TY - JOUR A1 - Linke, S. A1 - Kühn, Julius A1 - Nörthemann, K. A1 - Unger, Wolfgang A1 - Moritz, W. T1 - Sensor high throughput screening using photocurrent measurements in silicon N2 - A new high throughput screening method to characterise alloys used as gate metal of Metal/solid Electrolyte/Insulator/Semiconductor (MEIS) gas-sensors was developed. Samples with continuous gradients in alloy concentration for the system Pd1-x-yNiyCoy were analysed regarding H2 sensitivity. First results showed reduced poisoning effects of H2S for Ni concentrations between 4-11 at-% in Pd. T2 - Eurosensors XXVI CY - Kraków, Poland DA - 09.09.2012 KW - LAPS KW - Ternary alloy KW - MEIS sensor KW - H2 sensor KW - High throughput screening PY - 2012 DO - https://doi.org/10.1016/j.proeng.2012.09.366 SN - 1877-7058 VL - 47 SP - 1195 EP - 1198 PB - Elsevier CY - Amsterdam [u.a.] AN - OPUS4-27926 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kromm, Arne T1 - Exploring the interaction of phase transformation and residual stress during welding by synchrotron diffraction N2 - Controlling the level of mostly detrimental residual stresses already during the welding process would be highly attractive as time and cost consuming post processing may be prevented. Therefore, in this study, the approach using suitable alloy concepts with reduced phase transformation temperatures has been evaluated concerning the interactions between transformation temperature, transformation kinetics and resulting residual stresses. Ideal tools for observing these phenomena in-situ are diffraction techniques. For that purpose, a special setup was developed allowing for localized observation of phase transformation kinetics during a real welding process by energy dispersive synchrotron diffraction (EDXRD). In the present work, this setup was successfully applied for the first time in order to characterize a selection of alloys especially designed for residual stress control. The results demonstrate that in-process observation is highly suitable for characterizing and discussing phase transformation sensitive phenomena like residual stress formation. Furthermore, it was proven that residual stresses can be effectively controlled by means of an adjusted alloy design. KW - Austenite KW - Diffraction KW - Martensite KW - Residual stresses KW - Transformation KW - X-rays PY - 2012 SN - 0043-2288 SN - 1878-6669 VL - 56 IS - 09/10 SP - 2 EP - 11 PB - Springer CY - Oxford AN - OPUS4-27482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krause, Christina A1 - Yin, Huajie A1 - Cerclier, C. A1 - Morineau, D. A1 - Wurm, Andreas A1 - Schick, C. A1 - Emmerling, Franziska A1 - Schönhals, Andreas T1 - Molecular dynamics of a discotic liquid crystal investigated by a combination of dielectric relaxation and specific heat spectroscopy N2 - The molecular dynamics of the discotic liquid crystal pyrene-1,3,6,8-tetracarboxylic tetra(2-ethylhexyl)ester is studied by dielectric relaxation and specific heat spectroscopy. Dielectric spectroscopy shows 3 processes: a β-relaxation at low temperatures and an α-relaxation in the temperature range of the mesophases followed by conductivity. The dielectric α-relaxation is assigned to a restricted glassy dynamics in the plastic crystal as well as in the liquid crystalline phase. The obtained different Vogel–Fulcher–Tammann laws (different Vogel temperatures and fragility) are related to the different restrictions of the dipolar fluctuations in the corresponding phases. By means of specific heat spectroscopy glassy dynamics is also detected in the plastic crystalline phase but with quite a different temperature dependence of the relaxation times. This is discussed considering the different probes involved and how they are influenced by the structure. In the frame of the fluctuation approach a correlation length of glassy dynamics is calculated to 0.78 nm which corresponds to the core–core distance estimated by X-ray scattering. PY - 2012 DO - https://doi.org/10.1039/c2sm25610j SN - 1744-683X VL - 8 IS - 43 SP - 11115 EP - 11122 PB - RSC Publ. CY - Cambridge AN - OPUS4-26826 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kreutzbruck, Marc A1 - Neubauer, Andreas A1 - Pelkner, Matthias A1 - Reimund, Verena T1 - Adapted GMR array used in magnetic flux leakage inspection N2 - GMR sensors are increasingly used for magnetic surface inspection due to their high sensitivity and high spatial resolution. In case of simple planar or cylindrical shaped components, the GMR-based inspection procedure can be automated easily. In order to reduce the inspection time we present a GMR-based NDT-system consisting of a yoke and a coil as a local magnetization unit. This way the global magnetization step and, if necessary, the corresponding demagnetization cycle can be avoided reducing the number of working steps. Using a local probe we measured plates, bearings, and rails, each of which containing real fatigue cracks and reference artificial cracks of different depths and orientations. Cracks with a depth of 40 ìm could be resolved with a signalto-noise ratio of about 20. A reduction of the measuring time can be obtained using a sensor array. We present an optimized sensor array for nondestructive testing application, where gradiometric arranged GMR layers were fabricated on a board with up to 48 GMR sensors. Each sensor detects the vertical field gradient. In our example the baseline was chosen to be 250 ìm which efficiently suppress external Background fields without losing sensitivity for the detection of surface breaking defects. T2 - 18th WCNDT - World conference on nondestructive testing CY - Durban, South Africa DA - 16.04.2012 KW - Flux leakage testing KW - GMR-Sensors KW - Sensor arrays PY - 2012 SN - 978-0-620-52872-6 SP - 1 EP - 8 (Paper 498) AN - OPUS4-26351 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kreutzbruck, Marc A1 - Prager, Jens A1 - Boehm, Rainer A1 - Kitze, Jessica A1 - Brekow, Gerhard T1 - Progress in acoustical defect sizing NDT methods for the inspection of power-plant components N2 - The demand of improved NDT methods with proper visualization and sizing capabilities is a persistent trend in maintenance and manufacturing quality inspection. Especially when dealing with high quality standards in conjunction with safety-critical components in the sector of energy and transportation quantitative NDT techniques are vital to provide reliable quality control systems and a corresponding deeper insight into the component structure for a further fracture-mechanical estimation. The paper thus focuses the progress of the defect sizing capabilities of modern Ultrasonic Testing (UT). In Ultrasonic Testing the SAFT-algorithm (Synthetic Aperture Focusing Technique) currently experiences a renaissance. The method is based on combining the data of different transducer positions with their corresponding varied propagating time and it is currently applied in several industrial applications. SAFT enhances the SNR and the spatial resolution and is thus a valuable tool when it comes to improved defect detection and sizing. A tomographic-like data mapping is illustrated on several examples, where adapted phased array systems were used for the inspection of turbine components and also for a cladded mock-up of a nuclear reactor pressure vessel. In a statistical investigation we also performed a comparison with other defect sizing methods like TOFD (Time of flight diffraction). T2 - 18th WCNDT - World conference on nondestructive testing CY - Durban, South Africa DA - 16.04.2012 KW - SAFT KW - TOFD KW - Cracks KW - Phased Array PY - 2012 SN - 978-0-620-52872-6 SP - 1 EP - 8 (Paper 497) AN - OPUS4-26350 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Pütz, E. A1 - Smales, Glen Jacob A1 - Jegel, O. A1 - Emmerling, Franziska A1 - Tremel, W. T1 - Tuning ceria catalysts in aqueous media at the nanoscale: how do surface charge and surface defects determine peroxidase- and haloperoxidase-like reactivity N2 - Designing the shape and size of catalyst particles, and their interfacial charge, at the nanometer scale can radically change their performance. We demonstrate this with ceria nanoparticles. In aqueous media, nanoceria is a functional mimic of haloperoxidases, a group of enzymes that oxidize organic substrates, or of peroxidases that can degrade reactive oxygen species (ROS) such as H2O2 by oxidizing an organic substrate. We show that the chemical activity of CeO2−x nanoparticles in haloperoxidase- and peroxidaselike reactions scales with their active surface area, their surface charge, given by the ζ-potential, and their surface defects (via the Ce3+/Ce4+ ratio). Haloperoxidase-like reactions are controlled through the ζ-potential as they involve the adsorption of charged halide anions to the CeO2 surface, whereas peroxidase-like reactions without charged substrates are controlled through the specific surface area SBET. Mesoporous CeO2−x particles, with large surface areas, were prepared via template-free hydrothermal reactions and characterized by small-angle X-ray scattering. Surface area, ζ-potential and the Ce3+/Ce4+ ratio are controlled in a simple and predictable manner by the synthesis time of the hydrothermal reaction as demonstrated by X-ray photoelectron spectroscopy, sorption and ζ-potential measurements. The surface area increased with synthesis time, whilst the Ce3+/Ce4+ ratio scales inversely with decreasing ζ-potential. In this way the catalytic activity of mesoporous CeO2−x particles could be tailored selectively for haloperoxidase- and peroxidase-like reactions. The ease of tuning the surface properties of mesoporous CeO2x particles by varying the synthesis time makes the synthesis a powerful general tool for the preparation of nanocatalysts according to individual needs. KW - SAXS KW - Ceria KW - Zeta potential PY - 2022 DO - https://doi.org/10.1039/D2NR03172H SP - 1 EP - 12 PB - Royal Society of Chemistry AN - OPUS4-55649 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Paris, O. A1 - Li, C. A1 - Siegel, S. A1 - Weseloh, G. A1 - Emmerling, Franziska A1 - Riesemeier, Heinrich A1 - Erko, A. A1 - Fratzl, P. T1 - A new experimental station for simultaneous X-ray microbeam scanning for small- and wide-angle scattering and fluorescence at BESSY II N2 - A new instrument for simultaneous microbeam small- and wide-angle X-ray scattering and X-ray fluorescence (SAXS/WAXS/XRF) is presented. The instrument is installed at the microfocus beamline at BESSY II and provides a beam of 10 µm size with a flux of about 109 photons s-1. A SAXS resolution up to 500 Å d-spacing and a range of scattering vectors of almost three orders of magnitude are reached by using a large-area high-resolution CCD-based detector for simultaneous SAXS/WAXS. The instrument is particularly suited for scanning SAXS/WAXS/XRF experiments on hierarchically structured biological tissues. The necessary infrastructure, such as a cryo-stream facility and an on-site preparation laboratory for biological specimens, are available. KW - Scanning SAXS KW - Scanning WAXS KW - Microbeam KW - Synchrotron radiation PY - 2007 SN - 0021-8898 SN - 1600-5767 VL - 40 IS - Supplement SP - s466 EP - s470 PB - Blackwell CY - Oxford AN - OPUS4-15049 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kraus, Werner A1 - Emmerling, Franziska A1 - Noll, B. A1 - Noll, S. A1 - Pietzsch, H.-J. T1 - (4-Methoxybenzenethiolato-kS)oxido[2,2'-(propylimino)bis-(ethanethiolato)-k3S,N,S']rhenium(V) N2 - The central Re atom of the mononuclear title complex, [Re(C8H18NS2)(C6H4OS)O], is five-coordinate (ReNOS3) with a square-pyramidal geometry comprising a tridentate 2,2'-(propylimino)diethanethiolate ligand, a 4-methoxybenzenethiolate ligand and a doubly-bonded O atom. PY - 2007 DO - https://doi.org/10.1107/S1600536807056814 SN - 1600-5368 VL - 63 IS - 12 SP - m3018 PB - Munksgaard CY - Copenhagen AN - OPUS4-16196 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Carvalho, José Joao A1 - Emmerling, Franziska A1 - Schneider, Rudolf T1 - 7-(5-Carboxypentyl)-1,3-dimethylxanthine monohydrate N2 - The title compound [systematic name: 6-(1,3-dimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purin-7-yl)hexanoic acid monohydrate, CAS 61444-23-3], C13H18N4O4·H2O, was synthesized and crystallized from ethyl acetate. Hydrogen bonds between xanthine and water molecules contribute to the formation of layers parallel to (10). KW - Kristallstruktur KW - Koffein KW - Antikörperentwicklung KW - Biokonjugate PY - 2007 DO - https://doi.org/10.1107/S1600536807037257 SN - 1600-5368 VL - 63 IS - 9 SP - o3718 PB - Munksgaard CY - Copenhagen AN - OPUS4-15731 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emmerling, Franziska A1 - Kraus, Werner A1 - Noll, B. A1 - Noll, S. A1 - Pietzsch, H.-J. T1 - Two mononuclear Tc complexes: [2,2'-(3-phenylpropylimino)- and [2,2'-(propylimino)bis(ethanethiolato)](4-methoxybenzenethiolato)-oxidotechnate(V) PY - 2007 DO - https://doi.org/10.1107/S0108270107052870 SN - 0108-2701 SN - 1600-5759 VL - 63 IS - 12 SP - m579 EP - m582 PB - Blackwell Publ. CY - Oxford AN - OPUS4-16283 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Stephan, H. A1 - Kubeil, M. A1 - Emmerling, Franziska A1 - Müller, C.E. T1 - Polyoxometalates as versatile enzyme inhibitors N2 - Polyoxometalates (POMs) are inorganic cluster compounds that have been shown to possess a number of pharmacological properties, including antidiabetic, antibacterial, antiprotozoal, antiviral and anticancer activities. Their molecular mechanism of action is largely unknown. However, several studies indicate that many of their activities may be due to the inhibition of enzymes, in particular, of those enzymes that are accessible from the extracellular space and do not require the penetration of cell membranes. In this review, we describe the recent progress in the preparation and optimization of POMs, and an evaluation of their use as inhibitors of different families of enzymes. The next important steps in this area of research will be to gain a better understanding of the interactions of POMs with enzymes on a structural level through an X-ray crystallographic study of enzyme–POM complexes and the analysis of structure–activity relationships. Furthermore, POMs with increased stability and in vivo half-lives have to be prepared. Surface modification may allow the targeting of POM drugs at their sites of action. KW - Cluster compounds KW - Poly­oxometalates KW - Metalloprotein mimics KW - Enzymes KW - Inhibitors KW - Bioinorganic chemistry PY - 2013 DO - https://doi.org/10.1002/ejic.201201224 SN - 1434-1948 SN - 1099-0682 VL - 2013 IS - 10-11 SP - 1585 EP - 1594 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-28076 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grunert, B. A1 - Saatz, Jessica A1 - Hoffmann, Katrin A1 - Appler, F. A1 - Lubjuhn, Dominik A1 - Jakubowski, Norbert A1 - Resch-Genger, Ute A1 - Emmerling, Franziska A1 - Briel, A. T1 - Multifunctional rare-earth element nanocrystals for cell labeling and multimodal imaging N2 - In this work, we describe a simple solvothermal route for the synthesis of Eu3+-doped gadolinium orthovanadate nanocrystals (Eu:GdVO4−PAA) functionalized with poly(acrylic)acid (PAA), that are applicable as cell labeling probes for multimodal cellular imaging. The Eu3+ doping of the vanadate matrix provides optical functionality, due to red photoluminescence after illumination with UV light. The Gd3+ ions of the nanocrystals reduce the T1 relaxation time of surrounding water protons, allowing these nanocrystals to act as a positive MRI contrast agent with a r1 relaxivity of 1.97 mM−1 s−1. Low background levels of Eu3+, Gd3+, and V5+ in biological systems make them an excellent label for elemental microscopy by Laser Ablation (LA)-ICP-MS. Synthesis resulted in polycrystalline nanocrystals with a hydrodynamic diameter of 55 nm and a crystal size of 36.7 nm, which were further characterized by X-ray diffraction (XRD), photoluminescence spectroscopy (PL) and transmission electron microscopy (TEM). The multifunctional nanocrystals were subsequently used for intracellular labeling of both human adipose-derived stem cells (MSCs) and A549 (adenocarcinomic human alveolar basal epithelial) cells. KW - Bioimaging KW - Nanoparticle KW - Multimodal KW - Lanthanide PY - 2018 DO - https://doi.org/10.1021/acsbiomaterials.8b00495 SN - 2373-9878 VL - 4 IS - 10 SP - 3578 EP - 3587 PB - ACS Publications CY - Washington, USA AN - OPUS4-46244 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wuithschick, M. A1 - Paul, B. A1 - Bienert, Ralf A1 - Sarfraz, A. A1 - Vainio, U. A1 - Sztucki, M. A1 - Kraehnert, R. A1 - Strasser, P. A1 - Rademann, K. A1 - Emmerling, Franziska A1 - Polte, J. T1 - Size-controlled synthesis of colloidal silver nanoparticles based on mechanistic understanding N2 - Metal nanoparticles have attracted much attention due to their unique properties. Size control provides an effective key to an accurate adjustment of colloidal properties. The common approach to size control is testing different sets of parameters via trial and error. The actual particle growth mechanisms, and in particular the influences of synthesis parameters on the growth process, remain a black box. As a result, precise size control is rarely achieved for most metal nanoparticles. This contribution presents an approach to size control that is based on mechanistic knowledge. It is exemplified for a common silver nanoparticle synthesis, namely, the reduction of AgClO4 with NaBH4. Conducting this approach allowed a well-directed modification of this synthesis that enables, for the first time, the size-controlled production of silver nanoparticles 4–8 nm in radius without addition of any stabilization agent. KW - Silver nanoparticles KW - Growth mechanism KW - SAXS KW - Size control KW - Sodium borohydride PY - 2013 DO - https://doi.org/10.1021/cm401851g SN - 0897-4756 SN - 1520-5002 VL - 25 IS - 23 SP - 4679 EP - 4689 PB - American Chemical Society CY - Washington, DC AN - OPUS4-30194 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schulz, K. A1 - Schmack, R. A1 - Klemm, H. W. A1 - Kabelitz, Anke A1 - Schmidt, T. A1 - Emmerling, Franziska A1 - Kraehnert, R. T1 - Mechanism and kinetics of hematite crystallization in air: Linking bulk and surface models via mesoporous films with defined nanostructure N2 - Iron can form numerous oxides, hydroxides, and oxide−hydroxides. Despite their relevance, many of the transformation processes between these phases are still poorly understood. In particular the crystallization of quasi-amorphous hydroxides and oxide−hydroxides is difficult to assess, since typical diffraction and scattering methods provide only sampleaveraged information about the crystallized phases. We report a new approach for the investigation of the crystallization of oxide−hydroxides. The approach relies on model-type films that comprise a defined homogeneous nanostructure. The nanostructure allows quantitative linking of Information obtained by bulk-averaging diffraction techniques (XRD, SAXS) with locally resolved information, i.e., Domain sizes (SEM, TEM, LEEM) and phase composition (SAED). Using time-resolved imaging and diffraction we deduce mechanism and kinetics for the crystallization of ferrihydrite into hematite. Hematite forms via nucleation of hematite domains and subsequent Domain growth that terminates only upon complete transformation. A Johnson−Mehl−Avrami−Kolmogorov model describes the kinetics over a wide temperature range. The derived understanding enables the first synthesis of ferrihydrite films with ordered mesoporosity and quantitative control over the films’ hematite and ferrihydrite content. KW - Iron oxide KW - Crystallization KW - Mesoporous films KW - Nanostructure PY - 2017 DO - https://doi.org/10.1021/acs.chemmater.6b05185 SN - 0897-4756 SN - 1520-5002 VL - 29 IS - 4 SP - 1724 EP - 1734 AN - OPUS4-39690 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Rautenberg, Max A1 - Bhattacharya, Biswajit A1 - Akhmetova, Irinia A1 - Emmerling, Franziska T1 - Mechanochemical and solution syntheses of two novel cocrystals of orcinol with two N,N0-Dipyridines: Structural diversity with varying ligand flexibility N2 - We studied the influence of coformers flexibility on the supramolecular assembly of 5-substituted resorcinol. Two cocrystals of orcinol (ORL) with two dipyridine molecules, i.e. 1,2-di(4-pyridyl)ethane (ORLeBPE) and 1,2-di(4-pyridyl)ethylene (ORLeBPY), were prepared by mechanochemical synthesis and slow evaporation of solvent. The new crystalline solids were thoroughly characterized by single crystal Xray diffraction (SCXRD), powder X-ray diffraction analysis (PXRD), Fourier-transform infrared spectroscopy (FT-IR), differential thermal analysis (DTA), and thermogravimetric analysis (TGA). Structural determination reveals that in both cocrystals, the phenolepyridine, i.e. OeH/N(py) heterosynthon takes the main role in the formation of cocrystals. In ORLeBPE, the components form infinite 1D zig-zag chains, which are extended to 2D layer structure by inter-chain CeH/O interactions between BPE hydrogen atoms and hydroxyl oxygen atoms of ORL. In ORLeBPY, the components form a 0D fourcomponent complex. Formation of the discrete assemblies is attributed to the comparative rigid nature of BPY, which restricts the formation of an extended network. KW - Cocrystal KW - Single crystal KW - X-ray diffraction KW - Mechanochemistry PY - 2020 DO - https://doi.org/10.1016/j.molstruc.2020.128303 SN - 0022-2860 VL - 1217 SP - 128303 PB - Elsevier B.V. AN - OPUS4-51023 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Nguyen, Thi Yen A1 - Roessler, Ernst A1 - Rademann, Klaus A1 - Emmerling, Franziska T1 - Control of organic polymorph formation: crystallization pathways in acoustically levitated droplets N2 - Theoretical and experimental studies indicate that crystal nucleation can take more complex pathways than expected on the ground of the classical nucleation theory. Among these pathways are the formation of pre-nucleation clusters and amorphous precursor phases. A direct in situ observation of the different pathways of nucleation from solution is challenging since the paths can be influenced by heterogeneous nucleation sites, such as container walls. Here, we provide insights into the crystallization process using the in situ combination of an acoustic levitator, Raman spectroscopy, and X-ray scattering. The contactless sample holder enables the observation of homogeneous crystallization processes and the detection of intermediates and final crystalline forms. We provide evidence for the existence of multiple pathways of nucleation based on the investigation of the crystallization of organic molecules from different solvents. Starting from a diluted solution, a supersaturation is reached during the experiment due to the evaporation of the solvent. The highly supersaturated solution reveals different pathways of crystallization. Depending on the degree of supersaturation either the thermodynamically stable or the metastable crystal form is observed. KW - Crystallization KW - In situ XRD KW - Polymorphism KW - Polyamorphism KW - Raman spectroscopy PY - 2017 DO - https://doi.org/10.1515/zkri-2016-1964 SN - 2194-4946 SN - 2196-7105 VL - 232 IS - 1-3 SP - 15 EP - 24 PB - De Gruyter CY - Berlin AN - OPUS4-39708 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Linberg, Kevin A1 - Ali, Naveed Zafar A1 - Etter, M. A1 - Michalchuk, Adam A1 - Rademann, K. A1 - Emmerling, Franziska T1 - A Comparative Study of the Ionic Cocrystals NaX (α-d-Glucose)2 (X = Cl, Br, I) N2 - The mechanochemical formation of the ionic cocrystals of glucose (Glc) and sodium salts Glc2NaCl·H2O (1) and Glc2NaX (X = Br (2), I (3)) is presented. Products are formed by co-milling Glc with three sodium salts (NaCl, NaBr, NaI). The ionic cocrystals were obtained under both neat grinding and liquid-assisted grinding conditions, the later found to accelerate the reaction kinetics. The crystal structures of the ionic cocrystals (2) and (3) were solved from powder X-ray diffraction data. The structure solution contrasts with the structure of Glc2NaCl·H2O (1) where the electron density at three halide crystallographic sites is modeled as of being the intermediate between water molecule and a chloride ion. The reaction pathways of the three ionic cocrystals were investigated in real time using our tandem approach comprising a combination of in situ synchrotron powder X-ray diffraction and Raman spectroscopy. The results indicate the rapid formation of each cocrystal directly from their respective starting materials without any intermediate moiety formation. The products were further characterized by DTA-TG and elemental analysis. KW - In situ KW - Co-crystal KW - Mechanochemistry KW - Glucose PY - 2019 DO - https://doi.org/10.1021/acs.cgd.8b01929 VL - 19 IS - 8 SP - 4293 EP - 4299 PB - ACS Publications AN - OPUS4-48781 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Greiser, Sebastian A1 - Benemann, Sigrid A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Knowing When To Stop-Trapping Metastable Polymorphs in Mechanochemical Reactions N2 - The cocrystal formation of pyrazinamide (PZA) with malonic acid (MA) was studied in situ. The mechanochemical reaction proceeds via conversion of a crystalline intermediate (PZA:MA II) into the thermodynamically more stable form (PZA:MA I) upon further grinding. The information derived from in situ powder X-ray diffraction (PXRD) enabled the isolation of this new metastable polymorph. On the basis of the PXRD data, the crystal structure of the 1:1 cocrystal PZA:MA II was solved. The polymorphs were further characterized and compared by Raman spectroscopy, solid-state NMR spectroscopy, differential thermal analysis/thermogravimetric analysis, and scanning electron microscopy. Our study demonstrates how monitoring mechanochemical reactions by in situ PXRD can direct the discovery and isolation of even short-lived intermediates not yet accessed by conventional methods. KW - Mechanochemistry KW - Polymorphs KW - Metastable KW - In situ PXRD KW - Cocrystal KW - Pyrazinamide PY - 2017 DO - https://doi.org/10.1021/acs.cgd.6b01572 SN - 1528-7483 SN - 1528-7505 VL - 17 IS - 3 SP - 1190 EP - 1196 AN - OPUS4-39420 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Wilke, Manuel A1 - Fischer, Franziska A1 - Röllig, Mathias A1 - Maierhofer, Christiane A1 - Emmerling, Franziska T1 - Warming up for mechanosynthesis – temperature development in ball mills during synthesis N2 - We present a first direct measurement of the temperature during milling combined with in situ Raman spectroscopy monitoring. The data reveal a low temperature increase due to the mechanical impact and clear temperature increases as a consequence of the reaction heat. Based on the data, temperature rises as postulated in the magma plasma and hot spot theory can be excluded for soft matter milling syntheses. KW - Thermography KW - Milling KW - Mechanochemistry KW - Soft matter PY - 2017 DO - https://doi.org/10.1039/c6cc08950j SN - 1364-548X SN - 1359-7345 SN - 0009-241X VL - 53 IS - 10 SP - 1664 EP - 1667 AN - OPUS4-39251 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Dietzsch, Michael A1 - Andrusenko, Iryna A1 - Branscheid, Robert A1 - Emmerling, Franziska A1 - Kolb, Ute A1 - Tremel, Wolfgang T1 - Snapshots of calcium carbonate Formation - a step by step analysis N2 - Recent advances in our understanding of CaCO, nucleation from solution have provoked new and challenging questions. We have studied CaC03 formation using precipitation by carbonate ester hydrolysis which ensures precipitation from a strictly homogeneous solution state and allows “titrating” carbonate to a solution with a given Ca2+ concentration on a timescale suited for kinetic studies. Nucleation and crystallization were traced by combining dynamic light Scattering (DLS) and transmission electron microscopy (TEM). DLS served as in situ technique to identify the nucleation time, to monitor particle size evolution, to discriminate different precipitation mechanisms and to validate reproducibility. TEM snapshots taken during different stages of the precipitation process identified different phases and morphologies. At a high level of supersaturation homogeneous nucleation in solution led to the formation of amorphous CaC03 particles (diameter=30 nm), which transformed via vaterite to calcite. Nucleation occurred uniformly in solution which appears to be unique for the CaC03 System. In the presence of Na-polymethacrylate (Na-PMA), heterogeneous nucleation was suppressed and Ca-polymer aggregates were formed in the prenucleation stage. Beyond a critical threshold supersaturation CaC03 particles formed in solution outside of these aggregates. The nucleation process resembled that without additive, indicating that Na-PMA exerts only a minor effect on the CaC03 nucleation. In the postnucleation stage, the polymer led to the formation of extended liquid-like networks, which served as a precursor phase for solid ACC particles that formed alongside the network. KW - biomineralization KW - calcium carbonate KW - nucleation KW - polymer additives PY - 2017 DO - https://doi.org/10.1515/zkri-2016-1973 SN - 2194-4946 SN - 2196-7105 VL - 232 IS - 1-3 SP - 255 EP - 265 PB - De Gruyter CY - Berlin AN - OPUS4-39863 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Opitz, P. A1 - Besch, L. A1 - Panthöfer, M. A1 - Kabelitz, Anke A1 - Unger, R. A1 - Emmerling, Franziska A1 - Mondeshki, M. A1 - Tremel, W. T1 - Insights into the In Vitro Formation of Apatite from Mg‐Stabilized Amorphous Calcium Carbonate N2 - A protein‐free formation of bone‐like apatite from amorphous precursors through ball‐milling is reported. Mg2+ ions are crucial to achieve full amorphization of CaCO3. Mg2+ incorporation generates defects which strongly retard a recrystallization of ball‐milled Mg‐doped amorphous calcium carbonate (BM‐aMCC), which promotes the growth of osteoblastic and endothelial cells in simulated body fluid and has no effect on endothelial cell gene expression. Ex situ snapshots of the processes revealed the reaction mechanisms. For low Mg contents (<30%) a two phase system consisting of Mg‐doped amorphous calcium carbonate (ACC) and calcite “impurities” was formed. For high (>40%) Mg2+ contents, BM‐aMCC follows a different crystallization path via magnesian calcite and monohydrocalcite to aragonite. While pure ACC crystallizes rapidly to calcite in aqueous media, Mg‐doped ACC forms in the presence of phosphate ions bone‐like hydroxycarbonate apatite (dahllite), a carbonate apatite with carbonate substitution in both type A (OH−) and type B (PO43−) sites, which grows on calcite “impurities” via heterogeneous nucleation. This process produces an endotoxin‐free material and makes BM‐aMCC an excellent “ion storage buffer” that promotes cell growth by stimulating cell viability and metabolism with promising applications in the treatment of bone defects and bone degenerative diseases. KW - Total Scattering KW - XRD KW - Mechanochemistry PY - 2020 DO - https://doi.org/10.1002/adfm.202007830 VL - 31 IS - 3 SP - 7830 PB - Wiley VHC-Verlag AN - OPUS4-51761 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hoffmann, Katrin A1 - Dietzel, B. A1 - Schulz, B. A1 - Reck, Günter A1 - Hoffmann, Angelika A1 - Orgzall, I. A1 - Resch-Genger, Ute A1 - Emmerling, Franziska T1 - Combined structural and fluorescence studies of methyl-substituted 2,5-diphenyl-1,3,4-oxadiazoles - relation between electronic properties and packing motifs N2 - Prerequisite for the rational design of functional organic materials with tailor-made electronic properties is the knowledge of the structure–property relationship for the specific class of molecules under consideration. This encouraged us to systematically study the influence of the molecular structure and substitution pattern of aromatically substituted 1,3,4-oxadiazoles on the electronic properties and packing motifs of these molecules and on the interplay of these factors. For this purpose, seven diphenyl-oxadiazoles equipped with methyl substituents in the ortho- and meta-position(s) were synthesized and characterized. Absorption and fluorescence spectra in solution served here as tools to monitor substitution-induced changes in the electronic properties of the individual molecules whereas X-ray and optical measurements in the solid state provided information on the interplay of electronic and packing effects. In solution, the spectral position of the absorption maximum, the size of Stokes shift, and the fluorescence quantum yield are considerably affected by ortho-substitution in three or four ortho-positions. This results in blue shifted absorption bands, increased Stokes shifts, and reduced fluorescence quantum yields whereas the spectral position and vibrational structure of the emission bands remain more or less unaffected. In the crystalline state, however, the spectral position and shape of the emission bands display a strong dependence on the molecular structure and/or packing motifs that seem to control the amount of dye–dye-interactions. These observations reveal the limited value of commonly reported absorption and fluorescence measurements in solution for a straightforward comparison of spectroscopic results with single X-ray crystallography. This underlines the importance of solid state spectroscopic studies for a better understanding of the interplay of electronic effects and molecular order. KW - Diphenyl-oxadiazoles KW - X-ray structure KW - Packing motif KW - Optical properties KW - Fluorescence quantum yield PY - 2011 DO - https://doi.org/10.1016/j.molstruc.2010.11.071 SN - 0022-2860 SN - 1872-8014 SN - 0377-046X VL - 988 IS - 1-3 SP - 35 EP - 46 PB - Elsevier CY - Amsterdam AN - OPUS4-23253 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Müller, Urs A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - Deciphering the sulfate attack of cementitious materials by high-resolution micro-x-ray diffraction N2 - The durability of cementitious materials depends, among others, on their resistance against chemical attack during the service life of a building. Here, we present an approach to analyze changes in the phase composition due to chemical attack in the form of sulfate ingress within the microstructure. Micro-X-ray (µX-ray) diffraction using synchrotron radiation in Debye–Scherrer (transmission) geometry allowed a spatial resolution of 10 µm. Phase transformations in the wake of damaging processes were observed in a detailed high-resolution imaging study. In comparison, samples containing supplementary cementitious materials were investigated and used to reconstruct the influence of different degeneration processes in detail. Additionally, reaction fronts within the bulk were localized by micro-X-ray fluorescence analysis. The experimental setup provided the possibility for analyzing the phase assemblage of a given sample without destroying the microstructure. The specimens for phase analysis are thick sections of the primary material and can be used for further microscopic analysis of the microstructure and microchemistry, e.g., scanning electron microscopy–energy-dispersive X-ray spectroscopy (SEM–EDX) or Raman spectroscopy. PY - 2011 DO - https://doi.org/10.1021/ac200181g SN - 0003-2700 SN - 1520-6882 VL - 83 IS - 10 SP - 3744 EP - 3749 PB - American Chemical Society CY - Washington, DC AN - OPUS4-23669 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Polte, Jörg A1 - Kraehnert, R. A1 - Radtke, Martin A1 - Reinholz, Uwe A1 - Riesemeier, Heinrich A1 - Thünemann, Andreas A1 - Emmerling, Franziska T1 - New insights of the nucleation and growth process of gold nanoparticles via in situ coupling of SAXS and XANES N2 - Although metallic nanoparticles play an important role in the area of nanotechnology, a coherent mechanistic explanation for the evolution of the particles during their chemical synthesis has not yet been provided in many cases. To gain a profound understanding of the growth mechanism of colloidal nanoparticles, new approaches using Small Angle X-Ray Scattering (SAXS) combined with X-ray absorption near-edge structure (XANES) are presented. This combination allows for insights into two prominent syntheses routes of gold nanoparticles (GNP): The 'slow' reaction using sodium citrate (30-90 min) as a reducing agent and the 'fast' reaction employing NaBH4 (within few seconds). In the first case data derived with the coupled XANES and SAXS suggests a four-step particle formation mechanism. For the second system a time resolution in the order of 100-200 ms was achieved by coupling a common laboratory SAXS instrument with a microstructured mixer, which allows data acquisition in a continuous-flow mode. The results indicate a coalescence driven growth process. Based on the capabilities to deduce the size, number and polydispersity of the particles, the results of both methods enable the development of mechanistic schemes explaining the different phases of particle formation and growth, thus providing a basis for improved control over the synthesis processes. KW - SAXS KW - XANES KW - Nanoparticle formation PY - 2010 DO - https://doi.org/10.1088/1742-6596/247/1/012051 SN - 1742-6588 SN - 1742-6596 VL - 247 IS - 1 SP - 012051-1 - 012051-10 PB - IOP Publ. CY - Bristol, UK AN - OPUS4-22684 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Polte, Jörg A1 - Erler, Robert A1 - Thünemann, Andreas A1 - Emmerling, Franziska A1 - Kraehnert, R. T1 - SAXS in combination with a free liquid jet for improved time-resolved in situ studies of the nucleation and growth of nanoparticles PY - 2010 DO - https://doi.org/10.1039/c0cc03238g SN - 0022-4936 SN - 0009-241x SN - 1359-7345 SN - 1364-548x VL - 46 IS - 48 SP - 9209 EP - 9211 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-23049 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Hennig, C. A1 - Ikeda-Ohno, A. A1 - Emmerling, Franziska A1 - Kraus, Werner A1 - Bernhard, G. T1 - Comparative investigation of the solution species [U(CO3)5]6- and the crystal structure of Na6[U(CO3)5].12H2O PY - 2010 DO - https://doi.org/10.1039/B922624A SN - 1477-9226 SN - 1477-9234 SN - 1364-5447 VL - 39 IS - 15 SP - 3744 EP - 3750 PB - RSC CY - Cambridge AN - OPUS4-23047 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Ortel, Erik A1 - Fischer, A. A1 - Chuenchom, L. A1 - Polte, Jörg A1 - Emmerling, Franziska A1 - Smarsly, B.M. A1 - Kraehnert, R. T1 - New triblock copolymer templates, PEO-PB-PEO, for the synthesis of titania films with controlles mesopore size, wall thickness, and bimodal porosity N2 - The synthesis and properties of a series of new structure-directing triblock copolymers with PEO-PB-PEO structure (PEO = poly(ethylene oxide) and PB = polybutadiene) and their application as superior pore-templates for the preparation of mesoporous titania coatings are reported. Starting from either TiCl4 or from preformed TiO2 nanocrystalline building blocks, mesoporous crystalline titanium oxide films with a significant degree of mesoscopic ordered pores are derived, and the pore size can be controlled by the molecular mass of the template polymer. Moreover, the triblock copolymers form stable micelles already at very low concentration, i.e., prior to solvent evaporation during the evaporation-induced self-assembly process (EISA). Consequently, the thickness of pore walls can be controlled independently of pore size by changing the polymer-to-precursor ratio. Thus, unprecedented control of wall thickness in the structure of mesoporous oxide coatings is achieved. In addition, the micelle formation of the new template polymers is sufficiently distinct from that of typical commercial PPO-PEO-PPO polymers (Pluronics; PPO = poly(propylene oxide)), so that a combination of both polymers facilitates bimodal porosity via dual micelle templating. KW - Mesoporous materials KW - Titanium oxide films KW - Anatase nanoparticles KW - PEO-PB-PEO KW - Dual templating PY - 2012 DO - https://doi.org/10.1002/smll.201101520 SN - 1613-6810 SN - 1613-6829 VL - 8 IS - 2 SP - 298 EP - 309 PB - Wiley-VCH Verl. CY - Weinheim AN - OPUS4-26277 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Schlegel, Moritz-Caspar A1 - Sarfraz, Adnan A1 - Müller, Urs A1 - Panne, Ulrich A1 - Emmerling, Franziska T1 - Erste Sekunden im Leben eines Bauwerks - In-situ-Synchrotron-Röntgenbeugungsuntersuchungen der Zementhydratation mit Millisekunden-Auflösung N2 - Höchst dynamische Hydratationsprozesse in den ersten Sekunden bei der Entstehung eines Bauwerkes lassen sich mithilfe von Synchrotron-Röntgenbeugung mit einer sehr hohen Zeitauflösung nachverfolgen. Der Schwerpunkt lag dabei auf der Beeinflussung der Bildung erster kristalliner Hydratationsprodukte während des Frühstadiums der Zementhydratation. KW - SyXRD KW - High resolution KW - In-situ KW - Colloidal suspension KW - Cement hydration KW - In-situ-Analyse KW - Kolloidale Suspensionen KW - Röntgenbeugung KW - Zementhydratation PY - 2012 DO - https://doi.org/10.1002/ange.201200993 SN - 0044-8249 SN - 0932-2140 SN - 1521-3757 VL - 124 IS - 20 SP - 5078 EP - 5081 PB - Wiley-VCH CY - Weinheim AN - OPUS4-26284 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gorelik, T.E. A1 - Sarfraz, Adnan A1 - Kolb, U. A1 - Emmerling, Franziska A1 - Rademann, Klaus T1 - Detecting crystalline nonequilibrium phases on the nanometer scale N2 - The use of Automated electron Diffraction Tomography (ADT) is presented as a novel approach for crystallization studies at the nanometer scale for nonequilibrium phases. Here, ADT was applied to elucidate the structural identity of the recently reported hexagonal morphology of caffeine crystals, which grow only on specific surfaces. Caffeine was crystallized from solution on a specially treated TEM carbon grid. The analysis of ADT data revealed that the lattice parameters of these hexagons match those of the high temperature α-form of caffeine. Furthermore, it was observed that in this hexagonal morphology, the α-form remained stable for a prolonged period of time. The stabilization of hexagons can be interpreted in terms of enhanced interactions with the supporting surfaces. KW - Electron diffraction KW - Polymorphism caffeine KW - ADT PY - 2012 DO - https://doi.org/10.1021/cg300377j SN - 1528-7483 VL - 12 IS - 6 SP - 3239 EP - 3242 PB - American Chemical Society CY - Washington, DC, USA AN - OPUS4-26285 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Heiden, Sebastian A1 - Batzdorf, Lisa A1 - Wenzel, Klaus-Jürgen A1 - Emmerling, Franziska T1 - Mechanochemical synthesis and structural characterisation of a theophylline-benzoic acid cocrystal (1:1) N2 - The structure of a mechanochemically synthesised cocrystal containing theophylline (TP) and benzoic acid (BA) has been determined from powder X-ray diffraction data. PY - 2012 DO - https://doi.org/10.1039/c2ce25236h SN - 1466-8033 N1 - Geburtsname von Batzdorf, Lisa: Tröbs, L. - Birth name of Batzdorf, Lisa: Tröbs, L. VL - 14 IS - 16 SP - 5128 EP - 5129 CY - London, UK AN - OPUS4-26286 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Drzymala, Sarah A1 - Kraus, Werner A1 - Emmerling, Franziska A1 - Koch, Matthias T1 - (3S,7R)-7,14,16-trihydroxy-3-methyl-3,4,5,6,7,8,9,10,11,12-decahydro-1H-2-benzoxacyclotetradecin-1-one N2 - The asymmetric unit of the title compound, C18H26O5, which is known as α-zearalanol, contains two molecules having the same conformation, with a r.m.s. deviation of less than 0.03 Å for all non-H atoms. In each independent molecule, an intramolecular O—H···O hydrogen bond stabilizes the molecular conformation. In the crystal, O—H···O hydrogen bonds link the molecules, forming infinite chains along [110] and [1¯10]. KW - Alpha-zearalanol KW - Zearalenon KW - Estrogen KW - Growth promoter KW - Ralgro PY - 2012 DO - https://doi.org/10.1107/S1600536812041141 SN - 1600-5368 VL - 68 IS - 11 SP - o3071, sup-1 - sup-11 PB - Munksgaard CY - Copenhagen AN - OPUS4-26771 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CHAP A1 - Carvalho, José Joao A1 - Emmerling, Franziska A1 - Schneider, Rudolf ED - Preedy, V.R. T1 - The chemistry of caffeine KW - Koffein KW - Chemie KW - Kristallstrukturen KW - Geschichte PY - 2012 SN - 978-1-84973-367-0 DO - https://doi.org/10.1039/9781849734752-00041 SN - 2045-1695 N1 - Serientitel: Food and nutritional components in focus – Series title: Food and nutritional components in focus VL - 2 IS - Chapter 3 SP - 41 EP - 52 PB - RSC Publ. AN - OPUS4-26531 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Al-Terkawi, Abdal-Azim A1 - Scholz, G. A1 - de Oliveira Guilherme Buzanich, Ana A1 - Reinsch, Stefan A1 - Kemnitz, E. A1 - Emmerling, Franziska T1 - Ca- and Sr- tetrafluoroisophthalates: mechanochemical synthesis, characterization, and ab initio structure determination N2 - New fluorinated coordination polymers were prepared mechanochemically by milling the alkaline earth metal hydroxides MII(OH)2·xH2O (MII: Ca, Sr) with tetrafluoroisophthalic acid (H2mBDC-F4). The structures of [{Ca(mBDC-F4)(H2O)2}·H2O] and [{Sr(mBDC-F4)(H2O)2}·H2O] were determined based on ab initio calculations and their powder X-ray diffraction (PXRD) data. The compounds are isomorphous and crystallize in the orthorhombic space group P212121. The determined structures were validated by using extended X-ray absorption (EXAFS) data. The new materials were thoroughly characterized using elemental analysis, thermal analysis, magic angle spinning NMR, and attenuated total reflection-infrared spectroscopy. Further characterization methods such as BET, dynamic vapor sorption, and scanning electron microscopy imaging were also used. Our investigations indicate that mechanochemistry is an efficient method for preparing such materials. KW - Mechanochemistry KW - In situ KW - XRD KW - Coordination polymers PY - 2017 UR - http://pubs.rsc.org/-/content/articlehtml/2017/dt/c7dt00734e DO - https://doi.org/10.1039/c7dt00734e VL - 46 IS - 18 SP - 6003 EP - 6012 AN - OPUS4-41516 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Matoga, D. A1 - Roztocki, K. A1 - Wilke, Manuel A1 - Emmerling, Franziska A1 - Oszajca, M. A1 - Fitta, M. A1 - Bałanda, M. T1 - Crystalline bilayers unzipped and rezipped: solid-state reaction cycle of a metal–organic framework with triple rearrangement of intralayer bonds N2 - We present a series of remarkable structural transformations for a family of layered metal–organic frameworks (MOFs) in a three-step solid-state reaction cycle. The cycle represents new dynamic behavior of 2D coordination polymers and involves the sequence of reactions: {[Mn2(ina)4(H2O)2]·2EtOH}n (JUK-1) → {(NH4)2[Mn(ina)2(NCS)2]}n·xH2O (JUK-2) → {[Mn2(ina)2(Hina)2(NCS)2]}n (JUK-3) → JUK-1 (Hina = isonicotinic acid), each accompanied by rearrangement of intralayer coordination bonds and each induced by a different external stimulus. In situ investigation of the first step of the cycle by combined synchrotron X-ray diffraction and Raman spectroscopy reveals direct mechanochemical unzipping of JUK-1 bilayers to respective JUK-2 layers with reaction rates dependent on the milling conditions. In contrast, the reverse zipping of JUK-2 layers involves two steps and proceeds through a new MOF (JUK-3) whose structure was elucidated by powder X-ray diffraction. Magnetic measurements confirm conversions of manganese nodes in the reaction cycle. The findings indicate the possibility of developing coordination-based assemblies with large structural responses for use in smart stimuli-responsive systems and sensor technologies. KW - Mechanochemistry KW - In situ KW - XRD KW - MOF PY - 2017 UR - http://pubs.rsc.org/is/content/articlehtml/2017/ce/c7ce00655a DO - https://doi.org/10.1039/C7CE00655A VL - 19 SP - 2987 EP - 2995 AN - OPUS4-41517 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wilke, Manuel A1 - Kabelitz, Anke A1 - Zimathies, Annett A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Crystal structure and in situ investigation of a mechanochemical synthesized 3D zinc N-(phosphonomethyl)glycinate N2 - The mechanochemical synthesis of the zinc N-(phosphonomethyl)glycinate Zn(O₃PCH₂NH₂CH₂CO₂) H₂O is presented. The structure was solved from powder X-ray diffraction (PXRD) data. In the three-dimensional pillared structure, the Zn atoms are coordinated tetrahedrally. In situ investigations of the reaction process with synchrotron PXRD and Raman spectroscopy reveal a two-step process including the formation of an intermediate. KW - Mechanochemistry KW - Metal phosphonate KW - In situ PY - 2017 DO - https://doi.org/10.1007/s10853-017-1121-7 SN - 0022-2461 SN - 1573-4803 VL - 52 IS - 20 SP - 12013 EP - 12020 PB - Springer CY - New York AN - OPUS4-41490 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kulla, Hannes A1 - Fischer, Franziska A1 - Benemann, Sigrid A1 - Rademann, K. A1 - Emmerling, Franziska T1 - The effect of the ball to reactant ratio on mechanochemical reaction times studied by in situ PXRD N2 - The effect of the reactant powder mass on reaction times for the mechanochemical formation of a soft matter model system was studied by in situ PXRD. The syntheses were performed at a constant ball mass in a shaker mill with and without glassy SiO2 as an inert additive. Reaction times decreased with the increase of the ball to reactant ratio (BRR). The kinetic influence of the SiO2 powder was excluded. The decrease in the reaction time with decreasing mass of reactants was related to the rise in the stress energy transferred to the powder by a higher ball impact. The BRR had no effect on the induction time. But the product conversion was accelerated by raising the BRR. While a certain temperature is needed for the activation of reactants in the induction phase, the conversion of soft matter reactants is rather controlled by impact than temperature. KW - XRD KW - Mechanochemistry PY - 2017 UR - http://pubs.rsc.org/en/content/articlehtml/2017/ce/c7ce00502d DO - https://doi.org/10.1039/c7ce00502d VL - 19 IS - 28 SP - 3902 EP - 3907 AN - OPUS4-41197 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lohrer, Christian A1 - Fink, Heidrun A1 - Kurth, Lutz T1 - Quality systems for fireworks - auditing experiences by the notified body BAM N2 - The coming into force of the European Directive 2007/23/EC of the European Parliament and of the Council of 23 May 2007 on the placing on the market of pyrotechnic articles changed the Situation regarding fireworks productions and tests in Europe significantly. According to the provisions of this Directive, the manufacturers/importers have to assure that fireworks articles are type tested by a Notified Body (or on behalf of a Notified Body) under this Directive before being placed on the European market and fulfill the essential safety requirements as per Annex I of the Directive 2007/23/EC. In addition, it is mandatory that the articles produced after the initial type test will be in conformity to the introduced type. The best sustainable way to assure this is the application of effective quality Systems (QS). Germany has a comparatively long tradition regarding auditing of such QS. Since 1978 it is mandatory for manufacturers/importers to set up adequate QS. The respective QS were extensively audited since the beginning of the 1990s in various countries to cover imported fireworks that were tested in a foreign country where the production took place. Within this long term auditing process in Germany, the QS strategies and contents changed in time due to new regulations and Standards, as well as gaining experiences (“lessons learned”). Recent audits carried out by BAM showed significant nonconformities in the QS of several Companies. Moreover, numerous small importers in Europe might be overwhelmed by the new regulations, leading to situations where products are placed on the European market, which were not sufficiently tested. This paper aims at giving an overview of the various advantages and weak points of all possible conformity assessment procedures regarding QS as set out in the Annex II of the Directive 2007/23/EC for fireworks, taking into account comprehensive experiences in this field by the Notified Body, BAM. T2 - 13th International symposium on fireworks CY - Valletta, Malta DA - 23.04.2012 KW - 2007/23/EC KW - QS modules KW - Product safety PY - 2012 SN - 978-0-9867279-3-1 SP - 159 EP - 172 AN - OPUS4-25796 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Löhnert, Andrea A1 - Rabe, Frederik A1 - Knaust, Christian A1 - Krause, U. T1 - Numerical and experimental investigation of fire smoke toxicity N2 - To predict the toxic hazards of fire smoke the concept of the Fractional Effective Dose (FED) is used (ISO13571 2012, ISO13344 2004). The Fractional Effective Doses of the main components from the fire smoke (CO, CO2, HCN etc.) are formed for every minute of the exposure interval and then summed up. If the sum of all doses over the exposure time reaches the value 1, incapacitation or death occurs (ISO13571 2012). T2 - International congress ' Fire computer modeling' CY - Cantabria, Spain DA - 18.10.2012 PY - 2012 SN - 978-84-86116-69-9 SP - 171 EP - 188 AN - OPUS4-27893 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Lohrer, Christian A1 - Kampa, Andreas A1 - Fink, Heidrun A1 - Kurth, Lutz A1 - Alef, G. T1 - Burst height measurements of spherical shells for different calibers and mortar lengths N2 - The current European draft Standard series FprEN 16261:2012 for display fireworks gives requirements on mortar lengths for different calibers to be used in the respective type and batch tests of spherical Shells. For each nominal shell caliber, a minimum and maximum permitted mortar length is defined. The mortar lengths deviations increase by increasing nominal calibers and the possible influence on the bürst height can only roughly be estimated. The aim of this work was to specify this influence of the mortar length on the bürst height of spherical Shells with regard to the permitted tolerances on performance parameters in type and batch tests as given in FprEN 16261-2:2012. Moreover, commonly used height measuring techniques were parallel taken to determine the bürst heights and were compared to each other in order to find an optimal test method for such measurements concerning accuracy, handling, application and costs. The following spherical Shells were part of this study: • Caliber 65 mm red peony, • Caliber 100 mm red peony, • Caliber 150 mm red peony, and • Caliber 200 yellow to blue - white flashing. For each caliber type, 15 single items were fired: 7 from the mortar offering the required minimum length and 8 from the mortar close to the required maximum length according to FprEN 16261:2012. T2 - 13th International symposium on fireworks CY - Valletta, Malta DA - 23.04.2012 KW - Altitude measurement techniques KW - Measurement uncertainties KW - Standardisation PY - 2012 SN - 978-0-9867279-3-1 SP - 145 EP - 158 AN - OPUS4-25795 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lueck, S. A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Hentschel, Manfred P. A1 - Schmidt, V. T1 - Statistical comparison of various reconstruction algorithms with respect to missing wedge artifacts in computed tomography N2 - The presence of elongation, streak and blurring artifacts in tomograms recorded under a missing wedge of rotation angles presents a major challenge for the quantitative analysis of tomographic image data. We show that the missing wedge artifacts of standard reconstruction algorithms may be reduced by the innovative reconstruction technique DIRECTT. For the comparison of missing wedge artifacts we apply techniques from spatial statistics, which have been specifically designed to investigate the shape of phase boundaries in tomograms. KW - X-ray tomography KW - Scanning transmission electron microscopy (STEM) KW - Structural PY - 2012 DO - https://doi.org/10.1557/opl.2012.209 SN - 0272-9172 VL - 1421 SP - 1 EP - 6 PB - North-Holland Publ. Co. CY - New York, NY AN - OPUS4-25468 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bernal, S. A. A1 - Angst, U. M. A1 - Provis, J. L. A1 - Thiel, C. A1 - Gluth, Gregor A1 - Villagran-Zaccardi, Y. A1 - De Belie, N. T1 - Recommendation of RILEM TC 281-CCC: RILEM CPC-18R1—guideline for measuring the carbonation depth of hardened concrete using a pH indicator solution N2 - This recommendation provides a procedure for determining the carbonation depth on the surface of concrete by applying a pH indicator. This includes definitions of carbonation, carbonation depth and carbonation front, as well as descriptions of the different pH indicator solutions that can be used. Recommendations for testing laboratory-prepared specimens and those obtained from concrete structures are also given. This involves guidelines for sample preparation and/or extraction, CO2 exposure duration, carbonation depth determination and reporting of results. A section on data interpretation is also provided, as carbonation results are used for determining durability of concrete, as well as a criterion for materials selection or for carbon uptake calculations. The new Recommendation CPC-18R1 is intended to supersede the former RILEM recommendation CPC-18, particularly when prescribed as the preferred method for evaluating and reporting carbonation depths. KW - Carbonation KW - Concrete KW - pH indicator KW - Phenolphthalein KW - Testing PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656191 DO - https://doi.org/10.1617/s11527-026-02966-0 SN - 1359-5997 SN - 1871-6873 VL - 59 IS - 3 SP - 1 EP - 11 PB - Springer Nature AN - OPUS4-65619 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scholl, Juliane A1 - Scharpmann, Philippa A1 - Bagheri, Abbas A1 - Lisec, Jan A1 - Meiers, Emelie A1 - Jaeger, Carsten A1 - Leonhardt, Robert A1 - Haase, Hajo A1 - Koch, Matthias T1 - Beyond the lab: Real-world composition of commercial Li-ion battery electrolytes N2 - This study presents a systematic, characterization of electrolytes from commercial lithium-ion batteries (LIB), encompassing 90 batteries from leading global manufacturers across diverse formats and application sectors. An integrated, complementary mass spectrometric workflow combining LC–MS/MS, GC–MS, and high-resolution MS was employed. To ensure robust structural annotation, molecular identifications were assigned confidence levels following Schymanski et al. (2014). Across all formats, PF6− was confirmed as the dominant Li+ counterion, frequently coexisting with BF4−, PO2F2−, and bis(fluorosulfonyl)imide (FSI−), forming binary and ternary salt systems optimized for both conductivity and safety. Solvent systems revealed the widespread use of propylene carbonate (PC) combined with diverse carbonate mixtures, demonstrating trends in performance optimization specific to cell format. A variety of additives were identified, reflecting a clear shift towards multifunctional, synergistic additive packages and the gradual replacement of fluorinated species with environmentally safer alternatives. Cycling studies demonstrated that electrolyte degradation mechanisms are strongly influenced by electrode composition and additive chemistry, with oxidative degradation pathways dominating. Together, these findings provide rare empirical insight into the evolving formulation strategies of electrolytes in commercial LIB, still employing classic carbonates and LiPF6, but highlighting a trend toward safer, more robust, and sustainable electrolyte architectures by using synergistic multifunctional systems. KW - Mass Spectrometry KW - Lithium-ion batteries KW - Electrolyte degradation PY - 2026 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-656254 DO - https://doi.org/10.1016/j.jpowsour.2026.239739 SN - 0378-7753 VL - 673 SP - 1 EP - 13 PB - Elsevier B.V. AN - OPUS4-65625 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lange, Axel A1 - Hentschel, Manfred P. A1 - Kupsch, Andreas A1 - Müller, Bernd R. T1 - Numerical correction of X-ray detector backlighting N2 - A novel approach to strongly suppress artifacts in radiography and computed tomography caused by the effect of diffuse background signals ('backlighting') of 2D X-ray detectors is suggested. Depending on the detector geometry the mechanism may be different, either based on the optical scattering by the fluorescent screen materials into optical detection devices or Compton or X-ray fluorescence scattering by the detector components. Consequently, these erroneous intensity portions result in locally different violations of Lambert–Beer's law in single projections (radiographs). When used as input data for computed tomography these violations are directly observed via modulation of the projected mass as a function of the rotation phase and the sample’s aspect ratio (dynamics). The magnitude of the diffuse background signal depends on the detector area covered by the projected sample. They are more pronounced the smaller the shadowed area and the stronger the total attenuation. This implies that the reconstruction suffers from additional anisotropic artifacts caused by elongated sample structures. This issue is studied simply by absorption of flat plates in a conventional laboratory radiography set-up and at a synchrotron radiation facility. In the latter case beam hardening artifacts can be excluded due to the monochromatic radiation. The proposed correction procedure requires simple integral intensity offsets as a constant (non-local) light scattering mechanism is assumed. KW - Detector backlighting KW - X-ray detector scattering KW - Fluorescent screen KW - Diffuse background KW - Computed tomography PY - 2012 DO - https://doi.org/10.3139/146.110659 SN - 1862-5282 VL - 103 IS - 2 SP - 174 EP - 178 PB - Carl Hanser CY - München AN - OPUS4-25553 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krebber, Katerina A1 - Lenke, Philipp A1 - Liehr, Sascha A1 - Nöther, N. A1 - Wendt, Mario A1 - Wosniok, Aleksander A1 - Daum, Werner T1 - Structural health monitoring by distributed fiber optic sensors embedded into technical textiles N2 - Technical textiles with embedded distributed fiber optic sensors have been developed for the purposes of structural health monitoring in geotechnical and civil engineering. The distributed fiber optic sensors are based on Brillouin scattering in silica optical fibers and OTDR in polymer optical fibers. Such 'smart' technical textiles are used for reinforcement of geotechnical and masonry structures. The embedded fiber optic sensors provide online information about the condition of the structure and about the occurrence and location of any damage or degradation. N2 - Technische Textilien mit integrierten faseroptischen Sensoren eröffnen neue Möglichkeiten der Zustandsüberwachung (structural health monitoring) in Geotechnik und Ingenieurbau. Die verteilt messenden Sensoren basieren auf der Brillouin-Streuung in Glasfasern und auf der OTDR in polymeroptischen Fasern. Derartige 'intelligente' technische Textilien werden in erster Line zur Verstärkung von geotechnischen Bauwerken und von Gebäuden genutzt. Die integrierten Sensoren liefern eine zeitnahe Information über den bestimmungsgemäßen Zustand des Bauwerks sowie über die Entstehung und den Ort von lokalen Bauwerksschäden. KW - Fiber optic sensor KW - Distributed sensor KW - Brillouin scattering KW - Polymer optical fiber KW - Strain sensor KW - Smart geotextiles KW - Faseroptischer Sensor KW - Verteilter Sensor KW - Brillouin-Streuung KW - Polymeroptische Faser KW - Dehnungssensor KW - Intelligentes Geotextil PY - 2012 DO - https://doi.org/10.1524/teme.2012.0238 SN - 0340-837X SN - 0178-2312 SN - 0171-8096 VL - 79 IS - 7-8 SP - 337 EP - 347 PB - Oldenbourg CY - München AN - OPUS4-26387 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Liehr, Sascha A1 - Burgmeier, J. A1 - Krebber, Katerina A1 - Schade, W. ED - Liao, Y. ED - Jin, W. ED - Sampson, D.D. ED - Yamauchi, R. ED - Chung, Y. ED - Nakamura, K. ED - Rao, Y. T1 - Fiber optic bend and temperature sensing in femtosecond laser-structured POF N2 - We propose focused femtosecond laser irradiation to create stable and permanent scattering damage in large-core polymer optical fibers. Possible sensing applications using optical time domain reflectometry are discussed and presented. Experiments show that quasi-distributed fiber bend sensors and absolute temperature sensors can be realized by evaluating backscatter intensities. T2 - OFS2012 - 22nd International conference on optical fiber sensors CY - Beijing, China DA - 15.10.2012 KW - Polymer optical fiber KW - POF KW - Optical fiber sensors KW - Bend sensor KW - Temperature sensor KW - Femtosecond laser KW - OTDR KW - Reflectometry PY - 2012 DO - https://doi.org/10.1117/12.976051 SN - 0277-786X SN - 1996-756X N1 - Serientitel: Proceedings of SPIE – Series title: Proceedings of SPIE IS - 8421 SP - 84213I-1 EP - 84213I-4 PB - SPIE, the International Society for Optical Engineering CY - Bellingham, Wash. AN - OPUS4-27221 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Grothausmann, R. A1 - Zehl, G. A1 - Manke, I. A1 - Fiechter, S. A1 - Bogdanoff, P. A1 - Dorbandt, I. A1 - Kupsch, Andreas A1 - Lange, Axel A1 - Hentschel, Manfred P. A1 - Schumacher, G. A1 - Banhart, J. T1 - Dreidimensionale Charakterisierung von Katalysatornanopartikeln N2 - We present transmission electron microscope (TEM) tomography investigations of ruthenium-based fuel cell catalyst materials as employed in direct methanol fuel cells (DMFC). The digital three-dimensional representation of the samples not only enables detailed studies on number, size, and shape but also on the local orientation of the ruthenium particles to their support and their freely accessible surface area. The shape analysis shows the ruthenium particles deviate significantly from spherical symmetry which increases their surface to volume ratio. The morphological studies help to understand the structure formation mechanisms during the fabrication as well as the high effectiveness of these catalysts in the oxygen reduction reaction at the cathode side of fuel cells. KW - Radiography KW - Tomography KW - Neutrons KW - Polymer electrolyte membrane fuel cell (PEMFC) KW - Fuel cell stack PY - 2012 SN - 1862-5282 VL - 103 IS - 1 SP - 135 EP - 136 PB - Carl Hanser CY - München AN - OPUS4-25976 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Krüger, Oliver A1 - Adam, Christian T1 - Resource recovery potential of sewage sludge ashes (SSA) N2 - Phosphorous is essential for all animate beings and not replaceable in its functions, e.g. for intracellular energy transfer (ATP) or storage and expression of genetic information (DNA, RNA). Currently, 125,000 t of phosphorous is used as mineral fertilizer in Germany annually. Most of the phosphorous is mined as rock phosphate and thus a finite resource with an estimated static Lifetime of around 120 years. Since Europe does not possess significant deposits, the dependence on Imports is very high. This problem may be diminished by phosphorous recovery from sewage sludge ash (SSA). More than half of the thermally treated sewage sludge is currently co-incinerated in cement or power plants as well as municipal waste incineration plants. T2 - Crete 2012 - 3rd International conference on industrial and hazardous waste management CY - Chania, Crete, Greece DA - 12.09.2012 KW - Sewage sludge ash KW - Phosphorous recovery KW - Mass balance KW - Resource recovery potential PY - 2012 SN - 978-960-8475-17-5 SN - 2241-3138 IS - Session 5: Recovery opportunities SP - 73 EP - 74 AN - OPUS4-26570 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kühl, Christiane T1 - Ausschuss für Rohrfernleitungen - Ergebnisse und Empfehlungen zu nationalen und internationalen Fach- und Regelungsfragen N2 - Rohrfernleitungen für die Beförderung von Öl oder Gas sind wichtige Einrichtungen zur Sicherstellung der Energieversorgung. Entsprechende Gesetze, Verordnungen, technische und organisatorische Regelungen sorgen dafür, dass beginnend mit der Planung bis hin zum Bau und Betrieb von Rohrfernleitungen zum Schutz von Mensch und Umwelt ein hohes Maß an Sicherheit gewährleistet ist. Über diese Regelungen hinaus sind oftmals auch fachliche Fragestellungen zu klären, die sich zum Beispiel aus dem Praxisbetrieb ergeben. Das Bundministerium für Umwelt, Naturschutz und Reaktorsicherheit (BMU) hat über die Rohrfernleitungsverordnung einen Ausschuss etabliert, der sich sowohl mit konkreten Anpassungen des Rohrfernleitungsrechts an den Stand der Technik auseinandersetzt als auch Vorschläge und Empfehlungen für das BMU und für die Fachwelt zu fachlichen Problemen und Fragen erarbeitet. Im Folgenden werden Ergebnisse und Empfehlungen des Ausschusses für Rohrfernleitungen zu nationalen und internationalen Fach- und Regelungsfragen beschrieben. T2 - 26. Oldenburger Rohrleitungsforum - Rohrleitungen - in neuen Energieversorgungskonzepten CY - Oldenburg, Deutschland DA - 09.02.2012 KW - Rohrfernleitungen KW - Pipelines KW - Ausschuss für Rohrfernleitungen PY - 2012 SN - 978-3-8027-2857-0 N1 - Serientitel: Schriftenreihe aus dem Institut für Rohrleitungsbau Oldenburg – Series title: Schriftenreihe aus dem Institut für Rohrleitungsbau Oldenburg VL - 37 IS - Kap. II.D.4 SP - 551 EP - 561 PB - Vulkan CY - Essen AN - OPUS4-25519 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kruschwitz, Sabine A1 - Niederleithinger, Ernst A1 - Trela, Christiane A1 - Wöstmann, Jens T1 - Use of complex resistivity tomography for moisture monitoring in a flooded masonry specimen N2 - Moisture ingress is one of the major deteriorating factors for building materials. Today, the only approved way to assess such damage is the gravimetric Darr method, which is essentially destructive. Substantial progress has been made using the geophysical complex-resistivity method, which can be applied non-destructively and provides spatial information along two-dimensional sections, rather than punctual along one borehole. Considerable advantages of complex resistivity are its sensitivity to textural properties, as well as the pore-fluid chemistry of wet, porous media. In a comprehensive laboratory study, and later in field scale experiments, it could be shown that complex resistivity may even be able to distinguish between salt content and saturation degree in a single measurement. A comparison with complementary nondestructive testing techniques points to the benefit and further research to be explored in multimethodical approaches. KW - Moisture KW - Salt KW - Masonry KW - Damage KW - Electrical resistivity KW - Radar KW - Radiography KW - Microwaves KW - Ground-penetrating radar KW - Microwave transmission PY - 2012 DO - https://doi.org/10.1061/(ASCE)IS.1943-555X.0000053 SN - 1076-0342 SN - 1943-555X VL - 18 IS - 1 (Special issue) SP - 2 EP - 11 CY - New York, NY AN - OPUS4-29536 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - INPR A1 - Smales, Glen J. A1 - Appel, Paul Alexander A1 - Breßler, Ingo A1 - Chambers, Aaron A1 - Dumele, Oliver A1 - Ebisch, Maximilian A1 - Frontzek, Julius A1 - del Refugio Monroy, José A1 - Rosalie, Julian M. A1 - Pauw, Brian R. T1 - DACHS and RoWaN: The Automated and Traceable Synthesis of ZIF-8 N2 - Automated synthesis and open-data practices are increasingly seen as key enablers of transparent, traceable, and reproducible science. By combining automation with structured, metadata-rich documentation, it becomes possible to systematically com- pare synthesis strategies and link outcomes to detailed parameters. In this work, we implement such an approach to study the synthesis of ZIF-8, comparing hand and automation-assisted methods under controlled conditions. Using over 100 synthesis experiments, we assess the repeatability of particle size and yield, and explore how variations in mixing and injection influence outcomes. This study demonstrates how traceable synthesis workflows can support repeatability and comparison across synthe- sis strategies. The DACHS (Database for Automation, Characterization and Holistic Synthesis) framework underpins this work, providing a lightweight infrastructure for transparent synthesis data capture. KW - Automation KW - MOFs KW - SAXS PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-645861 DO - https://doi.org/10.26434/chemrxiv-2025-7fgg0 SP - 1 EP - 32 PB - Cambridge AN - OPUS4-64586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Diehn, S. A1 - Zimmermann, B. A1 - Tafintseva, V. A1 - Seifert, S. A1 - Bagcioglu, M. A1 - Ohlson, M. A1 - Weidner, Steffen A1 - Fjellheim, S. A1 - Kohler, A. A1 - Kneipp, Janina T1 - Combining Chemical Information From Grass Pollen in Multimodal Characterization N2 - The analysis of pollen chemical composition is important to many fields, including agriculture, plant physiology, ecology, allergology, and climate studies. Here, the potential of a combination of different spectroscopic and spectrometric methods regarding the characterization of small biochemical differences between pollen samples was evaluated using multivariate statistical approaches. Pollen samples, collected from three populations of the grass Poa alpina, were analyzed using Fourier-transform infrared (FTIR) spectroscopy, Raman spectroscopy, surface enhanced Raman scattering (SERS), and matrix assisted laser desorption/ionization mass spectrometry (MALDI-TOF MS). The variation in the sample set can be described in a hierarchical framework comprising three populations of the same grass species and four different growth conditions of the parent plants for each of the populations. Therefore, the data set can work here as a model system to evaluate the classification and characterization ability of the different spectroscopic and spectrometric methods. ANOVA Simultaneous Component Analysis (ASCA) was applied to achieve a separation of different sources of variance in the complex sample set. Since the chosen methods and sample preparations probe different parts and/or molecular constituents of the pollen grains, complementary information about the chemical composition of the pollen can be obtained. By using consensus principal component analysis (CPCA), data from the different methods are linked together. This enables an investigation of the underlying global information, since complementary chemical data are combined. The molecular information from four spectroscopies was combined with phenotypical information gathered from the parent plants, thereby helping to potentially link pollen chemistry to other biotic and abiotic parameters. KW - Pollen KW - MALDI-TOF MS KW - FTIR KW - Raman KW - Multivariate analyses PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-504822 DO - https://doi.org/10.3389/fpls.2019.01788 VL - 10 SP - 1788 AN - OPUS4-50482 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -