TY - CONF A1 - Maiwald, Michael T1 - How far does the light shine? A check-up of quantitative high and low field NMR spectroscopy N2 - The Royal Society of Chemistry NMR Discussion Group and Molecular Spectroscopy Group would like to invite you to the 2017 Spring Meeting, which will be held at GlaxoSmithKline (GSK), Stevenage. The theme for the meeting is “Low level detection and quantification by NMR” and different NMR technologies, including solution state NMR, solid state NMR and benchtop/low field NMR will be discussed. The presentations will cover a range of NMR related disciplines, including conventional low level detection and quantification, the use of cryoprobes, quantification of polymorphism using ssNMR and also methods for spectral simplification. Recent developments and applications of hyperpolarisation techniques, within both solution state and solid state NMR, will be presented in conjunction with the effect these sensitivity enhancements have with respect to quantification and limits of detection. T2 - NMR Discussion Group and Molecular Spectroscopy Group Spring Meeting: "Low Level Detection and Quantification by NMR Spectroscopy" CY - Stevenage, UK DA - 29.03.2017 KW - Online NMR Spectroscopy KW - Quantitative NMR Spectroscopy KW - qNMR KW - Indirect Hard Modeling KW - Limit of Detection KW - NMR Spectroscopy KW - Metrology PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-395936 AN - OPUS4-39593 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Design and validation of a compact NMR analyser N2 - Monitoring chemical reactions is the key to chemical process control. Today, mainly optical online methods are applied. NMR spectroscopy has a high potential for direct loop process control. Compact NMR instruments based on permanent magnets are robust and inexpensive analysers, which feature advantages like low maintenance, ease of use, and cryogen-free operation. Instruments for online NMR measurements equipped with a flow-through cell, possessing a good signal-to-noise-ratio, robustness, and meeting the requirements for integration into industrial plants (i.e., explosion safety and fully automated data analysis) are currently not available off the rack. Intensified continuous processes are in focus of current research. Flexible (modular) chemical plants can produce different products using the same equipment with short down-times between campaigns and quick introduction of new products to the market. In continuous flow processes online sensor data and tight closed-loop control of the product quality are mandatory. Otherwise there is a huge risk of producing large amounts of out-of-spec (OOS) products. This is addressed in the European Union’s Research Project CONSENS by development and integration of smart sensor modules for process monitoring and control within such modular plant setups. The presented NMR module is provided in an explosion proof housing with a module size of 57 x 57 x 85 cm and involves a compact 43.5 MHz NMR spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction) and evaluation. Indirect Hard Modeling (IHM) was selected for data analysis of the low-field NMR spectra. A set-up for monitoring continuous reactions in a thermostated 1/8” tubular reactor using automated syringe pumps was used to validate the IHM models by using high-field NMR spectroscopy as analytical reference method. T2 - ANAKON 2017 CY - Tübingen, Germany DA - 03.04.2017 KW - Online NMR spectroscopy KW - Low-Field NMR spectroscopy KW - Modular production plants KW - Process analytical technology PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-396960 AN - OPUS4-39696 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Design and validation of a compact online NMR module N2 - Monitoring chemical reactions is the key to process control. Today, mainly optical online methods are applied, which are calibration intensive. NMR spectroscopy has a high potential for direct loop process control while cutting the calibration and validation needs to an minimum and thus exhibiting short set-up times. Compact NMR instruments make NMR spectroscopy accessible in industrial and harsh environments for advanced process monitoring and control. Intensified continuous processes are in focus of current research. Flexible (modular) chemical plants can produce different products using the same equipment with short down-times between campaigns and quick introduction of new products to the market. In continuous flow processes online sensor data and tight closed-loop control of the product quality are mandatory. Data analysis techniques are available but currently mostly used for off-line data analysis to detect the causes of variations in the product quality. This is addressed within the EU’s Research Project CONSENS by the development and integration of a smart NMR module for process monitoring. The presented NMR module is provided in a mobile explosion proof housing and involves a compact spectrometer together with an acquisition unit and a programmable logic controller for automated data preparation (phasing, baseline correction), and evaluation. Such “smart sensors” provide the basis for the future project “Industrie 4.0”, and Industrial Internet of Things (IIoT), along with current requirements to process control, model based control, or soft sensing. The module transforms the acquired online spectra of various technically relevant reactions to either conventional 4‒20 mA signals as well as WiFi based OPC-UA communication protocols, which enables NMR-based advanced process control and funny discussions with plant managers along with automation and safety engineers. T2 - Small Molecule NMR Conference (SMASH) CY - Baveno, Italy DA - 17.09.2017 KW - Online NMR spectroscopy KW - CONSENS KW - Reaction monitoring KW - Process control KW - Process analytical technology KW - Indirect hard modeling KW - Industrie 4.0 KW - Smart sensors KW - SMASH PY - 2017 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-419473 UR - http://www.smashnmr.org/conference/program AN - OPUS4-41947 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Tiebe, Carlo A1 - Maiwald, Michael A1 - Schukar, Marcus T1 - Beiträge der Prozessanalytik und Sensorik zur Sicherheit in Wasserstofftechnologien N2 - Intelligent sensor systems, certified reference materials and instrumental analytical-chemical methods contribute to safety and functionality in hydrogen technologies. This article gives a brief overview of SensRef activities in the Competence Centre H2Safety@BAM on the issues: Analytical methods for the determination of hydrogen purity, certified reference materials as measurement standards with regard to gas quality (primary calibrators) of BAM, test methods for gas sensor systems to detect hydrogen in air as well as the application of fibre-optic sensor systems to monitor the expansion and ageing behaviour of composite containers in hydrogen technologies. T2 - Berlin Brandenburger Optik-Tag "Einsatz von Sensorik und Mikroelektronik in der Wasserstoffwirtschaft" CY - Online meeting DA - 29.11.2021 KW - H2Safety@BAM KW - SensRef KW - Gas analysis KW - Gas purity KW - Fibre-optic sensors KW - Sensor response KW - Certified reference materials PY - 2021 AN - OPUS4-54138 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Martins, Inês C.B. A1 - Al-Sabbagh, Dominik A1 - Meyer, Klas A1 - Maiwald, Michael A1 - Scholz, G. A1 - Emmerling, Franziska T1 - Insight into the Structure and Properties of Novel Imidazole-Based Salts of Salicylic Acid N2 - The preparation of new active pharmaceutical ingredient (API) multicomponent Crystal forms, especially co-crystals and salts, is being considered as a reliable strategy to improve API solubility and bioavailability. In this study, three novel imidazole-based salts of the poorly water-soluble salicylic acid (SA) are reported exhibiting a remarkable improvement in solubility and dissolution rate properties. All structures were solved by powder X-ray diffraction. Multiple complementary techniques were used to solve co-crystal/salt ambiguities: density functional Theory calculations, Raman and 1H/13C solid-state NMR spectroscopies. In all molecular salts, the Crystal packing interactions are based on a common charged assisted +N-H SA)...O-(co-former) hydrogen bond interaction. The presence of an extra methyl group in different positions of the co-former, induced different supramolecular arrangements, yielding salts with different physicochemical properties. All salts present much higher solubility and dissolution rate than pure SA. The most promising results were obtained for the salts with imidazole and 1-methylimidazole co-formers. KW - Salicylic acid KW - Imidazole KW - Salts KW - Powder X-ray diffraction KW - SsNMR KW - DFT PY - 2019 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-502825 DO - https://doi.org/10.3390/molecules24224144 VL - 24 IS - 22 SP - 4144 PB - MDPI AN - OPUS4-50282 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Batzdorf, Lisa A1 - Zientek, Nicolai A1 - Rump, Doreen A1 - Fischer, Franziska A1 - Maiwald, Michael A1 - Emmerling, Franziska T1 - Make and break - Facile synthesis of cocrystals and comprehensive dissolution studies N2 - Mechanochemistry is increasingly used as a ‘green alternative’ for synthesizing various materials including pharmaceutical cocrystals. Herein, we present the mechanochemical synthesis of three new cocrystals containing the API carbamazepine (cocrystals CBZ:Indometacin 1:1, CBZ:Benzamide 1:1, and CBZ:Nifedipine 1:1). The mechanochemical reaction was investigated in situ documenting a fast and complete reaction within one minute. Online NMR spectroscopy proved the direct influence of the dissolution behaviour of the coformers to the dissolution behaviour of the API carbamazepine. The dissolution behaviour of the organic cocrystals is compared to the behaviour of the pure drug indicating a general applicability of this approach for detailed cocrystal dissolution studies. KW - Cocrystals KW - Carbamazepine KW - Mechanochemistry KW - Powder diffraction KW - Online NMR spectroscopy PY - 2017 DO - https://doi.org/10.1016/j.molstruc.2016.11.063 SN - 0022-2860 SN - 1872-8014 VL - 1133 SP - 18 EP - 23 AN - OPUS4-38664 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Villajos Collado, José Antonio A1 - Bienert, M. A1 - Gugin, Nikita A1 - Emmerling, Franziska A1 - Maiwald, Michael T1 - A database to select affordable MOFs for volumetric hydrogen cryoadsorption considering the cost of their linkers N2 - Physical adsorption at cryogenic temperature (cryoadsorption) is a reversible mechanism that can reduce the pressure of conventional compressed gas storage systems. Metal–organic framework (MOF) materials are remarkable candidates due to the combination of high specific surface area and density which, in some cases, provide a high volumetric storage capacity. However, such extensive use of MOFs for this application requires the selection of affordable structures, easy to produce and made from feasible metallic and organic components. Herein, we introduce a MOF database detailing the crystallographic and porous properties of 3600 existing MOFs made from industrially relevant metals and their organic composition. The comparison of the available minimum costs of linkers allowed the creation of a database to select affordable structures with high potential for volumetric hydrogen storage by cryoadsorption, considering their composition based on individual or mixed building blocks. A user inter� face, available online, facilitates the selection of MOFs based on the properties or names of structures and linkers. KW - MOF´s PY - 2023 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-583619 DO - https://doi.org/10.1039/d3ma00315a VL - 4 IS - 18 SP - 4226 EP - 4237 PB - Royal Society of Chemistry (RSC) AN - OPUS4-58361 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - JOUR A1 - Gugin, Nikita A1 - Villajos Collado, José Antonio A1 - Dautain, O. A1 - Maiwald, Michael A1 - Emmerling, Franziska T1 - Optimizing the Green Synthesis of ZIF-8 by Reactive Extrusion Using In Situ Raman Spectroscopy N2 - We report the scale-up of a batch solid synthesis of zeolitic imidazolate framework-8 (ZIF-8) for reactive extrusion. The crystalline product forms in the extruder directly under the mixture of solid 2-methylimidazole and basic zinc carbonate in the presence of a catalytic amount of liquid. The process parameters such as temperature, liquid type, feeding rate, and linker excess were optimized using the setup specifically designed for in situ Raman spectroscopy. Highly crystalline ZIF-8 with a Brunauer–Emmett–Teller (BET) surface area of 1816 m2 g–1 was quantitatively prepared at mild temperature using a catalytic amount of ethanol and a small excess of the linker. Finally, we developed a simple and comprehensive approach to evaluating the environmental friendliness and scalability of metal–organic framework (MOF) syntheses in view of their large-scale production. KW - Mechanochemistry KW - In situ Raman KW - Large-scale processing KW - Metal−organic frameworks KW - Twin-screw extrusion (TSE) PY - 2023 DO - https://doi.org/10.1021/acssuschemeng.2c07509 SN - 2168-0485 VL - 11 IS - 13 SP - 5175 EP - 5183 PB - ACS Publications AN - OPUS4-57366 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Zientek, Nicolai A1 - Batzdorf, Lisa A1 - Kraume, M. A1 - Emmerling, Franziska A1 - Maiwald, Michael T1 - Online-NMR-Methoden zur Analyse des Auflösungsverhaltens von pharmazeutischen Cokristallen N2 - Pharmazeutische Cokristalle bestehen aus einem Wirkstoff und einem sogenannten Cokristall-Bildner. Bei letzterem handelt es sich typischerweise um eine organische Base oder Säure. Die Synthese und Charakterisierung von pharmazeutischen Cokristallen ist von patentrechtlicher Relevanz und Gegenstand aktueller Forschungen, da die Bildung solcher Cokristalle häufig mit einer Verbesserungen der physiko-chemischen Eigenschaften der enthaltenen Wirkstoffe einhergeht. In den letzten Jahren ist es gelungen, insbesondere das Auflösungsverhalten der pharmazeutischen Wirkstoffe gezielt zu verbessern und dadurch eine optimierte Bioverfügbarkeit zu realisieren. T2 - 8. Kolloquium Arbeitskreis Prozessanalytik CY - Berlin, Germany DA - 03.12.2012 KW - Quantitative Online-NMR-Spektroskopie KW - Cokristalle KW - Auflösungskinetik PY - 2012 SN - 978-3-9815360-1-0 N1 - Geburtsname von Batzdorf, Lisa: Tröbs, L. - Birth name of Batzdorf, Lisa: Tröbs, L. IS - P12 SP - 40 AN - OPUS4-28267 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Online-qNMR-Spektroskopie zur Charakterisierung des Lösungsverhaltens von pharmazeutischen Wirkstoffen und Formulierungen N2 - Nur weit weniger als ein Prozent aller pharmazeutischen Wirkstoffe finden den Weg in die Anwendung. Grund dafür sind in fast allen Fällen die äußerst schlechten biopharmazeutischen Eigenschaften der Wirkstoffe, wie ihre Löslichkeit, Stabilität und – bei festen Darreichungsformen – ihre Kristalleigenschaften, auch wenn die Wirkstoffe eine gute Wirksamkeit oder gute toxikologische Eigenschaften aufweisen. Mit dem Trend zu höheren Molmassen bei chemischen Wirkstoffen nimmt ihre Löslichkeit in wässrigen Systemen rapide ab. Verbesserungen der Löslichkeit und des Auflösungsverhalten stellen heute die zentrale Herausforderung bei der Entwicklung neuer Arzneimittel dar und liegen im Fokus der aktuellen pharmazeutischen Forschung und Entwicklung. Für eine Verbesserung der physikalisch chemischen Eigenschaften werden verschiedene Verfahren beforscht: Mikronisierung, gezielte Salzbildung bzw. Salzscreening, Solubilisierung mit Cosolventien oder die Nutzung von Polymeren als mögliche Transportwege. Pharmazeutische Cokristalle bestehen aus einem Wirkstoff und einem sogenannten Cokri-stall-Bildner. Bei letzterem handelt es sich typischerweise um ein organisches Molekül, das ähnliche Struktureigenschaften wie der pharmazeutische Wirkstoff aufweist. Die Synthese und Charakterisierung von pharmazeutischen Cokristallen ist von patentrechtlicher Relevanz und Gegenstand aktueller Forschungen, da die Bildung solcher Cokristalle häufig mit einer Verbesserung der physikochemischen Eigenschaften der enthaltenen Wirkstoffe einhergeht. In den letzten Jahren ist es gelungen, insbesondere das Auflösungsverhalten der pharmazeutischen Wirkstoffe gezielt zu verbessern und dadurch eine optimierte Bioverfügbarkeit zu realisieren. Um einige Einschränkungen der Methoden UV/VIS-Detektion und HPLC zu umgehen, verfolgen wir das Auflösungsverhalten der Cokristalle mittels Online-NMR-Spektroskopie als ein direktes Verfahren: Die Methode erlaubt zum einen die direkte Beobachtung und Quantifizierung individueller Species, die bei der Auflösung beteiligt sind, d. h. Wirkstoff(e), Cokristallbildner und Lösungsmittel lassen sich getrennt voneinander mit einer hohen zeitlichen Auflösung und spektraler Dispersion beobachten. Ferner kommt diese Me-thode ohne Kalibrierung aus, da die NMR-Spektroskopie eine "absolute Vergleichsmethode" ist. Darüber hinaus kann die absolute Konzentration gemessen werden, wenn gegen Standards gearbeitet wird. Der Einsatz dieses Verfahrens zum Studium des Auflösungsverhaltens ist völlig neu. Perspektivisch reizvoll ist die Weiterentwicklung zu einem mikroanalytischen Verfahren, das mit äußerst geringen Substanzmengen auskommt. T2 - Institutskolloquium Pharmazie und Lebensmittelchemie, Julius-Maximilians-Universität Würzburg CY - Würzburg, Germany DA - 27.07.2017 KW - Pharmazeutische Wirkstoffe KW - Pharmazeutische Formulierungen KW - Cokristalle KW - qNMR-Spektroskopie KW - Quantitative NMR-Spektroskopie KW - Auflösungsverhalten PY - 2017 AN - OPUS4-41166 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -