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Eingeladener Vortrag
- nein (10)
Die Bundesanstalt für Materialforschung und -prüfung (BAM) ist eine wissenschaftlich technische Bundesoberbehörde im Geschäftsbereich des Bundesministeriums für Wirtschaft und Energie (BMWi), die über einen gesetzlichen Auftrag für die Sicherheit in Technik und Chemie verfügt und auf nahezu 150 Jahre zurückblicken kann. Vor diesem Hintergrund forscht, entwickelt, und prüft die BAM in den fünf Themenfeldern Energie, Infrastruktur, Umwelt, Material und Analytical Sciences mit einer unikalen Vielfalt an analytischen Methoden.
Ugly Spectra and Lousy interfaces – Challenges for Compact NMR Spectroscopy in Process Control
(2016)
With the introduction of advanced process analytical technology, the closeness of key process variables to their limits can be directly controlled and the product can be classified or even released in real time.
Compact NMR instruments can make NMR spectroscopy accessible in industrial and harsh environments for process control.
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.
Homogen katalysierte Reaktionen sind wichtige Werkzeuge der chemischen Industrie. Milde Reaktionsbedingungen und hohe Selektivitäten führen zu einer energie- und ressourcenschonenden Produktion. Ein bedeutender Prozessschritt ist die Hydroformylierung. Hier kommen Kobalt- und Rhodiumkomplexe mit mehrzähnigen Liganden zum Einsatz, die zumeist in wässriger Lösung vorliegen. Die Anwendbarkeit beschränkt sich demnach auf kurzkettige Edukte mit hinreichender Wasserlöslichkeit.
This key comparison aims to assess the capabilities of the participants to determine the amount-of-substance fraction oxygen in nitrogen. The GAWG has classified this as a track B comparison, due to the unexpected 50 μmol/mol argon mole fraction content of the transfer standards, which effects the achievable performance of some measurement techniques such a GC-TCD. The separation of oxygen and argon is challenging, and not all systems in use are equally well designed for it. As this analytical challenge due to a substantial fraction of argon in the transfer standards became a reality, the Gas Analysis Working Group (GAWG) decided to qualify this key comparison as a regular key comparison and not as a core comparison, which may be used to support calibration and measurement capabilities (CMCs) for oxygen in nitrogen, or for oxygen in nitrogen mixtures containing argon only (see also the section on support to CMCs).
Currently research in chemical manufacturing moves towards flexible plug-and-play approaches focusing on modular plants, capable of producing small scales on-demand with short down-times between individual cam-paigns. This approach allows for efficient use of hardware, a faster optimization of the process conditions, and thus, an accelerated introduction of new products to the market. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The re-sulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via compara-bly straightforward and robust analysis techniques. Here we report on a fast and reliable calibration-free online high field NMR monitoring approach for technical mixtures. It combines a versatile fluidic system, continuous-flow measurement with a time interval of 20 s per spectrum, and a robust, automated algo-rithm to interpret the ob-tained data. All spectra were acquired using a 500 MHz NMR spectrometer (Varian) with a dual band flow probe having a 1/16 inch polymer tubing working as a flow cell. Single scan 1H spectra were recorded with an acquisition time of 5 s, relaxation delay of 15 s.