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On-line monitoring of microwave-assisted chemical reactions by small-volume NMR techniques (Micro(wave)-NMR)
Start date: 01 Apr 2009, End date: 30 Sep 2012 PROJECT  FINISHED 

The Micro(wave)- NMR project involves the coupling of continuous flow microwave (MW) chemical reactions with small-volumes Nuclear Magnetic Resonance (NMR) techniques. The aim is the on-line monitoring of a chemical process under continuous-flow microwave irradiation by NMR with the main goal of optimizing a process within less time and lower cost.On one hand, the project combines the unique heating mechanism of microwave irradiation with the safety, reproducibility and facile automation of continuous flow techniques. On the other hand, microcoils NMR will be used as the detection method providing the detection of mass-limited samples as well as more complete structural information than any other analytical technique. It is the first time than NMR will be coupled to the microwave technology for an on-line analysis of the reaction product. For the achievement of the objectives, regarding the microwave set-up, a continuous-flow microwave cell has to be designed. The cell will contain capillary-sized reaction tubes defining a small heated coil that winds in and out of the microwave cavity. Reaction mixtures can be flowed through defining a low reaction volume, in the µL range in order to optimize a chemical process with lower cost. Regarding the NMR set-up, microfluidic chips containing a radiofrequency microcoil (NMR-chip) will be used as the detection method and hyphenated to the microwave reactor by means of capillaries. The use of microcoils for NMR provides a sensitivity enhancement, enabling the detection of samples in the picomole range. Microcoils provide higher signals when the detection volume matches the diameter coil, thus, the detection volume will be very small and in the same range than the reaction volume for a better analysis. The NMR-chip concept has been designed and optimized during my previous Marie Curie Fellowship. The proposed project allows me to share the knowledge acquired during my current Fellowship with my University of origin.
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