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Solvent Suppression in High-Resolution 1H NMR Spectroscopy Using Conventional and Phase Alternated Continuous Wave Free Precession
Authors:Claudimar Junker Duarte  Luiz Alberto Colnago  Rodrigo Bagueira de Vasconcellos Azeredo  Tiago Venâncio
Institution:1. Departamento de Química, Universidade Federal de S?o Carlos, Rodovia Washington Luis, km 235, S?o Carlos, SP, 13565-905, Brazil
2. Embrapa Instrumenta??o Agropecuária, Rua XV de Novembro 1452, S?o Carlos, SP, 13560-970, Brazil
3. Instituto de Química, Universidade Federal Fluminense, Outeiro S?o Jo?o Batista, Niterói, RJ, 24020-141, Brazil
Abstract:Solvent suppression is frequently mandatory in 1H high-resolution nuclear magnetic resonance (NMR), especially for those experiments designed for non-deuterated solvent, normally used in protein and in vivo analysis, and also in liquid chromatography-NMR. Here, simple pulse sequences, which are based on continuous wave free precession (CWFP), consisting of a train of pulses separated by a time interval $ T_{\text{p}} \ll T_{2}^{*} $ , is applied to suppress one or more solvent signals in 1H high-resolution NMR experiments, because of its dependency on the offset frequency. The conventional CWFP pulse sequence, that uses pulses with the same phase and duration, introduces some phase anomaly in the Fourier-transformed spectrum. This problem is minimized when the pulses are applied with phase alternation by π/2 in relation to the preceding pulse. Some problems with signal intensity can also be minimized using a shorter pulse width. Both CWFP and phase alternated CWFP can be easily used to suppress two solvent signals simultaneously, just using the correct T p value, that must be equal to the inverse of frequency difference (?ν) between both signals to be suppressed. After modifications, we could introduce the CWFP train into 2D routine pulse sequences.
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