Can we improve solid-state NMR sensitivity without DNP ?
Résumé
Solid-state Nuclear Magnetic Resonance (NMR) is suffering from an intrinsic low sensitivity, despite recent improvements. Instrumentation, fast acquisition, and signal processing approaches were investigated to circumvent this drawback as far as possible. Firstly, micro-coils (Magic Angle Coil Spinning, MACS) were placed into rotors and inductively coupled to the standard probe coil. A time gain of 5 was obtained for microquantities with a mass m = 100-200 µg. Secondly, Non-Uniform Sampling (NUS) was chosen as a way to decrease the acquisition time of indirect dimensions of multi-dimensional experiments. Poisson sampling appeared to be the best choice to limit artifacts, whereas hybrid sampling proved to be efficient on spectra with both broad and narrow peaks. A time gain of 4 was achieved. Thirdly, spectra were processed with Singular Value Decomposition (SVD) denoising. We highlighted an overestimation of Gaussian peaks by 20 %. Automatic thresholding was implemented, giving a time gain of 2.3. Finally, computation time was decreased by 100 by combining the 'divide and conquer' algorithm, optimized libraries, hardware instruction calls, and single
precision.
Domaines
Chimie analytiqueFormat | Présentation |
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Origine | Fichiers produits par l'(les) auteur(s) |