High-field NMR using resistive and hybrid magnets

Resistive and resistive-superconducting hybrid magnets can generate dc magnetic fields much higher than conventional superconducting NMR magnets but the field spatial homogeneity and temporal stability are usually not sufficient for high-resolution NMR experiments. Hardware and technique development addressing these issues are presented for high-resolution NMR at magnetic fields up to 40T. Passive ferromagnetic shimming and magic-angle spinning are used effectively to reduce the broadening from inhomogeneous magnetic field. A phase correction technique based on simultaneous heteronuclear detection is developed to compensate magnetic field fluctuations to achieve high spectral resolution.     

Free vibration analysis of a hanged clamped-free cylindrical shell partially submerged in fluid: The effect of external wall,internal shaft,and flat bottom

The free flexural vibration of a hanged clamped-free cylindrical shell with various boundary conditions partially submerged in a fluid is investigated. Specifically, the effects of the boundary conditions such as the existence of the external wall, internal shaft, and bottom on the natural vibration characteristics of the partially submerged cylindrical shell are investigated both theoretically and experimentally. The fluid is assumed to be inviscid and irrotational. The cylindrical shell is modeled by using the Rayleigh–Ritz method based on the Sanders shell theory. The kinetic energy of the fluid is derived by solving a boundary-value problem related to the fluid motion. The theoretical predictions were in good agreement with the experimental results validating the theoretical approach developed in this study. The effects of the external wall, internal shaft, and bottom on the natural vibration characteristics can be neglected when its boundaries are not very close to the shell structure.     

Enhancing sensitivity of quadrupolar nuclei in solid-state NMR with multiple rotor assisted population transfers

Rotor-assisted population transfer (RAPT) was developed as a method for enhancing MAS NMR sensitivity of quadrupolar nuclei by transferring polarization associated with satellite transitions to the central m=12-->-12 transition. After a single RAPT transfer, there still remains polarization in the satellite transitions that can be transferred to the central transition. This polarization is available without having to wait for the spin system to return to thermal equilibrium. We describe a new RAPT scheme that uses the remaining polarization of the satellites to obtain a further enhancement of the central transition by performing RAPT-enhanced experiments multiple times before waiting for re-equilibration of the spin system. For 27Al (I=5/2) in albite we obtain a multiple RAPT enhancement of 3.02, a 48% increase over single RAPT. For 93Nb (I=9/2) in NaNbO(3) we obtain a multiple RAPT enhancement of 5.76, an 89% increase over single RAPT. We also describe a data processing procedure for obtaining the maximum possible signal-to-noise ratio.     

Double-quantum filtered STMAS

Double-quantum and double-quantum-filtered satellite-transition magic-angle spinning (STMAS) experiments are proposed. The experiments efficiently convert satellite-transition coherence from single- to double-quantum with a central-transition selective pi-pulse. The conversion allows the selection of double-quantum coherence transfer pathways with phase cycling that completely filters out unwanted diagonal and outer satellite-transition peaks. Both experiments are demonstrated with RbNO3 and AlPO4-berlinite as model compounds for obtaining clean STMAS spectra of spins 3/2 and 5/2, respectively.