TY - CONF A1 - Emmerling, Franziska T1 - May the force be with you - in situ investigation of mechanochemical reactions N2 - The past decade has seen a reawakening of solid-state to chemical synthesis, driven by the search for new, cleaner synthetic methodologies. Mechanochemistry has advanced to a widely applicable technique. T2 - SALSA's "Make and Measure 2019 CY - Berlin, Germany DA - 25.10.2019 KW - Mechanochemistry KW - Metal–organic frameworks PY - 2019 AN - OPUS4-50138 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, Ulrike T1 - Detektion von Mikroplastik in Flaschenwasser mittels thermoanalytischer Verfahren N2 - Im Vortrag wird ein Messfiltertiegel als Zusatztool für die TED-GC/MS vorgestellt, welcher für die Probenaufbereitung von kleinen Partikelfrachten oder kleinen Partikelgrößen genutzt werden kann. Er ist Filtereinheit und Messtiegel in einem, wodurch Verluste bei der Überführung der Probe in das Messgefäß sowie Kontaminationen vermindert werden. Das beispiel ist hier die Filtration von Flaschenwasser mit anschließender Detektion mit der TED-GC/MS. T2 - BVL_Kick-off Meeting "Mikroplastik in Lebensmitteln" CY - Online meeting DA - 03.12.2020 KW - Mikroplastik KW - TED-GC/MS KW - Kleine Partikel KW - Geringe Partikelfrachten KW - Mikroplastik-Massengehalte PY - 2020 AN - OPUS4-51794 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Mechanochemistrry - a time resolved perspective on unconventional crystallization N2 - Green chemsistry apporoach for the synthesis of metal organic frameworks. T2 - IFW BAM Workshop CY - Berlin, Germany DA - 25.11.2019 KW - Mechanochemistry KW - XRD KW - Metal-organic-frameworks PY - 2019 AN - OPUS4-50110 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Heilmann, Maria T1 - Synthesis of bimetallic nickel nanoparticles for catalysis N2 - We present the synthesis of monodisperse monometallic Ni nanoparticles (NPs) and bimetallic NiCu respectively NiCo NPs. The NPs were investigated using SAXS, STEM, EDX, and XANES, showing that the NPs are size tunable and stable while the surface is not entirely covered. Nickel NPs have exhibited immense potential as important catalyst for the Sabatier reaction, i.e. converting waste to energy via transformation of CO2 into CH4. T2 - 11th Joint BER II and BESSY II User Meeting CY - Berlin, Germany DA - 04.12.2019 KW - Nanoparticles KW - Catalysis KW - Synthesis PY - 2019 AN - OPUS4-50172 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Altmann, Korinna A1 - Braun, U. A1 - Herper, D. A1 - Knefel, M. A1 - Bednarz, M. A1 - Bannick, C.-G. T1 - Smart filters for the analysis of microplastic in beverages filled in plastic bottles N2 - The occurrence of microplastic (MP) in food products, such as beverages in plastic bottles, is of high public concern. Existing analytical methods focus on the determination of particle numbers, requiring elaborate sampling tools, laboratory infrastructure and generally time-consuming imaging detection methods. A comprehensive routine analysis of MP in food products is still not possible. In the present work, we present the development of a smart filter crucible as sampling and detection tool. After filtration and drying of the filtered-off solids, a direct determination of the MP mass content from the crucible sample can be done by thermal extraction desorption gas chromatography mass spectroscopy (TED-GC/MS). The new filter crucible allows a filtration of MP down to particle sizes of 5 µm. We determined MP contents below 0.01 µg/L up to 2 µg/L, depending on beverages bottle type. This may be directly related to the bottle type, especially the quality of the plastic material of the screw cap. Dependent on the plastic material, particle formation increases due to opening and closing operations during the use phase. However, we have also found that some individual determinations of samples were subjected to high errors due to random events. A conclusive quantitative evaluation of the products is therefore not possible at present. KW - Microplastic KW - TED-GC/MS KW - Plastic bottles KW - Bbeverages KW - Filter crucible PY - 2021 DO - https://doi.org/10.1080/19440049.2021.1889042 SN - 1944-0057 VL - 38 IS - 4 SP - 691 EP - 700 PB - Taylor & Francis AN - OPUS4-52323 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Repräsentative Untersuchungsstrategien für ein integratives Systemverständnis von spezifischen Einträgen von Kunststoffen in die Umwelt (RUSEKU) N2 - Der Vortrag wurde im Rahmen der Abschlusskonferenz des Forschungsschwerpunktes "Plastik in der Umwelt" des BMBF gehalten. Er fasst die Ergebnisse des Verbundprojektes RUSEKU zusammen. Es wurde die Herstellung verschiedener Testmaterialien für die Mikroplastik (MP) Analytik beschrieben. Im weiteren geht es um verschiedene Ansätze MP kostengünstig und schnell zu detektieren, z.B. mit Nahinfrarotspektroskopie. Nanoplastik konnte mit der Transmissionselektronenmikroskopie sichtbar gemacht werden. Für die praxisnahe Beprobung von Gewässern wurde die Fraktionierte Filtration entwickelt. Integrale Beprobungen können mit dem Sedimentationskasten erfolgen. Als Beispiele für die Beprobung realer Gewässer wurde das urbane Abwassersystem Kaiserslautern, Getränkewasser und Waschmaschinenwasser gezeigt. T2 - Abschlusskonferenz des Forschungsschwerpunktes "Plastik in der Umwelt" des BMBF CY - Online meeting DA - 20.04.2021 KW - Mikroplastik KW - TED-GC/MS KW - Probennahme KW - RUSEKU PY - 2021 AN - OPUS4-52546 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Mikroplastik an der BAM: TED-GC/MS und Referenzmaterialien N2 - Thema ist die Funktionsweise der TED-GC/MS als Methode für die Mikroplastik-Detektion sowie die Herstellung dazugehöriger Referenzmaterialien an der BAM T2 - 25. Kolloquium Massenspektrometrie von Polymeren CY - Online meeting DA - 17.06.2021 KW - Mikroplastik KW - TED-GC/MS KW - Referenzmaterial PY - 2021 AN - OPUS4-52835 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Results of the Plastic in the environment comparative test N2 - The talk describes the sturcture and the results of the "plastics in the environment" comparative test of 2019. T2 - Symposium "Challenges of microplastic analysis – Bridging state of the art and policy needs” CY - Online meeting DA - 09.09.2021 KW - Microplastic KW - Comparative test KW - ILC PY - 2021 AN - OPUS4-53236 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Dittmann, Daniel T1 - Aktivkohle-Charakterisierung als weiterer Schlüssel für das Verständnis der Spurenstoffadsorption in der 4. Reinigungsstufe N2 - Aktivkohle ≠ Aktivkohle, Adäquate Materialcharakterisierung - Voraussetzung für Adsorptionsprognosen und Wasserspezifische Auswahl von Aktivkohleprodukten. Ausblick: Publikationen zu Aktivkohlecharakterisierung und Adsorptionsprognose in Vorbereitung T2 - Wasser 2021 - Jahrestagung der Wasserchemischen Gesellschaft CY - Online meeting DA - 10.05.2021 KW - Aktivkohle KW - Thermogravimetrie KW - Zersetzungsgasanalyse KW - Proximatanalyse PY - 2021 AN - OPUS4-52742 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Linberg, Kevin T1 - Insights into Mechanochemical Reactions using High Pressure XRD and DFT Simulations N2 - The reactivity of organic solids under mechanochemical conditions remains very little understood, though many processes have been found empirically. Importantly, it is not well understood how mechanical treatment induces experimentally observed chemical transformations, and if the elevated pressures arising at the point of impact can play a role in the transformation. To understand this aspect of the mechanochemical reactions, the same compounds need to be explored under high pressure conditions. As a model system, we considered the reaction between the bis(4-chlorophenyl) disulfide and bis(2-nitrophenyl) disulfide. A powder mixture of these two compounds is known to undergo a disulfide exchange reaction under ball milling conditions. Using a combination of X-ray powder diffraction and dispersion-corrected density functional theory calculations, we investigated how this binary solid system behaves at elevated pressures and whether pressure alone can explain its mechanochemical reactivity. T2 - International Scientific Student Conference 2021 CY - Online meeting DA - 12.04.2021 KW - Mechanochemistry KW - High Pressure KW - Density-functional theory PY - 2021 AN - OPUS4-52494 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Lakshmipathi, M. A1 - Emmerling, Franziska A1 - Bhattacharya, Biswajit A1 - Ghosh, S. T1 - Structure-mechanical property correlation of a series of 4-(1-Napthylvinyl) pyridine based cocrystals N2 - We obtained three 4-(1-Napthylvinyl) pyridine based cocrystals ( 1–3 ) and studied its structure mechan- ical property correlation which aimed towards various applications for photo switches, mechanical ac- tuators etc. Selection of coformer molecules is important in fine tuning mechanical property outcome of synthesized cocrystals. Amongst three cocrystals, cocrystal 1 is mechanically flexible and its mechani- cal property is attributed to underlying crystal packing features which is in line with existing elastically bendable crystals while other two cocrystals ( 2, 3 ) are brittle in nature. Hirshfeld analysis was carried out to illustrate structure-property correlation particularly in terms of number as well as types of non- covalent interactions in the lattice and further to corroborate the space of the molecules in the lattice. KW - Cocrystals KW - Mechanical properties KW - Halogen bond interaction KW - Structure-mechanical property correlation PY - 2022 DO - https://doi.org/10.1016/j.molstruc.2022.133670 SN - 0022-2860 VL - 1268 SP - 1 EP - 16 PB - Elsevier CY - Amsterdam AN - OPUS4-55547 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Waniek, Tassilo T1 - The practical implementation of MP reference material production according to ISO standards N2 - Micro- and nanoplastic particles became a topic of public concern all over the world e.g. in water, soil, sludge and air. For a profound risk assessment, it is necessary to identify the origins, hotspots, or transport between different media. Therefore, a representative repeatable analysis is required and reference materials (RM) to proof and compare methods. The basis of MNP investigations is a harmonized analysis which includes sampling, sample preparation and detection. In recent years, spectroscopic methods like µRaman and µFTIR for the determination of particle numbers or thermoanalytical methods like Pyrolysis gas chromatography/mass spectrometry (py-GC/MS) and Thermo extraction/ desorption gas chromatography / mass spectrometry (TED-GC/MS) for mass determination have proven to be particularly suitable. The technical committees (TC) of ISO TC 61 “plastics” and TC 147 “water quality" are working on harmonisation processes on international level. For all standardization approaches, it is necessary that the detection methods and analysis processes can be validated. Therefore, BAM develops reference material for microplastic (MP) analysis for several years with focus on the most common polymers PE, PP, PS, PET and PA. MP particles with a close to reality fragment shape are obtained by cryomilling and sieving. For sample preparation purposes with mass detection methods MP particles are pressed into pills with a water-soluble matrix. Thereby losses due to sample preparation e.g. filtration are included in the verification of an analysis. To ensure a constant quality throughout all MP RM batches the homogeneity and stability is controlled according to ISO Guide 35. Next to TED-GC/MS measurements particle size distribution, infrared spectroscopy and differential scanning calorimetry spectra are taken as accompanying parameters. This presentation aims to introduce into the MP RM production process with ensured quality and special focus on pointing out customized setups for particle comminution, separation, and characterization for standardization. T2 - ASTM Syposioum on Microplastic Analytical and Reference Standards - Opportunities to Advance Microplastic Science CY - Seattle, WA, USA DA - 30.06.2022 KW - Microplastic KW - Reference material KW - Cryo milling KW - Polymer PY - 2022 AN - OPUS4-55891 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Cocrystal polymorphs & Mechanochemistry - Mechanism & Kinetics N2 - Mechanochemistry is an effective, environmentally benign, and facile method for the synthesis of new crystal forms. Different milling parameters are known to affect the mechanisms and rates of product formation: milling frequency, milling time, filling degree of the milling jar, ball diameter and vessel size, degree of milling ball filling, and material of jars. The increasing interest in mechanochemistry is contrasted by a limited mechanistic understanding of mechanochemical reactivity and selectivity. Control over ball milling transformations is needed before the transformative potential of mechanochemical processing can be realized. Different analytical methods and their combinations have been developed for the time-resolved in situ monitoring of mechanochemical transformations, including powder X-ray diffraction, X-ray absorption spectroscopy, NMR, Raman spectroscopy, and thermography. Here we will discuss our recent results investigating the formation of polymorphic cocrystals thereby elucidating the influence of milling parameters (solvent, temperature, time) and reaction sequences on the formation mechanism and kinetics. For the mechanochemical chlorination reaction of hydantoin normalizing the kinetic profiles to the volume of the milling ball showed clearly that milling reaction kinetics are conserved. Here physical kinetics dominate reaction rates in a ball-milling transformation. Attempting to interpret such kinetics in purely chemical terms risk misinterpreting the results. Our results indicate that time-resolved in situ investigations of milling reactions offer a new approach to tune and optimize mechanochemical processes. T2 - 33th European Crrystallography Meeting CY - Versailles, France DA - 23.08.2022 KW - Mechanochemistry KW - Cocrystals KW - Kinetics KW - Polymorphs PY - 2022 AN - OPUS4-55586 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, U. T1 - Detection of plastics in soil N2 - Soil acts as a final sink for pollutants. Microplastics from different sources such as plastic mulching, littering, compost, sewage sludge, sedimentary deposition, and tyre abrasion are expected to be found in soil. However, representative and comprehensive information is missing on the sources, transport, and fate. Therefore, a reliable analysis method for microplastics in soils needs to be developed. The presented work describes the development of a procedure for microplastics analysis in soils. A representative sampling based on the on-site conditions and a sample preparation method was established and comprised of a drying step, the separation of microplastic particles > 1 mm, and a density separation for particles < 1 mm. The detection of the large microplastic particles (> 1 mm) was conducted with Attenuated Total Reflection - Fourier Transform infrared Spectroscopy (ATR-FTIR) , while Thermal Extraction Desorption - Gas Chromatography / Mass Spectrometry (TED-GC/MS) was applied for particles < 1 mm, gaining information on the type of polymer and mass fraction. Based on the established method, 14 environmental soil samples ? with different exposure of microplastics from agriculture, industrial sites, roads, and floods were investigated. Due to the arbitrary microplastic particle distribution among the samples for large microplastics, it was reasoned that the found particles were unrepresentative. In contrast, microplastic particles < 1 mm were discovered in a high mass in soil samples exposed to plastic mulching or fertilization with sewage sludge or compost (0 – 115 mg/kg). On average, microplastic contents detected in soil samples taken from a construction site and an inner-city lake were higher (13 – 238 mg/kg). As expected, microplastic content in soil sampled in proximity to roads was more pronounced in the upper soil layers. In contrast, very remote sampling sites, expectably uncontaminated, did not lead to the detection of microplastic regarding to thermoanalytical detection method. In a proof of concept experiment several in vivo and in vitro ecotoxicological tests were applied to evaluate the effect of microplastics (tyre abrasion, polystyrene containing hexabromocyclododecane) in natural soils. In summary, while no effects of the examined probes could be detected on higher levels of biological organization after exposures to earthworm E. andrei, significant changes in several oxidative stress related biomarkers were observed. T2 - SETAC Europe 2022 CY - Kopenhagen, Denmark DA - 15.05.2022 KW - Microplastic KW - TED-GC/MS KW - Soil PY - 2022 AN - OPUS4-55872 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - Cocrystal polymorphs & Mechanochemistry - Mechanism & Kinetics N2 - Mechanochemistry is an effective, environmentally benign, and facile method for the synthesis of new crystal forms. Different milling parameters are known to affect the mechanisms and rates of product formation: milling frequency, milling time, filling degree of the milling jar, ball diameter and vessel size, degree of milling ball filling, and material of jars. The increasing interest in mechanochemistry is contrasted by a limited mechanistic understanding of mechanochemical reactivity and selectivity. Control over ball milling transformations is needed before the transformative potential of mechanochemical processing can be realized. Different analytical methods and their combinations have been developed for the time-resolved in situ monitoring of mechanochemical transformations, including powder X-ray diffraction, X-ray absorption spectroscopy, NMR, Raman spectroscopy, and thermography. Here we will discuss our recent results investigating the formation of polymorphic cocrystals thereby elucidating the influence of milling parameters (solvent, temperature, time) and reaction sequences on the formation mechanism and kinetics. For the mechanochemical chlorination reaction of hydantoin normalizing the kinetic profiles to the volume of the milling ball showed clearly that milling reaction kinetics are conserved. Here physical kinetics dominate reaction rates in a ball-milling transformation. Attempting to interpret such kinetics in purely chemical terms risk misinterpreting the results. Our results indicate that time-resolved in situ investigations of milling reactions offer a new approach to tune and optimize mechanochemical processes. T2 - 3rd CEFMC meeting CY - Kashmir, India DA - 31.08.2022 KW - Mechanochemistry KW - Crystal Engeneering PY - 2022 AN - OPUS4-55641 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Altmann, Korinna T1 - Harmonisation efforts of the CUSP projects N2 - The talk is about harmonisation approaches within CUSP. First the five H2020 projects for research on risk assessment regarding microplastics topic were presented. Secondly, harmonisation process were discussed. T2 - VAMAS SC 47 Meeting CY - Turin, Italy DA - 19.10.2022 KW - Microplastics KW - Harmonisation KW - Nanoplastics KW - H2020 KW - Risk assessment PY - 2022 AN - OPUS4-56077 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Braun, U. T1 - Analysis of Microplastics in Soil: Harmonisation and Standardisation - a first approach N2 - The talk is about microplastics in soil. Some results were presented with mainly state of the art according to microplastics in standardization. T2 - International Conference Microplastics in Soils CY - Berlin, Germany DA - 19.10.2022 KW - Microplastics KW - Microplastics standardisation KW - Microplastics in soil PY - 2022 AN - OPUS4-56078 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Fischer, Franziska A1 - Heidrich, Adrian A1 - Greiser, Sebastian A1 - Benemann, Sigrid A1 - Rademann, K. A1 - Emmerling, Franziska T1 - Polymorphism of mechanochemically synthesized cocrystals: a case study N2 - The liquid-assisted grinding cocrystallisation of theophylline with benzamide leading to polymorphic compounds was investigated. A solvent screening with seventeen different solvents was performed. The dipole moment of the solvent used in the synthesis determines the structure of the polymorphic product. A detailed investigation leads to the determination of the kinetically and thermodynamically favored product. In situ observations of the formation pathway during the grinding process of both polymorphs show that the thermodynamically favored cocrystal is formed in a two-step mechanism with the kinetic cocrystal as intermediate. KW - cocrystal KW - mechanochemistry KW - theophylline KW - benzamide KW - milling KW - polymorphism PY - 2016 DO - https://doi.org/10.1021/acs.cgd.5b01776 SN - 1528-7483 SN - 1528-7505 VL - 16 IS - 3 SP - 1701 EP - 1707 AN - OPUS4-35618 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Fischer, Franziska T1 - Survival of the fittest - Competetive cocrystal reactions in the ball mill N2 - Mechanochemistry is increasingly used for synthesizing various materials including cocrystals and metal organic compounds. Although this synthesis approach offers a fast and pure synthesis in high yields there is a lack in understanding the mechanisms of milling reactions. The driving forces triggering the formation of cocrystals under milling conditions were investigated using a set of multi-component competitive milling reactions. In these reactions, different active pharmaceutical ingredients were ground together with a further compound acting as coformer. The study was based on new cocrystals including the coformer anthranilic acid. The results of the competitive milling reactions indicate that the formation of cocrystals driven by intermolecular recognition are influenced and inhibited by kinetic aspects including the formation of intermediates and the stability of the reactants. T2 - Berliner Chemie Symposium CY - Berlin, Germany DA - 12.04.2016 KW - milling KW - cocrystal KW - mechanochemistry PY - 2016 AN - OPUS4-35862 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Trappe, Volker T1 - Dauerfestigkeitsgrenze in Faser-Kunststoff-Verbunden – Einfluss der Halbzeuge N2 - Mit Hilfe der an der BAM entwickelten Röntgenrefraktionstopographie lassen sich zerstörungsfrei innere Oberflächen insbesondere in CFK messen. Somit gelingt es quantitativ und ortsaufgelöst Mikrorisse im μm-Maßstab (Faser-Matrix-Ablösungen, Matrix-Matrix-Brüche) auch im komplexen Laminat zu bestimmen. Ziel ist es, die Mikrorissbildung an Geweben und Gelegen in-situ zur Schwingbeanspruchung zu ermitteln, um Materialkonstanten und Modelle zu bestimmen, mit Hilfe derer die Zwischenfaserbruchanstrengungen angeben werden kann, bei der die Grenze zum „unendlichen“ Leben liegt, also der Werkstoff als „dauerfest“ bezeichnet werden kann. Die Schädigungsmechanismen konnten aber auch an Schalenstrukturen aus GFK mit optischen Verfahren und mit In-Situ-Messungen mittels Thermographie nachgewiesen werden. Zudem spielt die Faser-Matrix-Grenzfläche, also die Oberflächenchemie auf der Faser sowie der Vernetzungsgrad der Epoxidharzmatrix eine entscheidende Rolle. T2 - CCeV - AG Strukturelle Integrität und UAG Composites Fatigue CY - Manching, Germany DA - 01.06.2016 KW - Faser-Kunststoff-Verbunde KW - Betriebsfestigkeit KW - Dauerfestigkeitsgrenze KW - Schädigungsmechanismen PY - 2016 AN - OPUS4-37566 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Emmerling, Franziska T1 - In situ analysis of mechanochemical reactions using combined X-ray diffraction and Raman spectroscopy N2 - Mechanochemistry is increasingly used for synthesizing various materials including metal organic compounds and cocrystals. Although this synthesis approach offers a fast and pure synthesis in high yields, there is a lack in understanding the mechanisms of milling reactions. The necessary data can only be obtained in in situ experiments, which were only recently established for milling reactions. Herein, we present a novel setup enabling a combined in situ investigation of mechanochemical reactions using synchrotron XRD and Raman spectroscopy. The specific combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. Besides well-known MOFs like ZIF-8, the formation process of new metal phosphonates and model cocrystals could be studied in detail. The syntheses pathway of the different compounds could be revealed. The results prove that the presented method combination is applicable for a wide range of materials and will provide the necessary understanding to tune and optimize mechanochemically synthesized compounds. T2 - 3oth Meeting of the European Crystallographic Association CY - Basel, Switzerland DA - 28.08.2016 KW - Mechanochemistry KW - In situ PY - 2016 AN - OPUS4-38363 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nguyen, Thi Yen T1 - Direct evidence of polyamorphism in paracetamol N2 - While polymorphism is a common phenomenon in the crystallization processes of organic compounds, polyamorphism has gained importance only recently. Using sophisticated sample environments and applying in situ scattering methods and vibrational spectroscopy, the complete crystallization process of organic compounds from solution can be traced and characterized. Diffuse scattering from amorphous intermediates can be investigated by analyzing the atomic pair Distribution function (PDF) to gain further insights into molecular pre-orientation. The crystallization behavior of Paracetamol was studied exemplarily under defined, surface-free conditions. Based on the choice of the solvent, the formation of different polymorphs is promoted. The thermodynamically stable form I and the metastable orthorhombic form II could be isolated in pure form directly from solution. For both polymorphs, the crystallization from solution proceeds via a distinct amorphous precursor phase. PDF analyses of these different amorphous states indicate a specific pre-orientation of the analyte molecules introduced by the solvent. The resulting crystalline polymorph is already imprinted in these proto-crystalline precursors. Direct experimental evidence for the polyamorphism of paracetamol is provided. T2 - Annual CM1402 crystallize COST meeting CY - Coimbra, Portugal DA - 06.04.2016 KW - Paracetamol KW - Crystallization KW - In situ analysis KW - Active pharmaceutical ingredient (API) PY - 2016 AN - OPUS4-35873 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kabelitz, Anke T1 - Time-resolved WAXS studies on the formation and dissolution of polynuclear aluminium sulfates N2 - Polynuclear aluminium species (Al13) find application in different areas like water purification, contaminant transport, and as pilling clays with high specific surface areas, due to their strong binding ability to aggregates and high positive charge. In the present contribution, we report on the in situ investigation of the Al13 sulfate synthesis and dissolution by synchrotron wide-angle X-ray scattering (WAXS). Al13 sulfates were crystallized by precipitating hydrolyzed aluminum solutions by the addition of sodium sulfate. Dissolution of the formed Al13 species was carried out by adding hydrochloric acid. The measurements were performed using a custom-made acoustic levitator as sample holder. The study provides information about the intermediates during the crystallization and dissolution processes. From the data, a mechanism was derived indicating the influence of the crystallization process. T2 - MS&T 2016: 3rd International Workshop of In-situ Studies with Photons, Neutrons and Electrons Scattering CY - Salt Lake City, USA DA - 24.10.2016 KW - WAXS KW - Aluminium sulfate KW - Time-resolved PY - 2016 AN - OPUS4-38173 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Kabelitz, Anke T1 - Direkt in-situ analysis of milling reactions: a look in the blackbox N2 - Mechanochemistry is increasingly used for synthesizing various materials. Although this synthesis approach offers a fast and pure synthesis in high yields, there is a lack in understanding the mechanisms of milling reactions. The necessary data can only be obtained by in situ experiments, which were only recently established for milling reactions. Herein, we present a novel setup combining in situ synchrotron XRD and Raman spectroscopy. This combination allows to study milling processes comprehensively on the level of the molecular and crystalline structure and thus obtaining reliable data for mechanistic studies. The formation process of MOFs, metal phosphonates and model cocrystals could be studied in detail. The results prove that the presented method combination is applicable for a wide range of materials and will provide the necessary understanding to tune and optimize mechanochemically synthesized compounds. T2 - MS&T 2016: Mechanochemical Synthesis and Reactions in Materials Science CY - Salt Lake City, USA DA - 24.10.2016 KW - Mechanochemistry KW - In situ KW - Mechanistic studies PY - 2016 AN - OPUS4-38174 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -