Analytische Chemie
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In verlegten Eisenbahnschienen entstehen durch Rollkontaktermüdung rissartige Oberflächenschädigungen. Der geschädigte Bereich wird im Rahmen der Schieneninstandhaltung regelmäßig abgetragen, um zu verhindern, dass durch unkontrolliertes Risswachstum schwerwiegende Schienenschäden entstehen. Hierzu werden u. A. Schienenschleifzüge eingesetzt.
Früher wurde das Schleifergebnis einer Sichtprüfung unterzogen. Es kommt jedoch vor, dass Risse in der Oberfläche beim Schleifen zugeschmiert oder durch Schleifriefen maskiert werden, so dass diese nicht mehr sichtbar obwohl noch vorhanden sind.
An der BAM wurde ein Wirbelstromprüfsystem entwickelt, das sowohl zur Planung als auch der Qualitätskontrolle der Schieneninstandhaltung genutzt wird. Dieses System ist in der Lage, Schädigungen zu detektieren und deren Schädigungstiefe zu bestimmen, selbst dann, wenn optisch keine Schädigung zu erkennen ist.
Seit 2013 ist die Qualitätskontrolle mit Wirbelstromprüfsystemen bei der Schienenbearbeitung fest im Regelwerk der DB verankert.
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 campaigns. 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 [1]. Driven mostly by the search for chemical syntheses under biocompatible conditions, so-called “click” chemistry rapidly became a growing field of research. The resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably 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 obtained 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.
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 campaigns. 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 resulting simple one-pot reactions are so far only scarcely accompanied by an adequate optimization via comparably 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 algorithm to interpret the obtained 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. As a proof-of-concept, the thiol-ene coupling between N-boc cysteine methyl ester and allyl alcohol was conducted in non-deuterated solvents while its time-resolved behaviour was characterised with step tracer experiments
Through the application of spectral modeling the signal area for each reactant can be deconvoluted in the online spectra and thus converted to the respective concentrations or molar ratios. The signals which were suitable for direct integration were used herein for comparison purposes of both methods.