TY - JOUR A1 - Weber, K. A1 - Weber, M. A1 - Menneken, M. A1 - Kral, A. G. A1 - Mertz-Kraus, R. A1 - Geisler, T. A1 - Vogl, Jochen A1 - Tütken, T. T1 - Diagenetic stability of non-traditional stable isotope systems (Ca, Sr, Mg, Zn) in teeth – An in-vitro alteration experiment of biogenic apatite in isotopically enriched tracer solution N2 - Stable isotope ratios and trace element concentrations of fossil bones and teeth are important geochemical proxies for the reconstruction of diet and past environment in archaeology and palaeontology. However, since diagenesis can significantly alter primary diet-related isotope signatures and elemental compositions, it is important to understand and quantify alteration processes. Here, we present the results of in-vitro Alteration experiments of dental tissues from a modern African elephant molar reacted in aqueous solutions at 30 °C and 90 °C for 4 to 63 days. Dental cubes with ≈ 3 mm edge length, comprising both enamel and dentin, were placed into 2 mL of acidic aqueous solution enriched in different isotopes (25Mg, 44Ca, 67Zn, 86Sr, initial pH 1). Element and isotope distribution profiles across the reacted cubes were measured with LA-(MC-)ICP-MS and EMPA, while potential effects on the bioapatite crystal structure were characterised by Raman spectroscopy. In all experiments isotope ratios measured by LA-(MC-)ICP-MS revealed an alteration of the enamel in the outer ≈ 200–300 μm. In contrast, dentin was fully altered (≈ 1.4 mm) after one week at 90 °C while the alteration did not exceed a depth of 150–200 μm during the 30 °C experiments. Then, the tracer solution started also to penetrate through the enamel-dentin junction into the innermost enamel, however, leaving the central part of the enamel unaltered, even after three months. The Raman spectra suggest an initial demineralisation in the acidic environment while organic matter (i.e. collagen) is still preserved. In the 90 °C experiment, Raman spectra of the v1 PO4) band of the dentin shift over time towards synthetic hydroxylapatite patterns and the Ca (and Sr) concentrations in the respective solutions decrease. This indicates precipitation of newly formed apatite. Isotope and element concentration profiles across the dental tissues reveal different exchange mechanisms for different isotope systems. Magnesium is leached from enamel and dentin, while Zn is incorporated into the apatite crystal structure. However, the distribution of both elements is not affected in the innermost enamel where their concentrations do not change over the whole duration of the experiments. We found no correlation of reaction depth in the cubes and experimental duration, which might be caused by natural variability of the dental material already at the beginning of the experiment. Our alteration experiments in a closed system at high temperatures ≤90 °C and low initial pH demonstrate that at least the central part of mm-thick mammalian enamel apatite seems to be resistant against alteration preserving its pristine bioapatite mineral structure as well as its in-vivo elemental and isotopic composition. The experiments assess diagenetic alteration in a novel multi-proxy approach using in-situ analyses in high spatial resolution. It is demonstrated that the isotopes of Ca, Sr, Zn and Mg in the dentin are prone for diagenetic alteration, while enamel is more resistant against alteration and could be used for dietary and physiological reconstructions in fossil teeth. KW - Bioapatite KW - Isotopes KW - Raman spectroscopy KW - Diagenesis KW - LA-(MC-)ICP-MS KW - EPMA PY - 2021 DO - https://doi.org/10.1016/j.chemgeo.2021.120196 VL - 572 SP - 120196 PB - Elsevier B.V. CY - Amsterdam AN - OPUS4-52447 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Bekemeier, Simon A1 - Caldeira Rêgo, C. R. A1 - Mai, H. L. A1 - Sikia, Ujjal A1 - Waseda, O. A1 - Apel, M. A1 - Arendt, F. A1 - Aschemann, A. A1 - Bayerlein, Bernd A1 - Courant, R. A1 - Dziwis, G. A1 - Fuchs, F. A1 - Giese, U. A1 - Junghanns, K. A1 - Kamal, M. A1 - Koschmieder, L. A1 - Leineweber, S. A1 - Luger, M. A1 - Lukas, M. A1 - Maas, J. A1 - Mertens, J. A1 - Mieller, Björn A1 - Overmeyer, L. A1 - Pirch, N. A1 - Reimann, J. A1 - Schröck, S. A1 - Schulze, P. A1 - Schuster, J. A1 - Seidel, A. A1 - Shchyglo, O. A1 - Sierka, M. A1 - Silze, F. A1 - Stier, S. A1 - Tegeler, M. A1 - Unger, Jörg F. A1 - Weber, M. A1 - Hickel, Tilmann A1 - Schaarschmidt, J. T1 - Advancing Digital Transformation in Material Science: The Role of Workflows Within the MaterialDigital Initiative N2 - The MaterialDigital initiative represents a major driver toward the digitalization of material science. Next to providing a prototypical infrastructure required for building a shared data space and working on semantic interoperability of data, a core focus area of the Platform MaterialDigital (PMD) is the utilization of workflows to encapsulate data processing and simulation steps in accordance with findable, accessible, interoperable, and reusable principles. In collaboration with the funded projects of the initiative, the workflow working group strives to establish shared standards, enhancing the interoperability and reusability of scientific data processing steps. Central to this effort is the Workflow Store, a pivotal tool for disseminating workflows with the community, facilitating the exchange and replication of scientific methodologies. This article discusses the inherent challenges of adapting workflow concepts, providing the perspective on developing and using workflows in the respective domain of the various funded projects. Additionally, it introduces the Workflow Store’s role within the initiative and outlines a future roadmap for the PMD workflow group, aiming to further refine and expand the role of scientific workflows as a means to advance digital transformation and foster collaborative research within material science. KW - Digitalisation KW - FAIR principles KW - MaterialDigital KW - Scientific workflows KW - Semantic interoperability PY - 2025 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-624088 DO - https://doi.org/10.1002/adem.202402149 SN - 1527-2648 IS - 2402149 SP - 1 EP - 25 PB - Wiley-VCH GmbH AN - OPUS4-62408 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - BOOK A1 - Maiwald, Michael A1 - Bassler, M. A1 - Deilmann, M. A1 - Ens, W. A1 - Frenzel, F. A1 - Gerlach, M. A1 - Großmann, J. A1 - Grümbel, F. A1 - Heisterkamp, M. A1 - Kaiser, U. A1 - Lambrecht, A. A1 - Ohlenkamp, R. A1 - Pötter, T. A1 - Pyka, P. A1 - Roos, E. A1 - Schmidt, A. A1 - Schünemann, U. A1 - Theuer, M. A1 - Tukle, A. A1 - Weber, N. T1 - Technologie-Roadmap „Prozess-Sensoren 2027+“ N2 - Die Technologie-Roadmap „Prozess-Sensoren 2027+“ ist eine Weiterentwicklung vorgängiger Technologie-Roadmaps. Im Zentrum dieser Roadmaps stehen Sensoren zur Erfassung von physikalischen und chemischen Messgrößen mittels spezifischer und unspezifischer Messverfahren, die zur Steuerung und dem besseren Verständnis von Prozessen dienen. Die Roadmap fasst die gemeinsame Technologie- und Marktsicht von Anwendern, Herstellern und Forschungseinrichtungen im Bereich Prozess-Sensorik in der verfahrenstechnischen Industrie zusammen. Sie beschreibt die wesentlichen Trends im Bereich Prozess-Sensorik und künftige Handlungsbedarfe für Hersteller, Anwender sowie für Einrichtungen der Forschung und Lehre. Für die aktuellen und zukünftigen Anforderungen an Prozess-Sensoren werden 19 Thesen formuliert. Die Thesen basieren auf den Thesen der vorangegangenen Roadmaps, wobei die aus heutiger Sicht erforderlichen Anpassungen, Ergänzungen und teilweise auch Streichungen vorgenommen wurden. Die Thesen sind in 5 Themencluster eingeordnet. Digitalisierung und Nachhaltigkeit sind übergreifende Kernthemen der künftigen Entwicklung. KW - Technologie-Roadmap Prozess-Sensoren KW - Prozessindustrie KW - Prozessanalytik KW - Sensorik KW - Digitalisierung KW - NAMUR PY - 2021 SP - 1 EP - 63 AN - OPUS4-53741 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Krebber, Katerina A1 - Weege, S. A1 - Großwig, S. A1 - Obermöller, M. A1 - Perk, M. A1 - Lu, Xin A1 - Schukar, Marcus A1 - Weber, U. A1 - Pfeiffer, T. A1 - Rembe, M. T1 - Kombinierte faseroptische Messungen in Bohrlöchern helfen bei der Detektion von Kleinstleckagen N2 - Seit November 2019 läuft ein breit angelegtes und vom BMWi gefördertes ZIM-Kooperationsprojekt zwischen der Bundesanstalt für Materialforschung und -prüfung (BAM), der IAB'Weimar gGmbH, der GKSO GmbH & Co. Projekt KG, der DEEP.KBB GmbH sowie der Rembe Consulting PartG mbB. Ziel des Forschungsvorhabens sind sowohl die Lokalisierung als auch die Quantifizierung insbesondere sehr kleiner Leckagen in einer Bohrlochverrohrung durch die Nutzung faseroptischer Messtechnik. Durch Messdatenkopplung und den Wegfall bewegungsbedingter Nachteile einer Messsonde werden wesentlich präzisere Ergebnisse zur Bewertung der Bohrlochintegrität als üblich erwartet. T2 - DGMK/ÖGEW-Frühjahrstagung 2020 CY - Meeting was canceled DA - 15.04.2020 KW - Wasserstoffspeicher KW - Kavernenspeicher KW - Verteilte faseroptische akustische Sensorik PY - 2020 VL - 6 SP - 43 EP - 43 PB - DVV Media Group CY - Hamburg AN - OPUS4-52233 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kern, Simon A1 - Wander, Lukas A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Gottu Mukkula, A. R. A1 - Holtkamp, M. A1 - Salge, M. A1 - Fleischer, C. A1 - Weber, N. A1 - King, R. A1 - Engell, S. A1 - Paul, Andrea A1 - Pereira Remelhe, M. A1 - Maiwald, Michael T1 - Flexible Automation with compact NMR instruments N2 - Modular plants using intensified continuous processes represent an appealing concept to produce pharmaceuticals. It can improve quality, safety, sustainability, and profitability compared to batch processes, and it enables plug-and-produce reconfiguration for fast product changes. To facilitate this flexibility by real-time quality control, we developed a solution that can be adapted quickly to new processes and includes a compact Nuclear Magnetic Resonance (NMR) spectrometer for online quality monitoring as well as a new model-based control approach. The NMR sensor is a benchtop device enhanced to the requirements of automated chemical production including ro-bust evaluation of sensor data. Here, we present alternatives for the quantitative determination of the analytes using modular, physically motivated models. These models can be adapted to new substances solely by the use of their corresponding pure component spectra, which can either be derived from experimental spectra as well as from quantum mechanical models or NMR predictors. Modular means that spec-tral models can simply be exchanged together with alternate reagents and products. Beyond that, we comprehensively calibrated an NIR spectrometer based on online NMR process data for the first time within an industrial plant. The integrated solution was developed for a metal organic reac-tion running on a commercial-scale modular pilot plant and it was tested under industrial conditions. T2 - 7th Annual PANIC Conference CY - Hilton Head Island, South Carolina, USA DA - 03.03.2019 KW - Online NMR Spectroscopy PY - 2019 AN - OPUS4-47715 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Kern, Simon A1 - Wander, Lukas A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Gottu Mukkula, A. R. A1 - Holtkamp, M. A1 - Salge, M. A1 - Fleischer, C. A1 - Weber, N. A1 - Engell, S. A1 - Paul, Andrea A1 - Pereira Remelhe, M. A1 - Maiwald, Michael T1 - Flexible automation with compact NMR spectroscopy for continuous production of pharmaceuticals N2 - Modular plants using intensified continuous processes represent an appealing concept for the production of pharmaceuticals. It can improve quality, safety, sustainability, and profitability compared to batch processes; besides, it enables plug-and-produce reconfiguration for fast product changes. To facilitate this flexibility by real-time quality control, we developed a solution that can be adapted quickly to new processes and is based on a compact nuclear magnetic resonance (NMR) spectrometer. The NMR sensor is a benchtop device enhanced to the requirements of automated chemical production including robust evaluation of sensor data. Beyond monitoring the product quality, online NMR data was used in a new iterative optimization approach to maximize the plant profit and served as a reliable reference for the calibration of a near-infrared (NIR) spectrometer. The overall approach was demonstrated on a commercial-scale pilot plant using a metal-organic reaction with pharmaceutical relevance. KW - NMR Spectroscopy KW - NIR Spectroscopy KW - Real-time process monitoring KW - Real-time quality control KW - Continuous processes KW - CONSENS KW - Data Fusion PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-480623 DO - https://doi.org/10.1007/s00216-019-01752-y SN - 1618-2642 SN - 1618-2650 VL - 411 IS - 14 SP - 3037 EP - 3046 PB - Springer Nature CY - Heidelberg AN - OPUS4-48062 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weber, A. A1 - von Randow, M. A1 - Voigt, A.-L. A1 - von der Au, Marcus A1 - Fischer, E. A1 - Meermann, Björn A1 - Wagner, M. T1 - Ingestion and toxicity of microplastics in the freshwater gastropodLymnaea stagnalis: No microplastic-induced effects alone or incombination with copper N2 - The interaction of microplastics with freshwater biota and their interaction with other stressors is still not very well understood. Therefore, we investigated the ingestion, excretion and toxicity of microplastics in the freshwater gastropod Lymnaea stagnalis. MP ingestion was analyzed as tissues levels in L. stagnalis after 6–96 h of exposure to 5–90 μm spherical polystyrene (PS) microplastics. To understand the excretion, tissue levels were determined after 24 h of exposure followed by a 12 h–7 d depuration period. To assess the toxicity, snails were exposed for 28 d to irregular PS microplastics (<63 μm, 6.4–100,000 particles mL−1), both alone and in combination with copper as additional stressor. To compare the toxicity of natural and synthetic particles, we also included diatomite particles. Microplastics ingestion and excretion significantly depended on the particle size and the exposure/depuration duration. An exposure to irregular PS had no effect on survival, reproduction, energy reserves and oxidative stress. However, we observed slight effects on immune cell phagocytosis. Exposure to microplastics did not exacerbate the reproductive toxicity of copper. In addition, there was no pronounced difference between the effects of microplastics and diatomite. The tolerance towards microplastics may originate from an adaptation of L. stagnalis to particle-rich environments or a general stress resilience. In conclusion, despite high uptake rates, PS fragments do not appear to be a relevant stressor for stress tolerant freshwater gastropods considering current environmental levels of microplastics. KW - Lymnaea stagnalis KW - Microplastic-induced effects KW - Mixture toxicity PY - 2020 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-513551 DO - https://doi.org/10.1016/j.chemosphere.2020.128040 VL - 263 SP - 128040 PB - Elsevier Ltd. AN - OPUS4-51355 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Villatoro, J. A1 - Zühlke, M. A1 - Riebe, D. A1 - Beitz, T. A1 - Weber, M. A1 - Riedel, Jens A1 - Löhmannsröben, H.-G. T1 - IR-MALDI ion mobility spectrometry: physical source characterization and application as HPLC detector N2 - Infraredmatrix-assisted laser dispersion and ionization(IR-MALDI) in combination with on mobility (IM) spectrometry enables the direct Analysis of biomolecules in aqueous solution. The release of ions directly from an aqueous solution is based on a phase explosion, induced by the Absorption of an IR laser pulse, which disperses the liquid as vapor, nano- and micro-droplets. The ionization process is characterized initially by a broad spatial distribution of the ions, which is a result of complex fluid dynamics and desolvation kinetics. These processes have a profound effect on the shape and width of the peaks in the IM spectra. In this work, the Transport of ions by the phase explosion-induced shockwave could be studied independently from the transport by the electric field. The shockwave-induced mean velocities of the ions at different time scales were determined through IM spectrometry and shadowgraphy. The results show a deceleration of the Ions from 118m∙s−1 at a distance of 400 μm from the liquid surface to 7.1 m∙s−1 at a distance of 10 mm, which is caused by a pileup effect. Furthermore, the desolvation kinetics were investigated and a first-order desolvation constant of 325 ± 50 s−1 was obtained. In the second part, the IR-MALDI-IM spectrometer is used as an HPLC detector for the twodimensional separation of a pesticide mixture. KW - Ion mobility spectrometry KW - IR-MALDI KW - Shadowgraphy KW - Laser PY - 2016 DO - https://doi.org/10.1007/s12127-016-0208-1 VL - 2016 IS - 4 SP - 197 EP - 207 PB - Springer-Verlag Berlin CY - Heidelberg AN - OPUS4-38467 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - GEN A1 - Kern, Simon A1 - Wander, Lukas A1 - Meyer, Klas A1 - Guhl, Svetlana A1 - Gottu Mukkula, A. R. A1 - Holtkamp, M. A1 - Salge, M. A1 - Fleischer, C. A1 - Weber, N. A1 - Engell, S. A1 - Paul, Andrea A1 - King, R. A1 - Maiwald, Michael T1 - Raw data of pilot plant runs for CONSENS project (Case study 1) N2 - In case study one of the CONSENS project, two aromatic substances were coupled by a lithiation reaction, which is a prominent example in pharmaceutical industry. The two aromatic reactants (Aniline and o-FNB) were mixed with Lithium-base (LiHMDS) in a continuous modular plant to produce the desired product (Li-NDPA) and a salt (LiF). The salt precipitates which leads to the formation of particles. The feed streams were subject to variation to drive the plant to its optimum. The uploaded data comprises the results from four days during continuous plant operation time. Each day is denoted from day 1-4 and represents the dates 2017-09-26, 2017-09-28, 2017-10-10, 2017-10-17. In the following the contents of the files are explained. KW - Process Analytical Technology KW - Multivariate Data Analysis KW - Nuclear Magnetic Resonance KW - Near Infrared Spectroscopy KW - Continuous Manufacturing KW - CONSENS PY - 2018 DO - https://doi.org/10.5281/zenodo.1438233 PB - Zenodo CY - Geneva AN - OPUS4-48063 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Beygi Nasrabadi, Hossein A1 - Hanke, T. A1 - Weber, M. A1 - Eisenbart, M. A1 - Bauer, F. A1 - Meissner, R. A1 - Dziwis, G. A1 - Tikana, L. A1 - Chen, Yue A1 - Skrotzki, Birgit T1 - Toward a digital materials mechanical testing lab N2 - To accelerate the growth of Industry 4.0 technologies, the digitalization of mechanical testing laboratories as one of the main data-driven units of materials processing industries is introduced in this paper. The digital lab infrastructure consists of highly detailed and standard-compliant materials testing knowledge graphs for a wide range of mechanical testing processes, as well as some tools that enable the efficient ontology development and conversion of heterogeneous materials’ mechanical testing data to the machine-readable data of uniform and standardized structures. As a basis for designing such a digital lab, the mechanical testing ontology (MTO) was developed based on the ISO 23718 and ISO/IEC 21838-2 standards for the semantic representation of the mechanical testing experiments, quantities, artifacts, and report data. The trial digitalization of materials mechanical testing lab was successfully performed by utilizing the developed tools and knowledge graph of processes for converting the various experimental test data of heterogeneous structures, languages, and formats to standardized Resource Description Framework (RDF) data formats. The concepts of data storage and data sharing in data spaces were also introduced and SPARQL queries were utilized to evaluate how the introduced approach can result in the data retrieval and response to the competency questions. The proposed digital materials mechanical testing lab approach allows the industries to access lots of trustworthy and traceable mechanical testing data of other academic and industrial organizations, and subsequently organize various data-driven research for their faster and cheaper product development leading to a higher performance of products in engineering and ecological aspects. KW - General Engineering KW - General Computer Science PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-582698 DO - https://doi.org/10.1016/j.compind.2023.104016 SN - 0166-3615 VL - 153 SP - 1 EP - 15 PB - Elsevier B.V. AN - OPUS4-58269 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Unterlass, M.M. A1 - Emmerling, Franziska A1 - Antonietti, M. A1 - Weber, J. T1 - From dense monomer salt crystals to CO2 selective microporous polyimides via solid-state polymerization N2 - Fully aromatic polyimides are synthesized via solid-state polymerization of the corresponding monomer salts. The crystal structure of salts shows strong hydrogen bonding of the reactive groups and thereby paves the way for solid-state transformations. The polycondensation yields copies of the initial salt crystallite habits, accompanied by the development of a porosity especially suited for CO2. PY - 2014 DO - https://doi.org/10.1039/c3cc47674j SN - 0022-4936 SN - 0009-241x SN - 1359-7345 SN - 1364-548x VL - 50 IS - 4 SP - 430 EP - 432 PB - Royal Society of Chemistry CY - Cambridge AN - OPUS4-29813 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Weber, C. A1 - Stockmann, Jörg M. A1 - Rosier, E. T1 - Corrosion of borosilicate glasses N2 - In contact with aqueous media glass tends to corrode leading to different surface properties. For the precision application this alteration might cause product failure. Hence precise knowledge of the surface interactions is essential. We performed an extensive investigation on the behavior of borosilicate glass under corrosive attack in order to identify critical processes. We identified appropriate investigation methods including sequential chemical analysis, ATR-IR, ellipsometry and SNMS. These techniques allow to identify the influence of specific production processes. KW - Glass corrosion KW - Borosilicate glass KW - SNMS KW - Ellipsometry KW - ATR-IR PY - 2015 UR - http://www.photonik.de/korrosion-von-borosilikatglas/150/21005/317573 SN - 1432-9778 VL - 47 IS - 6 SP - 64 EP - 68 PB - AT-Fachverl. CY - Fellbach AN - OPUS4-35240 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weber, Mike A1 - Völzke, Holger A1 - Zencker, Uwe A1 - Hauer, Katharina A1 - Herz, A. A1 - Kreienmeyer, M. T1 - Aufbau eines Aufprallfundamentes mit reproduzierbaren Eigenschaften für Baumusterprüfungen von Abfallbehältern für das Endlager Konrad N2 - Abgeleitet aus den in Teil 3 der „Systemanalyse Konrad“ definierten Lastannahmen für den „untertägigen Anlagenbereich“ müssen Verpackungen, die der Abfallbehälterklasse I (ABK I) mit dem zusätzlichen Merkmal der störfallfesten (sf) Verpackung oder der ABK II zugeordnet werden, gemäß den „Endlagerungsbedingungen, Endlager Konrad“, nach einem „…Fall aus 5 m Höhe auf eine unnachgiebige Unterlage…“ bestimmten Anforderungen genügen. Eine nähere Beschreibung der Prüfeinrichtung sowie die Definition detaillierter Anforderungen an das Aufprallfundament erfolgen in der „Produktkontrolle, Endlager Konrad“: „Die Prüfeinrichtung, bestehend aus einer Hebeeinrichtung und einem Fundament ist so zu gestalten, dass der Fall des Prüfmusters in jeder beliebigen Aufprallorientierung aus 5 m Höhe, gemessen von der Unterkante des Prüfmusters zum Fundament, möglich ist. Das Fundament ist aus Beton der Mindestgüte B 35 herzustellen und muss so beschaffen und verankert sein, dass keine Zerstörung in zahlreiche kleinere Bruchstücke erfolgt und keine horizontale Verschiebung des Fundamentes oder seiner Teile auftritt. Maße und Masse des Fundaments müssen so beschaffen sein, dass der Einfluss des Baugrundes unter dem Fundament auf den Aufprallwiderstand vernachlässigbar ist.“ Im Rahmen der Bauartprüfung für Behälter zur Endlagerung radioaktiver Abfälle mit zu vernachlässigender Wärmeentwicklung im Endlager Konrad wird die Bundesanstalt für Materialforschung und -prüfung (BAM) von der Bundesgesellschaft für Endlagerung (BGE) als Sachverständige hinzugezogen und ist in der Regel auch mit der Durchführung der notwendigen Fallprüfungen auf dem Testgelände Technische Sicherheit der BAM (BAM TTS) einschließlich der Bereitstellung der benötigten Prüfeinrichtungen sowie des regelkonformen Aufprallfundamentes beauftragt. Der Prozess, beginnend von der Gewährleistung einer von allen Beteiligten als gültig bewerteten Fallprüfung bis hin zur abschließenden Bewertung und Interpretation der Versuchsergebnisse erfordert dabei u.a. eine sorgfältige Planung und Fertigung der für das Endlager Konrad repräsentativen Fundamentplatte und deren Ankopplung an einen Untergrund im Sinne der „Regulations for the Safe Transport of Radioactive Material“ wie er zum Beispiel auf den beiden Fallversuchsanlagen des BAM Testgelände Technische Sicherheit (BAM TTS) zur Verfügung steht. Um diese Anforderungen zu erfüllen muss zum einen der Erhalt der Integrität der Fundamentplatte beim Fallversuch durch eine geeignete Auswahl und kraftflussgerechte Anordnung der Stabstahl-Bewehrung sowie deren Verankerung garantiert und damit eine unzulässige Energieaufnahme durch Risse sowie eine unzulässige „… Zerstörung (der Fundamentplatte) in zahlreiche kleinere Bruchstücke …“, wie in [3] gefordert, verhindert werden. Außerdem ist zu gewährleisten, dass der Beton die Anforderungen an die vorgeschriebene Mindestgüte bzw. -festigkeit zum Zeitpunkt der Fallprüfung erfüllt, die Betonfestigkeit jedoch zur Vermeidung unnötig verschärfter Prüfrandbedingungen eine zu definierende Obergrenze nicht überschreitet. Ausgehend von dem 2009 im Rahmen der KONTEC veröffentlichten Wissensstand präsentiert die BAM im vorliegenden Beitrag die wesentlichen Ergebnisse der zwischenzeitlich bei der Planung und Durchführung von zahlreichen Fallprüfungen gewonnenen Erfahrungen bzgl. Spezifikation und Fertigung der für die Fallversuche notwendigen Fundamentplatten sowie deren Anbindung an den Untergrund. Neben den immer wieder notwendigen Anstrengungen zur Gewährleistung einer im Rahmen der Definition korrekten Betondruckfestigkeit am Tag der Fallprüfung wird die Anpassung der Bewehrungsführung an verschiedene Fallpositionen diskutiert. Zur Ergänzung des gültigen Regelwerks entsteht parallel zu diesem Dokument eine Fachnotiz, in der BGE und BAM die Vorgaben und Spezifikationen zur regelwerkskonformen Herstellung und Montage von Fundamentplatten für Fallprüfungen im Rahmen der Behälterbauartprüfungsverfahren für das Endlager Konrad zusammenfassen und veröffentlichen werden. Diese Fachnotiz soll detaillierte Vorgaben und Spezifikationen zur Planung, Beauftragung, Herstellung und abschließenden Prüfung eines solchen Fundamentes und dessen Anbindung an den Untergrund enthalten. Damit soll allen beteiligten Organisationen wie Antragstellern, Sachverständigen und BGE ein langfristig verlässlicher Leitfaden im Hinblick auf die Durchführung anforderungsgerechter Fallprüfungen unter definierten und reproduzierbaren Randbedingungen im Rahmen der Bauartprüfungsverfahren für das Endlager Konrad an die Hand gegeben werden. T2 - KONTEC 2021 CY - Dresden, Germany DA - 25.08.2021 KW - Aufprallfundament KW - Endlager Konrad KW - Fallprüfung PY - 2021 SP - 1 EP - 10 CY - Dresden AN - OPUS4-53372 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weber, Mike A1 - Völzke, Holger A1 - Zencker, Uwe A1 - Hauer, Katharina A1 - Herz, A. A1 - Kreienmeyer, M. T1 - Aufbau eines Aufprallfundamentes mit reproduzierbaren Eigenschaften für Baumusterprüfungen von Abfallbehältern für das Endlager Konrad N2 - Abgeleitet aus den in Teil 3 der „Systemanalyse Konrad“ [1] definierten Lastannahmen für den „untertägigen Anlagenbereich“ müssen Verpackungen, die der Abfallbehälterklasse I (ABK I) mit dem zusätzlichen Merkmal der störfallfesten (sf) Verpackung oder der ABK II zugeordnet werden, gemäß den „Endlagerungsbedingungen, Endlager Konrad“ [2], nach einem „…Fall aus 5 m Höhe auf eine unnachgiebige Unterlage…“ bestimmten Anforderungen genügen. Eine nähere Beschreibung der Prüfeinrichtung sowie die Definition detaillierter Anforderungen an das Aufprallfundament erfolgen in der „Produktkontrolle, Endlager Konrad“ [3]: „Die Prüfeinrichtung, bestehend aus einer Hebeeinrichtung und einem Fundament ist so zu gestalten, dass der Fall des Prüfmusters in jeder beliebigen Aufprallorientierung aus 5 m Höhe, gemessen von der Unterkante des Prüfmusters zum Fundament, möglich ist. Das Fundament ist aus Beton der Mindestgüte B 35 herzustellen und muss so beschaffen und verankert sein, dass keine Zerstörung in zahlreiche kleinere Bruchstücke erfolgt und keine horizontale Verschiebung des Fundamentes oder seiner Teile auftritt. Maße und Masse des Fundaments müssen so beschaffen sein, dass der Einfluss des Baugrundes unter dem Fundament auf den Aufprallwiderstand vernachlässigbar ist.“ Im Rahmen der Bauartprüfung für Behälter zur Endlagerung radioaktiver Abfälle mit zu vernachlässigender Wärmeentwicklung im Endlager Konrad wird die Bundesanstalt für Materialforschung und -prüfung (BAM) von der Bundesgesellschaft für Endlagerung (BGE) als Sachverständige hinzugezogen und ist in der Regel auch mit der Durchführung der notwendigen Fallprüfungen auf dem Testgelände Technische Sicherheit der BAM (BAM TTS) einschließlich der Bereitstellung der benötigten Prüfeinrichtungen sowie des regelkonformen Aufprallfundamentes beauftragt. Der Prozess, beginnend von der Gewährleistung einer von allen Beteiligten als gültig bewerteten Fallprüfung bis hin zur abschließenden Bewertung und Interpretation der Versuchsergebnisse erfordert dabei u.a. eine sorgfältige Planung und Fertigung der für das Endlager Konrad repräsentativen Fundamentplatte und deren Ankopplung an einen Untergrund im Sinne der „Regulations for the Safe Transport of Radioactive Material“ [4], [5] wie er zum Beispiel auf den beiden Fallversuchsanlagen des BAM Testgelände Technische Sicherheit (BAM TTS) zur Verfügung steht. Um diese Anforderungen zu erfüllen muss zum einen der Erhalt der Integrität der Fundamentplatte beim Fallversuch durch eine geeignete Auswahl und kraftflussgerechte Anordnung der Stabstahl-Bewehrung sowie deren Verankerung garantiert und damit eine unzulässige Energieaufnahme durch Risse sowie eine unzulässige „… Zerstörung (der Fundamentplatte) in zahlreiche kleinere Bruchstücke …“, wie in [3] gefordert, verhindert werden. Außerdem ist zu gewährleisten, dass der Beton die Anforderungen an die vorgeschriebene Mindestgüte bzw. -festigkeit zum Zeitpunkt der Fallprüfung erfüllt, die Betonfestigkeit jedoch zur Vermeidung unnötig verschärfter Prüfrandbedingungen eine zu definierende Obergrenze nicht überschreitet. Ausgehend von dem 2009 im Rahmen der KONTEC veröffentlichten Wissensstand [6] präsentiert die BAM im vorliegenden Beitrag die wesentlichen Ergebnisse der zwischenzeitlich bei der Planung und Durchführung von zahlreichen Fallprüfungen gewonnenen Erfahrungen bzgl. Spezifikation und Fertigung der für die Fallversuche notwendigen Fundamentplatten sowie deren Anbindung an den Untergrund. Neben den immer wieder notwendigen Anstrengungen zur Gewährleistung einer im Rahmen der Definition korrekten Betondruckfestigkeit am Tag der Fallprüfung wird die Anpassung der Bewehrungsführung an verschiedene Fallpositionen diskutiert. Zur Ergänzung des gültigen Regelwerks entsteht parallel zu diesem Dokument eine Fachnotiz, in der BGE und BAM die Vorgaben und Spezifikationen zur regelwerkskonformen Herstellung und Montage von Fundamentplatten für Fallprüfungen im Rahmen der Behälterbauartprüfungsverfahren für das Endlager Konrad zusammenfassen und veröffentlichen werden. Diese Fachnotiz soll detaillierte Vorgaben und Spezifikationen zur Planung, Beauftragung, Herstellung und abschließenden Prüfung eines solchen Fundamentes und dessen Anbindung an den Untergrund enthalten. Damit soll allen beteiligten Organisationen wie Antragstellern, Sachverständigen und BGE ein langfristig verlässlicher Leitfaden im Hinblick auf die Durchführung anforderungsgerechter Fallprüfungen unter definierten und reproduzierbaren Randbedingungen im Rahmen der Bauartprüfungsverfahren für das Endlager Konrad an die Hand gegeben werden. T2 - KONTEC 2021 CY - Dresden, Germany DA - 25.08.2021 KW - Endlager Konrad KW - Fallprüfung KW - Aufprallfundament PY - 2021 AN - OPUS4-53374 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Emmerling, Franziska A1 - Chewle, S. A1 - Weber, M. T1 - Revealing Kinetics of Paracetamol Crystallization Using Time Resolved Raman Spectroscopy, Orthogonal Time-Lapse Photography, and Non-Negative Matrix Factorization (OSANO) N2 - Crystallization is a complex phenomenon with farreaching implications for the production and formulation of active pharmaceutical ingredients. Understanding this process is critical for achieving control over key physicochemical properties that can affect, for example, the bioavailability and stability of a drug. In this study, we were able to reveal intricate and diverse dynamics of the formation of metastable intermediates of paracetamol crystallization varying with the choice of solvent. We demonstrate the efficacy of our novel approach utilizing an objective function-based non-negative matrix factorization technique for the analysis of time-resolved Raman spectroscopy data, in conjunction with time-lapse photography. Furthermore, we emphasize the crucial importance of integrating Raman spectroscopy with supplementary experimental instrumentation for the mathematical analysis of the obtained spectra. KW - Polymorphism KW - Crystallization KW - Measurement KW - Algorithm PY - 2023 DO - https://doi.org/10.1021/acs.cgd.3c00617 SN - 1528-7483 VL - 23 SP - 6737 EP - 6746 PB - ACS Publications AN - OPUS4-58193 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Weber, Mike A1 - Völzke, Holger A1 - Zencker, Uwe A1 - Herz, A. A1 - Kreienmeyer, M. T1 - Design of a Drop Test Target with Reproducible Properties for Konrad Prototype Testing N2 - Beginning in 1976 the former iron ore mine Konrad was geologically investigated concerning its suitability as a location for a German final repository for low and intermediate level waste. After a comprehensive licensing procedure it was approved and is now being prepared and equipped for the planned start of storage in 2027. At the end of the 1980s, the requirements for waste containers for storage in this repository were defined for the first time on the basis of an incident analysis of the on-site handling procedures, beginning with the unloading of the packages after the arrival at the site up to the final positioning in the underground storage galleries. A 5-meter drop onto the rock ground of the mine was identified as the covering case for high mechanical requirements (ABK II container class). In contrast to the 9-meter drop according to the IAEA Regulations for the Safe Transport of Radioactive Material, the 5-meter drop is performed onto a hard but not essentially unyielding target. The container is typically not protected by an impact limiter. The requirements for a potential test facility are described in the regulations for the Konrad repository. The mechanical strength of the target is defined as a concrete strength equivalent to the identified properties of the rock ground of the mine. Since 1991 BAM has consistently used precast reinforced concrete slabs as target for drop tests in the framework of licensing procedures as well as in research projects. While the original design fulfilled the requirement for the integrity of the concrete slab in most cases, it failed when drop tests onto an edge of a container were performed. A redesigned concrete slab developed in a research project and suggested as a reference target in 2009 has been successfully used in Konrad licensing procedures since then. The paper gives a brief overview of the historical development and it describes BAM’s efforts and approaches to continuously guarantee a concrete slab of defined quality and to provide a test setup for valid drop tests from the applicants and the authorities view. T2 - PATRAM 2022, 20th International Symposium on the Packaging and Transportation of Radioactive Materials CY - Juan-les-Pins, France DA - 11.06.2023 KW - Target KW - Drop test KW - Final repository Konrad PY - 2023 SP - 1 EP - 11 AN - OPUS4-58563 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Sechi, R. A1 - Fackeldey, K. A1 - Chewle, Surahit A1 - Weber, M. T1 - SepFree NMF: A toolbox for analyzing the kinetics of sequential spectroscopic data N2 - This work addresses the problem of determining the number of components from sequential spectroscopic data analyzed by non-negative matrix factorization without separability assumption (SepFree NMF). These data are stored in a matrix M of dimension “measured times” versus “measured wavenumbers” and can be decomposed to obtain the spectral fingerprints of the states and their evolution over time. SepFree NMF assumes a memoryless (Markovian) process to underline the dynamics and decomposes M so that M = WH, with W representing the components’ fingerprints and H their kinetics. However, the rank of this decomposition (i.e., the number of physical states in the process) has to be guessed from pre-existing knowledge on the observed process. We propose a measure for determining the number of components with the computation of the minimal memory effect resulting from the decomposition; by quantifying how much the obtained factorization is deviating from the Markovian property, we are able to score factorizations of a different number of components. In this way, we estimate the number of different entities which contribute to the observed system, and we can extract kinetic information without knowing the characteristic spectra of the single components. This manuscript provides the mathematical background as well as an analysis of computer generated and experimental sequentially measured Raman spectra. KW - Kinetics from experiments KW - Separability assumption KW - Sequential spectroscopic data PY - 2022 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559046 DO - https://doi.org/10.3390/a15090297 SN - 1999-4893 VL - 15 IS - 9 SP - 1 EP - 16 PB - MDPI CY - Basel AN - OPUS4-55904 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fackeldey, K. A1 - Röhm, J. A1 - Niknejad, A. A1 - Chewle, Surahit A1 - Weber, M. T1 - Analyzing Raman spectral data without separabiliy assumption N2 - Raman spectroscopy is a well established tool for the analysis of vibration spectra, which then allow for the determination of individual substances in a chemical sample, or for their phase transitions. In the time-resolved-Raman-sprectroscopy the vibration spectra of a chemical sample are recorded sequentially over a time interval, such that conclusions for intermediate products (transients) can be drawn within a chemical process. The observed data-matrix M from a Raman spectroscopy can be regarded as a matrix product of two unknown matrices W and H, where the first is representing the contribution of the spectra and the latter represents the chemical spectra. One approach for obtaining W and H is the non-negative matrix factorization. We propose a novel approach, which does not need the commonly used separability assumption. The performance of this approach is shown on a real world chemical example. KW - Non-negative matrix factorization KW - NMF KW - Raman spectra KW - Separability condition KW - PCCA+ PY - 2021 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-559051 DO - https://doi.org/10.1007/s10910-020-01201-7 SN - 1572-8897 VL - 59 SP - 575 EP - 596 PB - Springer Science + Business Media CY - Dordrecht AN - OPUS4-55905 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Wolff, M. A1 - Wonneberger, R. A1 - Freiberg, K.E. A1 - Hertwig, Andreas A1 - Bonse, Jörn A1 - Giebeler, L. A1 - Koitzsch, A. A1 - Kunz, C. A1 - Weber, H. A1 - Hufenbach, J.K. A1 - Müller, F.A. A1 - Gräf, S. T1 - Formation of laser-induced periodic surface structures on Zr-based bulk metallic glasses with different chemical composition N2 - Bulk metallic glasses (BMG) are amorphous metal alloys known for their unique physical and mechanical properties. In the present study, the formation of femtosecond (fs) laser-induced periodic surface structures (LIPSS) on the Zr-based BMGs Zr46Cu46Al8, Zr61Cu25Al12Ti2, Zr52.5Cu17.9Al10Ni14.6Ti5 (Vit105) and Zr57Cu15.4Al10Ni12.6Nb5 (Vit106) was investigated as a function of their different chemical composition. For this purpose, LIPSS were generated on the sample surfaces in an air environment by fs-laser irradiation (λ = 1025 nm, τ = 300 fs, frep = 100 kHz). The surface topography was characterized by scanning electron microscopy and atomic force microscopy. Moreover, the impact of LIPSS formation on the structure and chemical surface composition was analyzed before and after fs-laser irradiation by X-ray diffraction and X-ray photoelectron spectroscopy as well as by transmission electron microscopy in combination with energy dispersive X-ray spectroscopy. Despite the different chemical composition of the investigated BMGs, the fs-laser irradiation resulted in almost similar properties of the generated LIPSS patterns. In the case of Zr61Cu25Al12Ti2, Vit105 and Vit106, the surface analysis revealed the preservation of the amorphous state of the materials during fs-laser irradiation. The study demonstrated the presence of a native oxide layer on all pristine BMGs. In addition, fs-laser irradiation results in the formation of laser-induced oxide layers of larger thickness consisting of an amorphous ZrAlCu-oxide. The precise laser-structuring of BMG surfaces on the nanoscale provides a versatile alternative to thermoplastic forming of BMG surfaces and is of particular interest for the engineering of functional material surfaces. KW - Bulk metallic glasses KW - Femtosecond laser KW - Laser-induced periodic surface structures (LIPSS) KW - Chemical analysis KW - Oxidation PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-581799 DO - https://doi.org/10.1016/j.surfin.2023.103305 SN - 2468-0230 VL - 42 SP - 1 EP - 11 PB - Elsevier B.V. AN - OPUS4-58179 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Scharkoi, O. A1 - Becker, Roland A1 - Esslinger, Susanne A1 - Weber, M. A1 - Nehls, Irene T1 - Predicting sites of cytochrome P450-mediated hydroxylation applied to CYP3A4 and hexabromocyclododecane N2 - This article describes a simple and quick in silico method for the prediction of cytochrome P450 (CYP)-mediated hydroxylation of drug-like compounds. Testosterone and progesterone, two known substrates of CYP3A4, are used to test the method. Further, we apply the procedure to predict sites of hydroxylation of isomers of the flame retardant hexabromocyclododecane by CYP3A4. Within the method, the compound is rotated in the binding pocket of the cytochrome, so that each hydrogen under consideration is placed near the active centre. Afterwards, short molecular dynamics simulations are provided for each step of the rotation. All steps of the simulation are compared concerning the distances between the hydrogens and the active centre and the corresponding energies. The computational results correlate well with experimental results. KW - Predicting sites of metabolism KW - Cytochrome P450 KW - Hydroxylation KW - Metabolism of HBCD PY - 2015 DO - https://doi.org/10.1080/08927022.2014.898845 SN - 0892-7022 SN - 1029-0435 VL - 41 IS - 7 SP - 538 EP - 546 PB - Gordon and Breach CY - New York, NY AN - OPUS4-30492 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Wittig, Günther A1 - Beller, M. A1 - Leider, A. A1 - Stumm, W. A1 - Weber, H. P. T1 - Application of Reference Standards for Control of Eddy-Current Test Equipment T2 - Symposium on Eddy-Current Characterization of Materials and Structures CY - Gaithersburg, MD, USA DA - 1979-09-05 PY - 1981 N1 - Serientitel: ASTM special technical publication – Series title: ASTM special technical publication IS - 722 SP - 79 EP - 85 PB - ASTM CY - Philadelphia, PA, USA AN - OPUS4-33329 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -