PFG-assisted selection and suppression of 1H NMR signals in the solid state under fast MAS.
Under fast MAS conditions, techniques for 1H signal selection and suppression, which have originally been developed for solution-state NMR, become applicable to solids. In this work, we describe how WATERGATE and DANTE pulse sequences can be used under MAS to selectively excite or suppress peaks in 1H solid-state spectra. As known from the liquid-state analogues, signal selection and/or suppression is supported by pulsed-field gradients which selectively dephase and rephase transverse magnetisation. Under MAS, the required field gradients are provided by a simple pair of coils which have been built into a standard fast-MAS probe. PFG-assisted techniques enable efficient selection or suppression of 1H peaks in a single transient of the pulse sequence without the need for phase cycles. Therefore, these tools can readily be incorporated into solid-state MAS NMR experiments, which is demonstrated here for 1H-1H double-quantum NMR spectra of supramolecular systems. In the examples presented here, the 1H signals of interest are relatively weak and need to be observed despite the presence of the strong 1H signal of long alkyl sidechains. PFG-assisted suppression of this strong perturbing signal is shown to be particularly useful for obtaining unambiguous results.
Max-Planck Institut für Polymerforschung, Postfach 3148, D-55021, Mainz, Germany.
Ingrid
I
Fischbach
Karena
K
Thieme
Anke
A
Hoffmann
Manfred
M
Hehn
Ingo
I
Schnell
D007093:Imidazoles / Q000737:chemistry; D046911:Macromolecular Substances; D009682:Magnetic Resonance Spectroscopy / Q000295:instrumentation / Q000379:methods*; D008280:Magnetics / Q000295:instrumentation; D008698:Mesylates / Q000737:chemistry; D008968:Molecular Conformation; D044367:Phase Transition; D011083:Polycyclic Compounds / Q000737:chemistry*; D011522:Protons; D011786:Quality Control; D012815:Signal Processing, Computer-Assisted; D013113:Spin Labels
D007093:Imidazoles; D046911:Macromolecular Substances; D008698:Mesylates; D011083:Polycyclic Compounds; D011522:Protons; D013113:Spin Labels; C045880:methanesulfonic acid; C012256:coronene