Triple, quintuple and higher order multiple quantum MAS NMR of quadrupolar nuclei.
The optimization of the coherence transfers involved in five, seven and nine-quantum versions of the recently discovered MQMAS technique, is analysed numerically. Data reported in this paper may serve as starting parameters for the experiment set up. An analysis of the intensity and resolution given by each type of experiment is performed, which confirms the need to use very high rf fields for MQ transfers. It follows that five-quantum is achievable rather easily but the use of seven and nine-quantum MAS experiments becomes increasingly difficult due to the demand for high rf power and decreasing sensitivity. The advantages of using the z-filter MQMAS method with respect to a two-pulse sequence are analysed. The method for qualitatively and quantitatively interpret the MQMAS spectra is described. The nature of the spinning side bands along the multiple quantum dimension is explained. It is shown that the rotor synchronization can be conveniently used to eliminate these side bands, but only for 3QMAS experiments. The use of the multiple-quantum method in combination with static samples and VAS, DAS and DOR techniques is finally discussed.
Amoureux
J P
JP
Laboratoire de Dynamique et Structure des Matériaux Moléculaires, CNRS URA 801, Université des Sciences et Technologies de Lille, Villeneuve d'Ascq, France.
Fernandez
C
C
D009682:Magnetic Resonance Spectroscopy