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Variable Temperature NMR Characterization of α-Glycine


Proton NMR spin-lattice relaxation times in the laboratory frame (T1) and in the rotating frame (T1ρ) were measured as a function of temperature for a static sample of α-glycine. Both T1 and T1ρ data can be fit quantitatively by a single thermally-activated motion (the modulation of the dipolar coupling by random hopping about the threefold axis of the -NH3 group), with no addition of other mechanisms at any temperature between 173 K and 415 K. An activation energy of 21.7 ± 1 kJ/mol was extracted and is compared with previously reported values for both α- and γ-glycine. Such comparisons allow the correction of glycine polymorphs misidentified in the literature. The minimum in T1 at 325 K corresponds to a correlation time of 0.53 ns. Chemical shifts as a function of temperature were measured by 1H CRAMPS and by 13C and 15N CP/MAS experiments. These results are discussed relative to a previous report of anomalous electrical behavior in α-glycine within this temperature range.

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