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The choice of solvents influences crystalline solid formed during the crystallization of active pharmaceutical ingredients (API). The underlying effects are not always well understood because of the complexity of the systems. Theoretical models are often insufficient to describe this phenomenon. In this study, the crystallization behavior of the model drug paracetamol in different solvents was studied based on experimental and molecular dynamics data. The crystallization process was followed in situ using time-resolved Raman spectroscopy. Molecular dynamics with simulated annealing algorithm was used for an atomistic understanding of the underlying processes. The experimental and theoretical data indicate that paracetamol molecules adopt a particular geometry in a given solvent predefining the crystallization of certain polymorphs
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.
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.
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.
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.
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.
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.
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.
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.