화학공학소재연구정보센터
Journal of Physical Chemistry A, Vol.101, No.46, 8597-8606, 1997
Sensitivity-enhanced quadrupolar-echo NMR of half-integer quadrupolar nuclei. Magnitudes and relative orientation of chemical shielding and quadrupolar coupling tensors
A novel approach to quadrupolar-echo (QE) NMR of half-integer quadrupolar nuclei in static powders is analyzed. By acquisition of the QE spectrum during a Carr-Purcell-Meiboom-Gill (CPMG) train of selective pi pulses, the second-order quadrupolar line shape for the central transition is split into a comb of sidebands leading to a considerable increase in the sensitivity compared to a conventional QE spectrum. The applicability of the method for determination of magnitudes and relative orientation of chemical shielding and quadrupolar coupling tensors is examined. Through numerical simulation and iterative fitting of experimental Rb-87 (RbClO4 and RbVO3) and Co-59 spectra (Co(NH3)(5) Cl-3), it is demonstrated that the quadrupolar CPMG experiment represents a useful method for studying half-integer quadrupolar nuclei exhibiting large quadrupolar coupling combined with anisotropic chemical shielding interactions. Sensitivity enhancements by a factor of up to about 30 are observed for the samples studied.