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Charles Crockford

Publications and source records attributed to Charles Crockford.

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Chemical shift anisotropy amplification with high amplification factor and improved sensitivity.

An improved version of the recently proposed chemical shift anisotropy amplification experiment is described. The original experiment correlates a fast magic angle spinning spectrum in the omega2 dimension with a sideband pattern in omega1 in which the intensities mimic those for a sample spinning at a fraction of the rate omegar/N. Advantages of the experiment include the use of standard methods to extract the principal tensor components from the omega1 sideband patterns and the small number of t1 increments required. The improved version described here permits large amplification factors N to be obtained without resort to prohibitively long sequences of pi-pulses and allows sensitivity to be maximized by eliminating the need to store the magnetization along the z-axis for t1. Amplification factors up to 32 are demonstrated experimentally.

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Chemical shift anisotropy amplification.

A new NMR experiment which allows a measurement of the chemical shift anisotropy (CSA) tensor under magic angle spinning (MAS) is described. This correlates a fast MAS spectrum in the omega2 dimension with a sideband pattern in omega1 in which the intensities mimic those for a sample spinning at a fraction of the rate omega r/N, and these sidebands result from an amplification by a factor N of the modulation caused by the CSA. Standard methods can be used to extract the principal tensor components from the omega1 sideband patterns, and the nature of the experiment is such that the use of a large number of t1 increments can be avoided without compromising the resolution of different chemical sites. The new experiment is useful for accurately measuring narrow shift anisotropies.

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Measurement of orientation distributions using chemical shift amplification.

A new three-dimensional magic angle spinning (MAS) experiment is proposed, based on a combination of the two-dimensional rotor-synchronized MAS experiment of Spiess and co-workers and a new chemical shift anisotropy amplification method. The new experiment is demonstrated on a macroscopically ordered sample of ultra-high molecular weight poly(ethylene).

Anisotropy↗