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MALDI TOF Massenspektrometrie wurde verwendet, um Kristallisationsprozesse in Polyestern (Polylactide, Polyglycolide) zu untersuchen. Dabei konnte gezeigt werden, dass Zyklen und Linearen simultan, aber in unterschiedlichen Kristalliten, kristallisieren. Die dabei ablaufenden Umesterungen (Transesterifizierungen) konnten mit der MALDI TOF Massenspektrometrie nachgewiesen werden. Damit wurde ein völlig neues Anwendungsgebiet dieser MS Methode demonstriert.
An Amorphous Lewis-acidic Zirconium Chlorofluoride as HF Shuttle: C-F Bond Activation and Formation
(2024)
In recent years, fluorine chemistry has gained increasing political attention. Owing to a growing shortage of fluorspar, a raw material used for producing fluorinated base chemicals, fluorospar has been named among the 30 critical raw materials in the EU.2 As such, it becomes increasingly important to recycle existing fluorinated compounds and make them available as sources of fluorine for reactions. Significant progress has been made in the field of C-F bond activation using heterogeneous catalysts such as aluminum chlorofluoride (ACF).3–5 However, the transfer of fluorine atoms from one molecule to another using heterogeneous catalysts has not yet been reported. In this study, we successfully synthesized amorphous zirconium chlorofluoride (ZCF), and we were able to establish a catalytic behavior of ZCF in C-F bond activation reactions. We present a heterogeneous catalyst that performs dehydrofluorination of a fluoroalkane and consecutive hydrofluorination of an alkyne at room temperature.
Microplastic reference material is required for validation and harmonization purposes. This includes the analysis of the pure polymer particles and the validation of the respective measurement methods. In addition, there is the harmonization of different laboratories. On the other hand, sample preparation methods must be validated and harmonized with regard to their recovery and subsequent analysis in the respective matrices. For this purpose, we produce reference material candidates in the form of tablets with different mass fractions and particle numbers of polyethelene terephthalate. In the presentation first measurement results by µ-Raman, µ-FTIR, pyrolysis-GC-MS and TED-GC/MS will be presented.
Im Rahmen des Vortrags wurden die Ergebnisse und die Methodik zur Erhebung von Forschungsbedarfen und Fähigkeitslücken bei den Behörden und Organisationen mit Sicherheitsaufgaben, welche im Rahmen des Projektes InnoBOSK durchgeführt wurden, vorgestellt. Den Schwerpunkt bildete dabei die Umsetzung der Workshops gemeinsam mit den Einsatzkräften und die Umsetzung der problemorientierten Erhebungsmethodik.
This study explores the acceleration of material design in the concrete industry, focusing on improving carbonation resistance, a key factor in the durability of concrete structures. Traditional tests for carbonation resistance are lengthy, but with the construction industry aiming for sustainable production, finding a balance between carbonation resistance and CO2 footprint is crucial. Our research employs two innovative methods: 1. Applying the Sequential Learning App for Materials Discovery (SLAMD), an AI materials design framework, to an extensive dataset of real-world concrete compositions to selectively test materials that meet market demands: maximum durability, optimal eco-durability, and the best cost-durability trade-off. 2. Investigating 1H Nuclear Magnetic Resonance (NMR) relaxometry as a quick alternative for characterizing carbonation behavior, as it saves time compared to traditional tests and assesses the complete material's pore space. Specific NMR features are then integrated into the material design model, with the model's performance compared against traditional approaches. The results of our study are compelling, demonstrating that materials can be precisely tailored to meet specific requirements with minimal data points. This marks a significant stride in the concrete industry, indicating that NMR-based, low-fidelity surrogate characterizations, combined with a focused, data-driven design approach, can substantially accelerate the development of durable, sustainable concrete mixtures.
In recent years, many protocols in computational materials science have been automated and made available within software packages (primarily Python-based). This ranges from the automation of simple heuristics (oxidation states, coordination environments) to the automation of protocols, including multiple DFT and post-processing tools such as (an)harmonic phonon computations or bonding analysis. Such developments also shorten the time frames of projects after such developments have been made available and open new possibilities. For example, we can now easily make data-driven tests of well-known rules and heuristics or develop quantum chemistry-based materials descriptors for machine learning approaches. These tests and descriptors can have applications related to magnetic ground state predictions of materials relevant for spintronic applications or for predicting thermal properties relevant for thermal management in electronics. Combining high-throughput ab initio computations with fitting, fine-tuning machine learning models and predictions of such models within complex workflows is also possible and promises further acceleration in the field. In this talk, I will show our latest efforts to link automation with data-driven chemistry and materials science.
This study aims to represent an approach for transferring the materials testing datasets to the digital schema that meets the prerequisites of the semantic web. As a use case, the tensile stress relaxation testing method was evaluated and the testing datasets for several copper alloys were prepared. The tensile stress relaxation testing ontology (TSRTO) was modeled following the test standard requirements and by utilizing the appropriate upper-level ontologies. Eventually, mapping the testing datasets into the knowledge graph and converting the data-mapped graphs to the machine-readable Resource Description Framework (RDF) schema led to the preparation of the digital version of testing data which can be efficiently queried on the web.
The presentation gives an overview of BAM's activities on processing influences and application properties of MPEAs in the form of joined and machined high and medium entropy alloys (CoCrFeMnNi and CoCrNi). In the case of welding, the focus is on defect-free welded joints with sufficient mechanical properties. In the case of machining, the focus is on the possible influence on the surface quality of the materials through adequate milling parameters. In addition, the hydrogen absorption and diffusion properties as well as the electrochemical corrosion behavior are fundamentally examined.
The heat-resistant cast iron EN-GJSA-XNiSiCr35-5-2 (Ni-Resist D-5S) was investigated for its fatigue crack growth behavior at room and high temperatures. Force-controlled tests were carried out at constant temperatures (20 °C, 500 °C, 700 °C) without and with hold time and different load ratios. The crack growth behavior was also characterized under TMF loading (Tmin = 400 °C, Tmax = 700 °C) by applying IP and OP conditions and different load ratios. Three different techniques were combined to monitor crack growth: potential drop, thermography, and compliance method. The effect of the different loading conditions on the fatigue crack growth behavior will be presented and discussed.
Ground Granulated Blast-Furnace Slag (GGBFS), a by-product of the iron-making process, has gained significant attention as a supplementary cementitious material and has become increasingly popular in recent years due to its remarkable properties. GGBFS can significantly reduce the environmental impact of cement production when it comes to building concrete structures. GGBFS can either be blended with ordinary Portland cement (OPC) (up to a 90% replacement), or it can be used in the production of alkali-activated materials (AAMs). However, a comprehensive understanding of the pore solution composition is necessary for understanding various aspects of cementitious materials and their durability, including corrosion behavior, passivation of steel, and resistance to deteriorative processes. In the present work, the pore solutions of seven different GGBFS-containing cements (alkali-activated slag, alkali-activated slag/fly ash blends, a hybrid alkaline cement, CEM III/C, and CEM III/B) were extracted and analysed by inductively coupled plasma-optical emission spectroscopy, ion chromatography, pH, redox potential, and conductivity measurements. For comparison, a Portland cement pore solution was analysed similarly. The Concentrations of reduced sulfur were noteworthy in all GGBFS-containing cements, particularly in alkali-activated cements, where concentrations were notably higher compared to standard cements. The redox potentials of the pore solutions were primarily dictated by the concentrations of reduced sulfur, although other factors may contribute. Additionally, sulfur species in the pore solutions had an impact on pH, electrical conductivity, and other properties pertinent to the corrosion of reinforcements.