW - XRD KW - Raman spectroscopy KW - Polymorphism KW - Crystallization KW - Acoustic levitation KW - Nifedipine PY - 2010 DO - https://doi.org/10.1021/la100540q SN - 0743-7463 SN - 1520-5827 VL - 26 IS - 13 SP - 11233 EP - 11237 PB - American Chemical Society CY - Washington, DC AN - OPUS4-21396 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kahlau, R. A1 - Gnutzmann, Tanja A1 - Emmerling, Franziska A1 - Rademann, K. A1 - Rössler, E.A. T1 - Quinaldine: Accessing two crystalline polymorphs via the supercooled liquid N2 - Quinaldine (2-methyl quinoline) is a liquid at room temperature, which can be supercooled to reach finally the glassy state. By heating the glass above the glass transition temperature Tg = 180 K the sample performs two subsequent transitions into, likewise, dielectrically active phases. Thus, the reorientational relaxations of these phases as well as the kinetics of the phase transitions can be tracked in a highly resolved way by dielectric spectroscopy. X-ray diffraction analysis clearly shows two structurally different crystalline phases in addition to the supercooled liquid. Calorimetric measurements support the notion of first order phase transitions, occurring irreversibly in the supercooled regime, and suggest that the intermediate crystalline phase is metastable, too. Analyzing the quite distinct dielectric relaxation strengths, we discuss the possible nature of the two crystalline phases. Additionally, a very similar behavior to quinaldine is observed for 3-methyl quinoline, indicating a broad field of polymorphism among the quinoline derivatives. KW - Calorimetry KW - Dielectric liquids KW - Dielectric relaxation KW - Glass transition KW - Liquid structure KW - Organic compounds KW - Polymorphism KW - Supercooling KW - X-ray diffraction PY - 2012 DO - https://doi.org/10.1063/1.4738583 SN - 0021-9606 SN - 1089-7690 VL - 137 IS - 5 SP - 054505-1 - 054505-10 PB - American Institute of Physics CY - Melville, NY AN - OPUS4-26347 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Leiterer, Jork A1 - Leitenberger, W. A1 - Emmerling, Franziska A1 - Thünemann, Andreas A1 - Panne, Ulrich T1 - The use of an acoustic levitator to follow crystallization in small droplets by energy-dispersive X-ray diffraction N2 - For the investigation of small sample volumes, the use of an acoustic levitator was tested as a `sample holder' for hovering droplets in a synchrotron beam. It might be advantageous to use levitated droplets instead of samples confined in solid holders, especially for the study of crystallization processes where the influence of containing walls has to be minimized. In a first experiment, the crystallization of sodium chloride in a small droplet of aqueous solution has been followed with a time resolution of 30 s. The collected diffraction peaks are compared with data in the ICSD database. KW - EDXD KW - Noncontact measurement technique KW - X-ray-scattering KW - Synchrotron-radiation KW - Acoustic levitation PY - 2006 DO - https://doi.org/10.1107/S0021889806024915 SN - 0021-8898 SN - 1600-5767 VL - 39 IS - 5 SP - 771 EP - 773 PB - Blackwell CY - Oxford AN - OPUS4-13516 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mönch, Bettina A1 - Emmerling, Franziska A1 - Kraus, Werner A1 - Becker, Roland A1 - Nehls, Irene T1 - n-Propyl 2,3,4,6-tetra-O-acetyl-beta-D-glucopyranoside N2 - The title compound [systematic name: (2R,3R,4S,5R,6R) 2-(acetoxymethyl)-6-propoxytetrahydro-2H-pyran-3,4,5-triyl triacetate], C17H26O10, was formed by a Koenigs-Knorr reaction of 2,3,4,6-tetra-O-acetyl-α-D-glucopyranosyl bromide and n-propanol. The central ring adopts a chair conformation. The crystal does not contain any significant interactions such as hydrogen bonds. PY - 2013 DO - https://doi.org/10.1107/S1600536812051495 SN - 1600-5368 VL - 69 IS - Part 2 SP - o158, sup-1 - sup-7 PB - Munksgaard CY - Copenhagen AN - OPUS4-27439 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wolf, S. E. A1 - Lieberwirth, I. A1 - Natalio, F. A1 - Bardeau, J.-F. A1 - Delorme, N. A1 - Emmerling, Franziska A1 - Barrea, R. A1 - Kappl, M. A1 - Marin, F. T1 - Merging models of biomineralisation with concepts of nonclassical crystallisation: is a liquid amorphous precursor involved in the formation of the prismatic layer of the Mediterranean Fan Mussel Pinna nobilis? N2 - The calcitic prisms of Pinna nobilis (Pinnidae, Linnaeus 1758) are shown to be perfect examples of a mesocrystalline material. Based on their ultrastructure and on the occurrence of an amorphous transient precursor during the early stages of prism formation, we provide evidence for the pathway of mesocrystallisation proposed by Seto et al. (2012), which proceeds not by self-organized oriented attachment of crystalline nano-bricks but by aggregation of initially amorphous nanogranules which later transform by epitaxial nucleation to a three-dimensional array of well aligned nanocrystals. We further fathom the role of a liquid amorphous calcium carbonate in biomineralisation processes and provide strong evidence for the occurrence of PILP-like intermediates during prism formation. We develop a new scenario of prism formation based on the presented findings presented findings and discuss the implications of a speculative liquid amorphous calcium carbonate (LACC) intermediate in vivo. PY - 2012 DO - https://doi.org/10.1039/c2fd20045g SN - 1359-6640 SN - 1364-5498 VL - 159 IS - 0 SP - 433 EP - 448 PB - Soc. CY - Cambridge [u.a.] AN - OPUS4-27122 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emmerling, Franziska A1 - Orgzall, I. A1 - Dietzel, B. A1 - Schulz, B. A1 - Larrucea, J. T1 - Ordering the amorphous - Structures in PBD LED materials N2 - The class of 2,5 disubstituted-1,3,4-oxadiazoles containing a biphenyl unit on one side is intensively used as electron transport materials to enhance the performance of organic light emitting diodes (OLEDs). In contrast to the ongoing research on these materials insights in their structure-property relationships are still incomplete. To overcome the structural tentativeness and ambiguities the crystal structures of 2-(4-biphenylyl)-5-(4-tert-butylphenyl)-1,3,4-oxadiazole, that of the related compound 2-(4-biphenylyl)-5-phenyl-1,3,4-oxadiazole and of 2-(4-biphenylyl)-5-(2,6-dimethylphenyl)-1,3,4-oxadiazole are determined. A comparison with the results of GAUSSIAN03 calculations and similar compounds in the Cambridge Structural Database leads to a profound characterization. KW - OLED KW - PBD KW - Diphenyl-1,3,4-oxadiazole KW - Crystallization PY - 2012 DO - https://doi.org/10.1016/j.molstruc.2012.04.040 SN - 0022-2860 SN - 1872-8014 SN - 0377-046X VL - 1030 SP - 209 EP - 215 PB - Elsevier CY - Amsterdam AN - OPUS4-27264 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Brirmi, M A1 - Chabbah, T. A1 - Chatti, S. A1 - Schiets, F. A1 - Casabianca, H. A1 - Marestin, C. A1 - Mercier, R. A1 - Weidner, Steffen A1 - Errachid, A. A1 - Jaffrezic-Renault, N. A1 - Ben Romdhane, H. T1 - Effect of the pendent groups on biobased polymers, obtained from click chemistry suitable, for the adsorption of organic pollutants from water N2 - In this work, four triazole-based poly(ether-pyridine)s polymers were synthesized and used as an adsorbent for the removal of phenolic compounds from aqueous solutions. For this purpose, new fluoromonomers containing 1,2,3-triazole units were prepared by the Cu(I)-catalyzed 1,3-dipolar cycloaddition reaction and then used for the elaboration of novel poly(ether-pyridine-triazole)s (PEPTs) by direct polyconden-sation with isosorbide and bisphenol A. Chemical structure of fluorinated pyridinicmonomers as well as resulting polymers was confirmed by 1H and 19F NMR spectroscopic methods. The thermal behavior of the obtained PEPTs was characterized using differential scanning calorimetry and thermogravimetric analysis. Results of sorption showed that polymers can be effectively used as a sorbent for the removal of polarorganic pollutants. The isosorbide-based poly(ether-pyridine-triazole) which contains hydrophilic hydroxyl groups as pendants chains (P4) exhibited the highest sorption efficiencies (78%–100% after 1 h). In order to explain the results an adsorption mech-anism mainly based on π–π interactions and hydrogen bonding with the pendent groups is proposed. KW - Adsorption KW - Biobased polymers KW - Cycloaddition KW - Pentafluoropyridine KW - Phenolic compounds PY - 2022 DO - https://doi.org/10.1002/pat.5809 SN - 1042-7147 SP - 1 EP - 21 PB - Wiley online library AN - OPUS4-55389 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Jlalia, I. A1 - Gomri, M. A1 - Chabbah, T. A1 - Chatti, S. A1 - Weidner, Steffen A1 - Abderrazak, H. A1 - Marestin, C. A1 - Mercier, R. A1 - Ben Halima, H. A1 - Lakard, B. A1 - Jaffrezic Renault, N. T1 - Design of Fluorinated Poly(Ether-Pyridine) Films for Impedimetric Detection of Heavy Metal Ions N2 - A series of fluorinated poly(ether-pyridine)s were synthesized via polycondensation of bis-perfluoropyridine with either bisphe-nol A (BPA) or isosorbide, a bio-sourced diol. The polymers were characterized using 1 H and 19 F NMR spectroscopy, and their molecular weights were determined using GPC. Thermal properties were assessed using thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC). The presence of isosorbide in polymer P2 increases the glass transition temperature and results in a lower molecular weight and a higher hydrophilicity. On the other hand, polymer P3, based on BPA, shows the best thermal stability, the highest molecular weight, and the most pronounced hydrophobic character. Electrochemical impedance spectroscopy (EIS) was used to evaluate the modified gold electrodes for the selective detection of metal ions. Among the four target ions (Ni 2+, Cd 2+, Pb2+, and Hg 2+), defined by the European Water Framework Directive, Pb2+ was selectively detected on the hydrophilic polymer P2, while Cd 2+ was selectively detected on the hydrophobic polymer P3. The achieved detection limits were 5 × 10−11 M, corresponding to 10 ng/L for Pb2+ and 5.6 ng/L for Cd 2+, respectively. KW - Cadmium KW - Electrochemical impedance spectroscopy KW - Fluorinated polyether pyridines KW - Isosorbide KW - Lead PY - 2025 DO - https://doi.org/10.1002/pat.70038 SN - 1099-1581 VL - 36 IS - 1 SP - 1 EP - 14 PB - John Wiley & Sons Ltd. AN - OPUS4-62384 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chabbah, T. A1 - Chatti, S. A1 - Zouaoui, F. A1 - Jlalia, A. A1 - Gaiji, H. A1 - Abderrazak, H. A1 - Casablanca, H. A1 - Mercier, R. A1 - Weidner, Steffen A1 - Errachid, A. A1 - Marestin, C. A1 - Jaffrezic-Renault, N. T1 - New poly(ether-phosphoramide)s sulfides based on green resources as sensitive films for the specific impedimetric detection of nickel ions N2 - For the development of selective and sensitive chemical sensors, we have developed a new family of poly(etherphosphoramide) polymers. These polymers were obtained with satisfactory yields by nucleophilic aromatic polycondensation using isosorbide as green resources, and bisphenol A with two novel difluoro phosphinothioic amide monomers. Unprecedented, the thiophosphorylated aminoheterocycles monomers, functionalized with two heterocyclic amine, N-methylpiperazine and morpholine were successfully obtained by nucleophilic substitution reaction of P(S)–Cl compound. The resulting polymers were characterized by different analytical techniques (NMR, MALDI–ToF MS, GPC, DSC, and ATG). The resulting partially green polymers, having tertiary phosphine sulfide with P–N side chain functionalities along the main chain of polymers are the sensitive film at the surface of a gold electrode for the impedimetric detection of Cd, Ni, Pb and Hg. The bio-based poly(etherphosphoramide) functionalized with N-methylpiperazine modified sensor showed better analytical performance than petrochemical based polymers for the detection of Ni2+. A detection limit of 50 pM was obtained which is very low compared to the previously published electrochemical sensors for nickel detection. KW - Poly(ether-phosphoramide)s sulfides KW - Green chemistry KW - Polymer film KW - MALDI TOF MS PY - 2022 DO - https://doi.org/10.1016/j.talanta.2022.123550 VL - 247 IS - 123550 SP - 1 EP - 9 PB - Elsevier B.V. AN - OPUS4-54980 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Chabbah, T. A1 - Chatti, S. A1 - Jaffrezic-Renault, N. A1 - Weidner, Steffen A1 - Marestin, C. A1 - Mercier, R. T1 - Impedimetric sensors based on diethylphosphonate-containingpoly(arylene ether nitrile)s films for the detection of lead ions N2 - This article describes the elaboration and characterization of diethylphosphonate-containing polymers coated electrodes as sensors for the detection of heavy metalstraces, by electrochemical impedance spectroscopy. Diethylphosphonate groupswere chosen as heavy metals binding sites. Two different series of polymers bearingthese anchoring groups were synthesized. Whereas the diethylphosphonate groupsare directly incorporated in the aromatic macromolecular chain in some polymers, analiphatic spacer is removing the chelating site from the polymer backbone in others.The influence of the macromolecular structure on the sensing response was studied,especially for the detection of Pb2+,Ni2+,Cd2+and Hg2+. Polymer P6, including thehigher amount of diethylphosphonate groups removed from the polymer chain by ashort alkyl spacer gave the higher sensitivity of detection of lead ions, with a detec-tion limit of 50 pM KW - Heavy metals KW - Phosphonate esters KW - Lead ions KW - MALDI TOF MS PY - 2023 DO - https://doi.org/10.1002/pat.6065 SN - 1042-7147 SP - 1 EP - 11 PB - John Wiley & Sons, Ltd AN - OPUS4-57356 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rösler, Alexander A1 - Weidner, Steffen A1 - Klamroth, Tillmann A1 - Müller, Axel HE A1 - Schlaad, Helmut T1 - Kinetics of anionic polymerization of β‐myrcene in hydrocarbon solvents N2 - AbstractThe kinetics of anionic polymerization of β‐myrcene initiated by sec‐butyllithium were examined in saturated and unsaturated hydrocarbon solvents, i.e. cyclohexane, cyclohexene, 4‐vinylcyclohexene and dl‐limonene. Polymerizations usually proceeded in a living manner, i.e. in the absence of termination and chain transfer reactions, in all solvents, to produce well‐defined polymyrcenes with high content (85%) of cis‐1,4 units. However, polymyrcenyllithium chains exhibited limited long‐term stability in 4‐vinylcyclohexene solution, most probably due to chain transfer to solvent. Reaction orders with respect to the concentration of active chains were found to be one‐quarter in cyclohexane increasing to one‐half in unsaturated solvents, indicating that the polymyrcenyllithium chains are present as tetrameric or dimeric associates, respectively. Apparent activation energies were found to be 81 kJ mol−1 in cyclohexane and 77 kJ mol−1 in dl‐limonene solution, which are close to the values obtained by quantum chemical calculations. © 2025 The Author(s). Polymer International published by John Wiley & Sons Ltd on behalf of Society of Chemical Industry. KW - Myrcene KW - Anionic polymerization KW - MALDI TOF MS PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-649039 DO - https://doi.org/10.1002/pi.6772 SN - 0959-8103 SP - 1 EP - 8 PB - Wiley AN - OPUS4-64903 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weidner, Steffen A1 - Kühn, Gerhard A1 - Decker, Renate A1 - Roessner, D. A1 - Friedrich, Jörg Florian T1 - Influence of Plasma Treatment on the Molar Mass of Poly(ethylene terephthalate) Investigated by Different Chromatographic and Spectroscopic Methods N2 - The influence of different types of low and atmospheric pressure plasma on poly(ethylene terephthalate) (PET) has been studied in terms of changes in molar mass and molar mass distribution. Apart from a variation of plasma gases (oxygen, helium) different types of plasma (microwave, radio frequency, corona discharge) were used for the plasma surface modification. The changes in molar mass and types of functional end groups of lower molar mass products were investigated by means of matrix-assisted laser desorption/ionization time of flight mass spectrometry (MALDI-TOFMS), whereas the high-molar mass fraction was analyzed by means of size-exclusion chromatography (SEC). The formation of crosslinked products during exposure to a helium plasma, which emits preponderately energy-rich and intense ultraviolet radiation, was proved by means of thermal field-flow fractionation (ThFFF). This method combined with a multiangle laser light scattering (MALLS) detector allows detection of weakly crosslinked polymers and microgels. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1639-1648, 1998 KW - Poly(ethylene terephthalate) KW - PET KW - Plasma PY - 1998 UR - http://www3.interscience.wiley.com/cgi-bin/abstract/36482/ABSTRACT DO - https://doi.org/10.1002/(SICI)1099-0518(19980730)36:10<1639::AID-POLA17>3.0.CO;2-H SN - 0360-6376 SN - 0887-624X VL - 36 IS - 10 SP - 1639 EP - 1648 PB - Wiley CY - Hoboken, NJ AN - OPUS4-6989 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Czichocki, G. A1 - Fiedler, H. A1 - Haage, K. A1 - Much, Helmut A1 - Weidner, Steffen T1 - Characterization of alkyl polyglycosides by both reversed-phase and normal-phase modes of high-performance liquid chromatography N2 - Alkyl polyglycosides today represent the most important sugar surfactant. Nonionic sugar surfactants produced via different synthetic routes are mixtures of alkyl homologues, oligomers, anomers and isomers. Alkyl homologues and oligomers of alkyl mono- and diglucosides were separated by reversed-phase high-performance liquid chromatography (HPLC) with methanol–water as the mobile phase using a gradient elution. The gradient was optimized in respect to a simultaneous separation of alkyl glycosides according to their alkyl chain length and alkyl polyoxyethylene glucosides with regard to their length of the polyoxyethylene spacer. The separation of alkyl glycosides into ?- and ?-anomers was carried out by normal-phase HPLC with isooctane–ethyl acetate (60:40, v/v)–2-propanol in the gradient mode. Light scattering detection was used. Matrix-assisted laser desorption ionization time-of-flight mass spectra of alkyl glucosides and dodecyl glucosides with oxyethylene spacer groups are presented. PY - 2002 DO - https://doi.org/10.1016/S0021-9673(01)01459-5 SN - 0021-9673 VL - 943 IS - 2 SP - 241 EP - 250 PB - Elsevier CY - Amsterdam AN - OPUS4-11099 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Braun, Ulrike A1 - Wachtendorf, Volker A1 - Geburtig, Anja A1 - Bahr, Horst A1 - Schartel, Bernhard T1 - Weathering resistance of halogen-free flame retardance in thermoplastics N2 - The influence of weathering on the fire retardancy of polymers is investigated by means of a cone calorimeter test, before and after artificial weathering. The surface degradation was monitored using different techniques (ATR–FTIR, microscopy, colour measurement). Different kinds of polymeric materials were chosen, all as they are used in practice: polycarbonate (PC) blends, polyamide (PA) and polypropylene (PP) flame-retarded with arylphosphate, melamine cyanurate (MC) and intumescent formulation based on ammonium polyphosphate (APP), respectively. All samples show material degradation at the surface due to weathering. No significant weathering influence occurs on the flame retardancy when it is a bulk property, as was observed for aryl phosphates in PC blends and MC in PA. When the fire retardancy is dominated by a surface mechanism, dependence on the duration of weathering is detected: for intumescent formulations based on ammonium APP in PP, a worsening in the formation of the intumescent network was observed. KW - Fire retardancy KW - Weathering resistance KW - Degradation KW - Intumescence KW - Cone calorimeter PY - 2010 DO - https://doi.org/10.1016/j.polymdegradstab.2010.08.020 SN - 0141-3910 SN - 1873-2321 VL - 95 IS - 12 SP - 2421 EP - 2429 PB - Applied Science Publ. CY - London AN - OPUS4-22612 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Trubiroha, Peter T1 - The Principle of Reciprocity and its Limits T2 - 3rd European Weathering Symposium CY - Krakow, Poland DA - 2007-09-12 KW - Spectral sensitivity KW - Weathering KW - UV KW - Action spectra KW - Activation spectra KW - Stabilizer KW - Spektrale Empfindlichkeit KW - Bewitterung KW - Aktivierungsspektrum KW - Wirkungsspektrum KW - Stabilisator PY - 2007 SN - 978-3-9810472-3-3 VL - 8 SP - 243 EP - 258 CY - Pfinztal AN - OPUS4-15925 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geburtig, Anja A1 - Goedecke, Thomas A1 - Wachtendorf, Volker T1 - Combined impact of ultraviolet and chemical fluids on high-density polyethylene packaging material N2 - To investigate the ageing behaviour of filled plastic containers outdoors, square cuts of the wall of two high-density polyethylene (HDPE) types were exposed to ultraviolet (UV) radiation at their front side and to specific liquid chemicals (de-ionized water, surfactant or White Spirit) at their back. The UV radiant exposure at the front side was 80 MJ/m². To compare the actions of the different exposures, separate dark backside fluid exposures were performed, in parallel. Besides, UV weathering was carried out until a UV radiant exposure of 325 MJ/m², being roughly comparable to outdoor exposure of one year in Northern Australia. An unpigmented HDPE included in the investigation gave no sufficient protection for the White Spirit. In addition, it showed clear degradation after several of these exposures. In combination with the White Spirit, an increase of carbonyl bonds was measured, presumably assignable to degradation products of the White Spirit. For a pigmented HDPE material, with the implemented combined exposures, no relevant damage was observed, within applied the exposure period. KW - Weathering KW - UV KW - HDPE KW - Packaging PY - 2012 DO - https://doi.org/10.1002/pts.959 SN - 0894-3214 VL - 25 IS - 1 SP - 53 EP - 61 PB - Wiley CY - Chichester, UK AN - OPUS4-25417 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Trubiroha, Peter T1 - Referenzmaterialien für Bewitterungsprüfungen T2 - 32. Jahrestagung der GUS, Gesellschaft für Umweltsimulation CY - Pfinztal bei Karlsruhe, Deutschland DA - 2003-03-26 KW - Referenzmaterialien KW - Bewitterung PY - 2003 SN - 3-9808382-1-8 SP - 61 EP - 72 PB - GUS CY - Pfinztal (Berghausen) AN - OPUS4-3360 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Anik, Yavuz A1 - Geburtig, Anja A1 - Sturm, Heinz A1 - Meyer-Plath, Asmus ED - Reichert, T. T1 - CarboLifeCycle -weathering-induced degradation of nanoparticle-functionalised composites N2 - A new research project 'CarboLifeCycle', funded by the German Federal Ministry of Education and Research (BMBF), investigates various nanoparticle release scenarios for carbon nanotube-containing polymer composites. The studied weathering concepts and conditions will be described. T2 - 5th European weathering symposium - Natural and artificial ageing of polymers CY - Lisbon, Portugal DA - 21.09.2011 KW - CNT KW - Nanoparticle KW - Weathering KW - Degradation PY - 2011 SN - 978-3-9813136-2-8 N1 - Serientitel: CEEES Publication – Series title: CEEES Publication IS - 15 SP - 125 EP - 135 PB - GUS (Gesellschaft für Umweltsimulation) CY - Pfinztal AN - OPUS4-24503 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Trubiroha, Peter T1 - Accelerated weathering test for plastics and coatings that are exposed to acidic precipitation N2 - Due to the occurrence of acidic precipitation, and due to the fact that polymers and stabilizers may be sensititve to acids, it is important to have a laboratory test that combines weathering exposure with acidic exposure. The loss of stabilization caused by an acid damage of stabilizing system gets evident only over the weathering progress. For solid samples, for wich mostly the surface properties are relevant, the "Acid Dew and Fog Test" (ADF test) was established. For woven or tufted materials, the "Acid Rain Test" (AR test) was developed. The proposed weathering tests aim at plastics as well as at coatings. T2 - 7th International Symposium on Weatherability (7th ISW) CY - Kanagawa, Japan DA - 2008-10-23 KW - Acid rain KW - ADF KW - Acid Dew and Fog test KW - Artificial Weathering test PY - 2009 SN - 1346-0633 VL - 21 IS - 2 SP - 69 EP - 73 PB - Materiaru-Raifu-Gakkai CY - Tokyo AN - OPUS4-18270 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Wachtendorf, Volker A1 - Geburtig, Anja A1 - Trubiroha, Peter ED - Jonathan W. Martin, ED - Rose A. Ryntz, ED - J. Chin, ED - Ray A. Dickie, T1 - Chemiluminescence detection: Principles, chances and limitations for the shortening of weathering tests T2 - 4th International Symposium on Service Life Prediction CY - Key Largo, FL, USA DA - 2006-12-03 KW - Chemiluminescence KW - Weathering KW - Quantum efficiency KW - Accelerated test KW - Automotive coating KW - PE Chemilumineszenz KW - Bewitterung KW - Quantenausbeute KW - Beschleunigter Test KW - Automobillacke PY - 2008 SN - 978-0-387-84875-4 SP - 309 EP - 326 PB - Springer AN - OPUS4-18245 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Trubiroha, Peter A1 - Wachtendorf, Volker A1 - Geburtig, Anja ED - Ziegahn, K.-F. T1 - Beispiele für die Nutzung des Energietransports durch langwellige (thermische) Strahlung T2 - 35. Jahrestagung der GUS 2006 - Umwelteinflüsse erfassen, simulieren, bewerten CY - Pfinztal, Deutschland DA - 2006-03-22 PY - 2006 SN - 3-9810472-0-6 SP - 205 EP - 214 PB - DWS Werbeagentur und Verlag GmbH CY - Pfinztal AN - OPUS4-21347 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Trubiroha, Peter T1 - Improved Evaluation of Activation Spectra Determined by the Filter Technique T2 - 3rd European Weathering Symposium CY - Krakow, Poland DA - 2007-09-12 KW - Spectral sensitivity KW - Weathering KW - UV KW - Action spectra KW - Activation spectra KW - Stabilizer KW - Spektrale Empfindlichkeit KW - Bewitterung KW - Aktivierungsspektrum KW - Wirkungsspektrum KW - Stabilisator PY - 2007 SN - 978-3-9810472-3-3 VL - 8 SP - 349 EP - 358 CY - Pfinztal AN - OPUS4-15924 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Trubiroha, Peter T1 - Der Einfluss von Feuchte und Nässe bei der Bewitterung T2 - 36. Jahrestagung der GUS 2007 CY - Pfinztal bei Karlsruhe, Deutschland DA - 2007-03-14 KW - Spectral sensitivity KW - Weathering KW - UV KW - Action spectra KW - Activation spectra KW - Stabilizer KW - Spektrale Empfindlichkeit KW - Bewitterung KW - Aktivierungsspektrum KW - Wirkungsspektrum KW - Stabilisator PY - 2007 SN - 978-3-9810472-1-9 VL - 36 SP - 247 EP - 256 CY - Pfinztal AN - OPUS4-14758 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Trubiroha, Peter T1 - Systematisierung der Alterungsvorgänge bei der Bewitterung von Polymerwerkstoffen T2 - 38. Jahrestagung der GUS CY - Stutensee-Blankenloch/Karlsruhe, Deutschland DA - 2009-03-18 KW - Witterungsbeständigkeit KW - Photochemische Alterung PY - 2009 SN - 978-3-9810472-7-1 SP - 51 EP - 60 CY - Pfinztal (Berghausen) AN - OPUS4-19162 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Trubiroha, Peter T1 - Correlations in weathering results T2 - 4th European weathering symposium - Natural and artificial ageing of polymers CY - Budapest, Hungary DA - 2009-09-16 KW - Witterungsbeständigkeit KW - Korrelation KW - Künstliche Bewitterung KW - Artificial weathering PY - 2009 SN - 978-3-9810472-8-8 IS - Publication 11 SP - 251 EP - 261 PB - DWS Werbeagentur und Verlag GmbH CY - Karlsruhe AN - OPUS4-20020 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Wachtendorf, Volker A1 - Geburtig, Anja ED - Moeller, E. T1 - Entwicklung künstlicher Bewitterungstests für Lacke und Beschichtungen T2 - GfKORR-Seminar Korrelation von Labortests mit Praxisbedingungen im Automobilbereich CY - Frankfurt am Main, Deutschland DA - 0008-02-15 KW - Künstliche Bewitterung KW - Freibewitterung KW - Verkürzung KW - Beschleunigung KW - Korrelation PY - 2006 SN - 3-935406-27-4 SP - 102 EP - 111 PB - GfKORR CY - Frankfurt am Main AN - OPUS4-12065 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Trubiroha, Peter T1 - Aussagekraft von Korrelationskoeffizienten T2 - 38. Jahrestagung der GUS CY - Stutensee-Blankenloch/Karlsruhe, Deutschland DA - 2009-03-18 KW - Witterungsbeständigkeit KW - Korrelation KW - Künstliche Bewitterung PY - 2009 SN - 978-3-9810472-7-1 SP - 61 EP - 70 CY - Pfinztal (Berghausen) AN - OPUS4-19161 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Zäh, M. A1 - Schönlein, A. A1 - Reichert, T. T1 - Polypropylene life time estimation by developing dose response functions with respect to irradiation and temperature - ViPQuali project T2 - 8th International symposium on weatherability (8th ISW) CY - Tokyo, Japan DA - 2010-10-14 KW - Life time estimation KW - Weathering KW - Polypropylene KW - Spectral sensitivity KW - Temperature PY - 2010 SN - 1346-0633 VL - 22 SP - 58 EP - 63 PB - Uni Publishers Co., Ltd. AN - OPUS4-22182 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Wachtendorf, Volker A1 - Geburtig, Anja A1 - Trubiroha, Peter T1 - Principles and Limitations in the Acceleration of Artificial Weathering Tests T2 - 6th International Paint, Varnish, Ink & Auxiliary Products Industry Congress & Exhibition, 2006 Paint CY - Istanbul, Turkey DA - 2006-05-17 KW - Bewitterung KW - Verkürzung KW - Zeitraffung KW - Weathering KW - Shortening KW - Time-lapse PY - 2006 SN - 994-489125-8 SP - 48 EP - 54 PB - TMMOB CY - Istanbul AN - OPUS4-12391 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Wachtendorf, Volker A1 - Geburtig, Anja A1 - Trubiroha, Peter ED - Ziegahn, K.-F. T1 - Grundsätzliches zur Verkürzung von Bewitterungstests durch künstliche Bewitterung T2 - 35. Jahrestagung der GUS 2006 - Umwelteinflüsse erfassen, simulieren, bewerten CY - Pfinztal, Deutschland DA - 2006-03-22 PY - 2006 SN - 3-9810472-0-6 SP - 165 EP - 175 PB - DWS Werbeagentur und Verlag GmbH CY - Pfinztal AN - OPUS4-21345 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Trubiroha, Peter T1 - Reference materials for weathering tests T2 - 1st European Weathering Symposium (EWS-1) ; 23rd Colloquium of Danubian Countries on Natural and Artificial Ageing of Polymers CY - Prague, Czech Republic DA - 2003-09-25 KW - Referenzmaterialien KW - Bewitterung PY - 2003 SN - 3-9808382-3-4 SP - 1(?) EP - 11(?) PB - Gesellschaft für Umweltsimulation e.V. CY - Pfinztal AN - OPUS4-2882 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Trubiroha, Peter T1 - Determination of the spectral response of polymers T2 - 3rd Service Life Symposium CY - Sedona, AZ, USA DA - 2004-02-01 KW - Spectral sensitivity KW - Weathering KW - UV KW - Action spectra KW - Activation spectra KW - Stabilizer KW - Spektrale Empfindlichkeit KW - Bewitterung KW - Aktivierungsspektrum KW - Wirkungsspektrum KW - Stabilisator PY - 2005 SN - 0-934010-60-9 SP - 241 EP - 253 PB - Federation of Societies for Coatings Technology CY - Philadelphia AN - OPUS4-13711 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Wachtendorf, Volker A1 - Geburtig, Anja A1 - Trubiroha, Peter T1 - Grundsätzliches zur Verfahrensauswahl bei der künstlichen Bestrahlung und Bewitterung KW - Bewitterung KW - Bestrahlung KW - Fluoreszenzlampe KW - Xenonlampe PY - 2008 SN - 978-3-9810472-6-4 SP - 109 EP - 121 AN - OPUS4-17338 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Geburtig, Anja A1 - Wachtendorf, Volker ED - Zieghahn, K. T1 - Grundsätzliches zur Lebensdauervorhersage in der Bewitterung T2 - Umwelteinflüsse erfassen, simulieren, bewerten : 34. Jahrestagung der GUS 2005 CY - Pfinztal bei Karlsruhe, Deutschland DA - 2005-03-02 KW - Lebensdauer KW - Bewitterung KW - Polymere PY - 2005 SN - 3-9808382-6-9 SP - 159 EP - 168 PB - GUS (Gesellschaft für Umweltsimulation) CY - Pfinztal AN - OPUS4-7141 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Mrkwitschka, Paul A1 - Sahre, Mario A1 - Corrao, Elena A1 - Pellegrino, Francesco A1 - Alonso, Beatriz A1 - Zurutuza, Amaia A1 - Radnik, Jörg A1 - Hodoroaba, Vasile-Dan T1 - Standardized Elemental Composition Analysis of Graphene‐Related 2D Materials (GR2M) With SEM/EDS and XPS Works Reliably N2 - Reliable quantification of the chemical composition of graphene‐related 2D materials (GR2M) as powders and liquid suspensions is a challenging task. Analytical methods such as X‐ray photoelectron spectroscopy (XPS), inductively coupled plasma mass spectrometry (ICP‐MS), thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy (FTIR) are recommended by standardization bodies. The specific parameters to be measured are also defined, e.g., the oxygen‐to‐carbon (O/C) atomic ratio, the trace metal impurities, or the functional groups. In this contribution, for the first time, results of a systematic study on the capability of energy‐dispersive X‐ray spectroscopy (EDS) at a scanning electron microscope (SEM) to reliably quantify the O/C ratio and impurities remained from the synthesis of selected GR2M are reported. The robustness of SEM/EDS analysis is verified for various measurement conditions (different excitations and EDS detectors) and the validity of the results is tested by comparison to the established XPS analysis. Moreover, an ionic liquid is used as a reference material for the quantification of the light elements such as C, N, O and F. The study clearly demonstrates the reliability of the fast and widely available SEM/EDS as a standard method for the quantification of the elemental composition of GR2M and generally of light materials. KW - Graphene oxide flakes KW - Impurities KW - O/C ratio KW - SEM/EDS KW - Standard KW - XPS PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656748 DO - https://doi.org/10.1002/smll.202511283 SN - 1613-6810 SP - 1 EP - 10 PB - Wiley-VHC GmbH AN - OPUS4-65674 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Geburtig, Anja A1 - Wachtendorf, Volker A1 - Trubiroha, Peter ED - Ziegahn, K.-F. T1 - Ermittlung der Beanspruchung bei Bewitterungsversuchen - Referenzmaterialien T2 - 33. Jahrestagung der GUS 2004 - Umwelteinflüsse erfassen, simulieren, bewerten CY - Pfinztal, Deutschland DA - 2004-03-17 PY - 2004 SN - 3-9808382-4-2 SP - 165 EP - 175 PB - DWS Werbeagentur und Verlag GmbH CY - Pfinztal AN - OPUS4-21346 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Aliyah, K. A1 - Berger, A. A1 - Lazaridis, T. A1 - Appel, C. A1 - Prehal, C. A1 - Menzel, A. A1 - Guizar-Sicairos, M. A1 - Smales, Glen J. A1 - Pauw, Brian Richard A1 - Gasteiger, H. A. A1 - Gubler, L. A1 - Büchi, F. N. A1 - Eller, J. T1 - Impact of Microporous Layer Composition on the Water Content in the Membrane Electrode Assembly of Polymer Electrolyte Fuel Cells N2 - Polymer electrolyte fuel cells are paramount for future emission-free mobility. One of the vital challenges for prospering commercialization of PEFCs is water management in the cells. A microporous layer (MPL) is typically positioned between the gas Diffusion layer (GDL) and the catalyst layer (CL) to boost the cell performance and facilitate water management. In this study, three different MPLs were investigated, namely, carbon black-based MPLs with different PTFE binder contents (20 wt % PTFE as a base case and 40 wt % PTFE), as well as perforated MPLs with micron-sized pores coated on the same GDL- Substrate (Freudenberg H14). The water content in the membrane, catalyst layers (CL), and MPLs was explored using operando scanning small- and wide-angle X-ray scattering (S/WAXS). At Tcell = 80 °C, relative humidity = 100%, pabs = 3 bar, the MPL with larger pores exhibits slightly higher performance than the base case, while a considerably lower cathode CL and MPL saturation levels were observed for the MPL. In contrast, the MPL with higher amounts of PTFE binder shows lower performance than the base case, with considerably higher cathode CL and MPL saturation levels. 3D representations of how the pores could be filled in the cathode CLs were obtained from operando SAXS profiles using representative structure modeling for the different materials and operating conditions. KW - Polymer electrolyte fuel cell KW - Catalyst layer saturation KW - Microporous layer saturation KW - Membrane hydration KW - Small and wide-angle scattering KW - MOUSE KW - SAXS KW - X-ray scattering KW - Energy storage materials PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656691 DO - https://doi.org/10.1021/acsami.5c22540 SN - 1944-8244 SP - 1 EP - 17 PB - American Chemical Society (ACS) AN - OPUS4-65669 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sanchez-Olivares, Guadalupe A1 - Brehme, Sven A1 - Calderas, F. A1 - Schartel, Bernhard T1 - Flame Retardant Polyolefins Using Fibers From Leather Waste: Adjusting Extrusion Variables to Balance the Property Profile N2 - The extrusion processing variables represent a key to the optimal use of additives and thus the development of flame-retardant polymer composites. Adjusting the property profile, for example, finding a balance between flame retardancy and mechanical properties is the main challenge. In this work, the effect of blending temperature and rotational speed on physico-mechanical properties and fire behavior of polyolefin composites was investigated. High-density polyethylene or polypropylene was used as polymer matrices; the polymers were compounded by the extrusion process using industrial-waste leather fibers as flame retardant adjuvant and commercial flame-retardant additives. A detailed rheological analysis highlighted different viscoelastic behavior, that is, a predominant elastic or viscous one. The effect of the extrusion processing variables was also investigated on the morphology, mechanical properties, thermal decomposition, fire behavior under forced flaming combustion and flammability. Important improvements were revealed with respect to using only high loading of flame retardants. For high-density polyethylene-based composites, impact resistance and elongation at break increased 8 and 7.5 times, respectively. The total heat evolved (87MJ/m2), effective heat of combustion (31.6MJ/kg), flame retardancy (UL 94 rating) results were comparable with the reference sample. Meanwhile for polypropylene composites, the impact resistance increased 2.2 times and the flame retardancy was improved from no rating in the UL 94 vertical test to V-0 rating. Tailored processing was highlighted as an autonomous and powerful approach to achieve balanced and demanding properties. KW - Biomaterials KW - Composites KW - Extrusion KW - Flame retardance KW - Leather waste KW - Polyolefins PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656732 DO - https://doi.org/10.1002/vnl.70048 SN - 1548-0585 SN - 1083-5601 VL - 32 IS - 2 SP - 410 EP - 430 PB - Wiley Periodicals LLC. AN - OPUS4-65673 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Charlesworth, M. A1 - Lampronti, G. A1 - Belenguer, Ana M. A1 - Day, S. A1 - Saunders, L. A1 - Connolly, E. A1 - Midgley, P. A1 - Michalchuk, Adam A. L. T1 - Influence of Liquid on Crystallite Size Evolution During Ball Milling N2 - Liquid assisted grinding (LAG) is a commonly used mechanochemical procedure, especially for polymorphic conversions. However, it is not understood what effect liquid additives actually play in driving mechanochemical polymorphic conversions, precluding our ability to control solid form transformations under mechanochemical conditions. We here present a time-resolved in situ (TRIS) synchrotron powder Xray diffraction (PXRD) monitoring strategy that can track, with few nm resolution, the evolution of crystalline size under liquid assisted ball milling conditions. We apply this method to investigate the influence of liquid additives on the polymorphic conversion of the 1:1 co-crystal of theophylline and benzamide, with particular focus on the role that crystallite size plays in driving ball milling induced polymorphic transformations. We find that the crystallite sizes achieved by ball milling are highly sensitive to the amount of liquid added to the reaction mixture. Liquid additives generally lead to larger crystallite sizes as compared with neat grinding protocol, with our findings indicating that crystallite size reduction is not the main factor that causes polymorph conversion under liquid assisted grinding conditions. The data presented clearly indicates the presence of an induction period before phase transformation begins with a minimum value in the crystallite size of the starting polymorph indicating the end of that induction period. KW - Ball milling KW - In situ diffraction KW - Phase transformation KW - Liquid assisted grinding KW - Crystallite size PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656783 DO - https://doi.org/10.1021/acs.cgd.5c01662 SN - 1528-7483 SP - 1 EP - 7 PB - American Chemical Society (ACS) AN - OPUS4-65678 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gründer, Klaus-Peter A1 - Geburtig, Anja T1 - Dreidimensionale Dehnungsfeldmessungen an parallelepipedischen Zugproben N2 - Es wird die Anwendung des Objektrasterverfahrens zur Untersuchung des elastischen und inelastischen, anisotropen und inhomogenen Verformungsverhaltens parallelepipedischer, metallischer Einkristall-Zugproben im Ergebnis unterbrochener Belastungsstufen von ca. 0,01%, 0,05%, 0,10% und 0,20% Restdehnung beschrieben. Diese Vorgehensweise ermöglicht die gleichzeitige Bestimmung aktivierter Gleitsysteme mit einem optischen Nano-Topografiesystem nach der Weißlichtinterferenzmethode. Aus den Verformungsdaten im elastischen Bereich können flächen- und richtungsabhängige Materialkennwerte ermittelt werden. A special grating method has been applied for three-dimensional investigation of elastic and inelastic, anisotropic and inhomogeneous deformation of parallelepipedal metallic single crystal specimen by interrupted tensile tests in steps of 0,01%, 0,05%, 0,10% and 0,20% residual strain. This procedure gives the ability to determine activated slip systems by white light interferometric nanoscale topometry. Elastic anisotropic material parameters of cubic crystals can be calculated from experimental data. KW - Optical 3D-deformation measurement KW - Grating method KW - Mono-crystalline metallic alloys KW - Elastic material parameters PY - 2002 DO - https://doi.org/10.1524/teme.2002.69.10.418 SN - 0340-837X SN - 0178-2312 SN - 0171-8096 VL - 69 IS - 10 SP - 418 EP - 420 PB - Oldenbourg CY - München AN - OPUS4-1575 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Gründer, Klaus-Peter A1 - Geburtig, Anja T1 - Optical methods in single crystal deformation analysis at high temperature T2 - International Symposium on Photonics in Measurement CY - Aachen, Germany DA - 2002-06-11 PY - 2002 SN - 3-18-091694-X SN - 0083-5560 N1 - Serientitel: VDI-Berichte – Series title: VDI-Berichte IS - 1694 SP - 137 EP - 142 PB - VDI-Verl. CY - Düsseldorf AN - OPUS4-1447 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -