TY - CONF A1 - Maiwald, Michael T1 - Low field NMR spectroscopy for online monitoring N2 - Online NMR spectroscopy is an excellent tool to study complex reacting multicomponent mixtures and gain process insight and understanding. For online studies under process conditions, flow NMR probes can be used in a wide range of temperature and pressure. This paper compiles the most important aspects towards quantitative process NMR spectroscopy in complex multicomponent mixtures and provides examples. After NMR spectroscopy is introduced as an online method and for technical samples without sample preparation in deuterated solvents, influences of the residence time distribution, pre-magnetization, and cell design are discussed. NMR acquisition and processing parameters as well as data preparation methods are presented and the most practical data analysis strategies are introduced. T2 - Sonderkolloquium der INVITE-GmbH CY - Leverkusen, Germany DA - 07.09.2016 KW - Industrie 4.0 KW - CONSENS KW - Prozessanalytik KW - Online NMR spectroscopy PY - 2015 UR - https://nbn-resolving.org/urn:nbn:de:kobv:b43-361417 AN - OPUS4-36141 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Forschung und Entwicklung für Prozessanalytik und Automatisierung in der Prozessindustrie N2 - Neue Prozess-Sensoren für neue Produktionskonzepte. Wie entsteht Innovation? Forschungsimpulse aus der Technologie-Roadmap „Prozess-Sensoren 2015+“. Herausforderungen durch das Zukunftsprojekt „Industrie 4.0“. Technologie-Roadmap „Prozess-Sensoren 4.0“ T2 - ACHEMA 2015: Automation im Dialog – Meet the experts CY - Frankfurt a. M., Germany DA - 15.06.2015 KW - Industrie 4.0 KW - Smart Sensors KW - Smarte Sensoren KW - Process Analytical Technology KW - Prozessanalytik PY - 2015 AN - OPUS4-36142 LA - deu AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - Quantitative and online NMR Spectroscopy at BAM N2 - Online NMR spectroscopy, Determination of impurities of fluids, NMR process Monitoring, purity assessment T2 - NMR-Kolloquium Buchs CY - Buchs, Switzerland DA - 29.05.2015 KW - qNMR KW - Quantitative NMR-Spektroskopie KW - Online NMR Spectroscopy KW - Reaction monitoring KW - Reference material KW - Metrology PY - 2015 AN - OPUS4-36143 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael T1 - qNMR forever – reference material metrology at high pressures and high purities N2 - Due to recent advances in technical developments of NMR instruments such as acquisition electronics and probe design, detection limits of components in liquid mixtures were improved into the lower ppm range (approx. 5–10 ppm amount of substance). This showed that modern NMR equipment is also suitable for the observation of hydrocarbon samples in the expanded fluid phase or gas phase. Since Quantitative NMR spectroscopy (qNMR) is a direct ratio method of analysis without the need of calibration it was used to determine impurities in appropriate liquid and liquefied hydrocarbon isomers up to C6, which are used for preparation of primary gas standards, e.g., natural gas or exhaust gas standards. At the same time it is possible to yield structural information with a minimum of sample preparation. Thus, cross contaminations between different isomers of the observed hydrocarbons and their (NMR-active) impurities can be identified and quantified. In general, most quantitative organic chemical measurements rely on the availability of highly purified compounds to act as calibration standards. The traceability and providence of these standards is an essential component of any measurement uncertainty budget and provides the final link of the result to the units of measurement, ideally the SI. The more recent increase in the use of qNMR for the direct assessment of chemical purity however can potentially improve the traceability and reduce the uncertainty of the measured chemical purity at a reduced cost and with less material. For example the method has beneficially been used by National Measurement institutes for recent CCQM comparisons including the CCQM–K55 series of purity studies. Traditional ‘indirect’ methods of purity analysis require that all impurities are identified and quantified, leading to a minimum of 4 individual analytical methods (organic impurities, water, solvents, inorganic residue). These multiple technique approaches measure an array of different chemical impurities normally present in purified organic chemical compounds. As many analytical methodologies have compound-specific response factors, the accuracy and traceability of the purity assessment is dependent on the availability of reference materials of the impurities being available. qNMR provides the most universally applicable form of direct purity determination without need for reference materials of impurities or the calculation of response factors but only exhibiting suitable NMR properties. The development of CRMs addressing qNMR specific measurement issues will give analysts compounds ideally suited for the analytical method and also provide full characterisation of qNMR related parameters to enable more realistic uncertainty budgets. These materials will give users the tools to exploit qNMR more easily and enable them to speed up analytical method development and reduce the time and financial burden of multiple analytical testing. T2 - 3rd Practical Application of NMR in Industry Conference (PANIC) 2015 CY - La Jolla, CA, USA DA - 09.02.2015 KW - qNMR KW - Quantitative NMR-Spektroskopie KW - Reference Material KW - Metrology PY - 2015 AN - OPUS4-36144 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Maiwald, Michael A1 - Meyer, Klas A1 - Zientek, Nicolai T1 - Towards online reaction monitoring with fully automated NMR data evaluation and modelling - Current results from simultaneous 19F-1H medium resolution NMR experiments N2 - NMR Process Monitoring Towards an automated field integration T2 - 3rd Practical Applications of NMR in Industry Conference (PANIC) - Mestrelab users' meeting CY - La Jolla, CA, USA DA - 08.02.2015 KW - Online NMR spectroscopy KW - Reaction monitoring KW - Prozessanalytik KW - Process analytical technology PY - 2015 AN - OPUS4-36145 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Guthausen, G. T1 - Online measurements in a bypass: challenges and possibilities N2 - The design of sample flow cells, commonly used in online analytics and especially for medium resolution NMR spectroscopy (MR-NMR) in low magnetic fields, was experimentally and theoretically investigated by 1H-NMR and numerical simulations. The flow pattern was characterised to gain information about the residence time distribution and mixing effects. Both 1H-NMR imaging and spectroscopy were used to determine the characteristics of flow cells and their significance for on-line measurements such as reaction monitoring or hyphenated separation spectroscopy. The volume flow rates investigated were in the range from 0.1 to 10 ml/min, typically applied in the above mentioned applications. When compared to those commonly used in high-field NMR, the special characteristics of flow cells for MR-NMR were revealed by various NMR experiments and compared with CFD simulations. The influence of the design of the inlet and outlet on the flow pattern was investigated as well as the effect of the length of the cell. For practical use, a numerical estimation of the inflow length was given. In addition, it was shown how experiments on the polarisation build-up revealed insight into the flow characteristics in MR-NMR. T2 - Quantitative NMR Methods for Reaction and Process Monitoring (NMRPM) Symposium CY - Kaiserslautern, Germany DA - 15.01.2015 KW - Online NMR spectroscopy KW - Process analytical technology KW - Flow profiles KW - Online monitoring KW - Reaction monitoring PY - 2015 AN - OPUS4-36147 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Gaal, Mate T1 - Focusing of ferroelectret air-coupled ultrasound transducers N2 - Air-coupled ultrasound has been applied increasingly as a non-destructive testing method for lightweight construction in recent years. It is particularly appropriate for composite materials being used in automotive and aviation industry. Air-coupled ultrasound transducers mostly consist of piezoelectric materials and matching layers. However, their fabrication is challenging and their signal-to-noise ratio often not sufficient for many testing requirements. To enhance the efficiency, air-coupled ultrasound transducers made of cellular polypropylene have been developed. Because of its small density and sound velocity, this piezoelectric ferroelectret matches the small acoustic impedance of air much better than matching layers applied in conventional transducers. In our contribution, we present two different methods of spherical focusing of ferroelectret transducers for the further enhancement of their performance in NDT applications. Measurements on carbon-fiber-reinforced polymer (CFRP) samples and on metal adhesive joints performed with commercially available focused air-coupled ultrasound transducers are compared to measurements executed with self-developed focused ferroelectret transducers. T2 - 42nd Annual Review of Progress in Quantitative Nondestructive Evaluation CY - Minneapolis, Minnesota, USA DA - 26.07.2015 KW - Focusing KW - Ferroelectret KW - Air-coupled KW - Transducer KW - Ultrasonic PY - 2015 AN - OPUS4-35957 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nolze, Gert T1 - Introduction to PowderCell N2 - The presentation give a short introduction into the free-available software PowderCell (BAM)for the simulation of X-ray diffraction patterns of polycrystalline materials. T2 - PowderCell Users meeting CY - Joinville, Brazil DA - 19.10.2015 KW - X-ray diffraction KW - Simulation KW - Structure viewer KW - Subgroup relationships PY - 2015 AN - OPUS4-37791 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nolze, Gert T1 - EBSD: more reliable and accurate N2 - The presentation discusses numerous new approaches in order to increase precision and accuracy of electrom backscatter diffraction measurements. T2 - 1st EBSD Workshop CY - Belo Horizonte, Brazil DA - 17.09.2015 KW - Orientation mapping KW - Electron backscatter diffraction KW - Lattice parameter determination KW - Orientation precision KW - Orientation noise PY - 2015 AN - OPUS4-37797 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER - TY - CONF A1 - Nolze, Gert A1 - Winkelmann, Aimo T1 - The challenge of band detection N2 - The presentation demonstrates different traps which are related to the detection of Kikuchi bands in EBSD patterns. T2 - EBSD 2015 CY - Glasgow, UK DA - 30.03.2015 KW - Electron backscatter diffraction KW - Image processing KW - Pseudo symmerty KW - Crystal lattice KW - Pyrite KW - Pattern matching KW - Misindexing PY - 2015 AN - OPUS4-37805 LA - eng AD - Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin, Germany ER -