Studies of minute quantities of natural abundance molecules using 2D heteronuclear correlation spectroscopy under 100kHz MAS
- JEOL Resonance Inc., Tokyo (Japan); RIKEN CLST-JEOL Collaboration Center, Kanagawa (Japan)
- Ames Lab., Ames, IA (United States)
- Ames Lab., Ames, IA (United States); Iowa State Univ., Ames, IA (United States)
Two-dimensional 1H{13C} heteronuclear correlation solid-state NMR spectra of naturally abundant solid materials are presented, acquired using the 0.75-mm magic angle spinning (MAS) probe at spinning rates up to 100 kHz. In spite of the miniscule sample volume (290 nL), high-quality HSQC-type spectra of bulk samples as well as surface-bound molecules can be obtained within hours of experimental time. The experiments are compared with those carried out at 40 kHz MAS using a 1.6-mm probe, which offered higher overall sensitivity due to a larger rotor volume. The benefits of ultrafast MAS in such experiments include superior resolution in 1H dimension without resorting to 1H–1H homonuclear RF decoupling, easy optimization, and applicability to mass-limited samples. As a result, the HMQC spectra of surface-bound species can be also acquired under 100 kHz MAS, although the dephasing of transverse magnetization has significant effect on the efficiency transfer under MAS alone.
- Research Organization:
- Ames Laboratory (AMES), Ames, IA (United States)
- Sponsoring Organization:
- USDOE
- Grant/Contract Number:
- AC02-07CH11358
- OSTI ID:
- 1227210
- Alternate ID(s):
- OSTI ID: 1360657
- Report Number(s):
- IS-J-8827; PII: S0926204015000053
- Journal Information:
- Solid State Nuclear Magnetic Resonance, Vol. 66-67, Issue C; ISSN 0926-2040
- Publisher:
- ElsevierCopyright Statement
- Country of Publication:
- United States
- Language:
- English
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