Sensitivity enhancement of NMR spectra of half-integer spin quadrupolar nuclei in solids using hyperbolic secant pulses.
The experimental factors influencing the enhancements achievable for the central NMR transition, m(I)=1/2-->m(I)=-1/2, of spin-3/2 and spin-5/2 nuclei in the solid state using hyperbolic secant, HS, pulses for population transfer are investigated. In the case of powder samples spinning at the magic angle, it is found that the spinning frequency, the bandwidth and the frequency offset of the HS pulse play a crucial role in determining the maximum enhancements. Specifically, the bandwidth must be set to the spinning frequency for maximum signal enhancements. The (87)Rb NMR enhancement obtained for RbClO(4) using HS pulses was relatively insensitive to the magic angle spinning frequency; however, in the case of Al(acac)(3), the (27)Al enhancement increased with MAS frequency. In order to obtain an adiabatic HS sweep, one should optimize the rf field for a given pulse duration or optimize the pulse duration for a given rf field.
Siegel
Renée
R
Department of Chemistry, Gunning/Lemieux Chemistry Centre, University of Alberta, Edmonton, Alta., Canada T6G 2G2.
Nakashima
Thomas T
TT
Wasylishen
Roderick E
RE
D000465:Algorithms; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D011208:Powders; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012815:Signal Processing, Computer-Assisted; D013113:Spin Labels
D011208:Powders; D013113:Spin Labels