Research output: Contribution to Journal/Magazine › Journal article › peer-review
Research output: Contribution to Journal/Magazine › Journal article › peer-review
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TY - JOUR
T1 - (33)S MAS NMR of a disordered sulfur-doped silicate: signal enhancement via RAPT, QCPMG and adiabatic pulses
AU - O'Dell, L. A.
AU - Klimm, K.
AU - Freitas, J. C. C.
AU - Kohn, S. C.
AU - Smith, Mark E.
PY - 2009/2/1
Y1 - 2009/2/1
N2 - Three different signal enhancement techniques have been applied to (33)S magic-angle spinning nuclear magnetic resonance (MAS NMR) of a disordered silicate containing 1.15 wt% (33)S. Partial saturation of the satellite transitions was achieved using a rotor-assisted population transfer (RAPT) pulse sequence, resulting in a signal enhancement of 1.63, albeit with a slight distortion of the line shape due to selective excitation. Adiabatic inversion of the satellite transitions by various amplitude-and frequency-modulated pulse shapes (such as hyperbolic secant and wideband uniform-rate smooth truncation) was also attempted, resulting in a signal enhancement of up to 1.85, with no apparent line shape distortion. Quadrupolar Carr-Purcell-Meiboom-Gill (QCPMG) and RAPT-QCPMG sequences were also used, both of which yielded spikelet spectra that accurately reflected the MAS line shape with a greatly improved signal-to-noise ratio. It is hoped that this study demonstrates that (33)S solid-state MAS NMR is now feasible even on disordered, low-sulfur-content systems.
AB - Three different signal enhancement techniques have been applied to (33)S magic-angle spinning nuclear magnetic resonance (MAS NMR) of a disordered silicate containing 1.15 wt% (33)S. Partial saturation of the satellite transitions was achieved using a rotor-assisted population transfer (RAPT) pulse sequence, resulting in a signal enhancement of 1.63, albeit with a slight distortion of the line shape due to selective excitation. Adiabatic inversion of the satellite transitions by various amplitude-and frequency-modulated pulse shapes (such as hyperbolic secant and wideband uniform-rate smooth truncation) was also attempted, resulting in a signal enhancement of up to 1.85, with no apparent line shape distortion. Quadrupolar Carr-Purcell-Meiboom-Gill (QCPMG) and RAPT-QCPMG sequences were also used, both of which yielded spikelet spectra that accurately reflected the MAS line shape with a greatly improved signal-to-noise ratio. It is hoped that this study demonstrates that (33)S solid-state MAS NMR is now feasible even on disordered, low-sulfur-content systems.
KW - INTEGER QUADRUPOLAR NUCLEI
KW - SOLID-STATE NMR
KW - HYPERBOLIC SECANT PULSES
KW - DOUBLE FREQUENCY SWEEPS
KW - NATURAL-ABUNDANCE
KW - SENSITIVITY ENHANCEMENT
KW - SATELLITE TRANSITIONS
KW - POPULATION TRANSFER
KW - COUPLING-CONSTANTS
KW - SPECTRA
U2 - 10.1007/s00723-008-0159-8
DO - 10.1007/s00723-008-0159-8
M3 - Journal article
VL - 35
SP - 247
EP - 259
JO - Applied Magnetic Resonance
JF - Applied Magnetic Resonance
SN - 1613-7507
IS - 2
ER -