Two-Dimensional Sideband Separation in Magic-Angle-Spinning NMR

Antzutkin, Oleg N.; Shekar, S. Chandra; Levitt, Malcolm H.

doi:10.1006/jmra.1995.1142

Cited by 289 publications

(373 citation statements)

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“…1. It consists of two segments, i.e., the water suppression segment involving the DANTE pulse sequence (23) followed by the 2D-PASS segment (22), where the cross-polarization component in the original report was replaced by a /2 pulse. In a 2D-PASS spectrum, the sidebands are separated by the order n of the SSB.…”

Section: Nmr Experimentsmentioning

confidence: 99%

“…22, an intrinsic T 2 weighting of one rotor period is introduced. In order to compensate for pulse imperfections and RF field inhomogeneity, a phase cycling sequence has to be applied.…”

Section: Nmr Experimentsmentioning

confidence: 99%

“…The timings tm 1 -tm 6 between the six pulses are determined by the so-called PASS-16 sequence given in Ref. 22. Here, 16 different combinations of delay times tm 1 -tm 6 are used (to be called evolution increments hereafter), which makes it possible to separate the centerband and 15 sideband spectra without spectral aliasing.…”

Section: Nmr Experimentsmentioning

confidence: 99%

“…These include Gan's (18) original MAT experiment and its subsequent modifications such as phase-corrected MAT (PHORMAT) (19). The second class (MAT-2) involves the use of five RF pulses during a constant evolution time period, e.g., one rotor period, including the five replicated magic angle turning (FIREMAT) (20,21) and the 2D-phase-altered spinning sidebands (PASS) (22) techniques. All of these experiments are 2D isotropic-anisotropic chemical shift correlation experiments yielding a highresolution isotropic chemical shift dimension and a chemical shift anisotropy dimension.…”

mentioning

confidence: 99%

“…The 2D-PASS experiment (22) was chosen as an initial approach because of its ease of implementation.…”

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confidence: 99%

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High‐resolution ¹H NMR spectroscopy in organs and tissues using slow magic angle spinning

Wind

Rommereim

2001

Magnetic Resonance in Med

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It is shown that high-resolution 1 H NMR spectra of intact excised tissues and organs can be obtained by rotating the sample slowly about an axis at the magic angle of 54°44 with the external magnetic field. In this way tissue and cellular damage invoked by standard magic angle spinning (MAS) experiments, where spinning speeds of several kHz are typically employed, are minimized. Special RF pulse sequences, developed originally in solid state NMR, can be used to produce a spinning sideband-free isotropic spectrum. In this article the first results are shown of the brain, heart, liver, gluteus muscle, and kidney excised from mice using the 2D-phase-altered spinning sidebands (PASS) technique and employing MAS spinning speeds of 43-125 Hz. It was found that with slow sample spinning similar, and in some cases even better, spectral resolutions are obtained as compared with fast MAS. Magn Reson Med 46: 213-218,

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Section: Nmr Experimentsmentioning

confidence: 99%

“…22, an intrinsic T 2 weighting of one rotor period is introduced. In order to compensate for pulse imperfections and RF field inhomogeneity, a phase cycling sequence has to be applied.…”

Section: Nmr Experimentsmentioning

confidence: 99%

Section: Nmr Experimentsmentioning

confidence: 99%

mentioning

confidence: 99%

“…The 2D-PASS experiment (22) was chosen as an initial approach because of its ease of implementation.…”

mentioning

confidence: 99%

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High‐resolution ¹H NMR spectroscopy in organs and tissues using slow magic angle spinning

Wind

Rommereim

2001

Magnetic Resonance in Med

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Solid‐State NMR Spectroscopy

Wang¹,

Yan²,

Li³

et al. 2022

Encyclopedia of Polymer Science and Technology

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Solid‐state NMR spectroscopy is an indispensable tool for probing detailed structures and dynamics of polymers at an atomic level due to its capability to selectively manipulate various types of anisotropic spin interactions in solids and its nondestructive property. Herein, this article mainly describes the properties of those anisotropic spin interactions in solids, and how they are used to extract structural and dynamic information via sophisticated one‐ and multidimensional solid‐state NMR spectroscopy. We hope this article can be a good tutorial for the researchers interested in using solid‐state NMR to study polymers.

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C‐13 Chemical‐Shift Tensors in Organic Materials

Harper

Iuliucci

2014

Encyclopedia of Analytical Chemistry

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The chemical‐shift tensor provides an exquisitely sensitive measure of the electronic environment around a nucleus. The tensor is defined by a real symmetric 3 × 3 matrix with six measurable components. Single crystals are usually required to measure all six components whereas three shifts per nucleus are measurable in powders. These powder data, known as principal values , are defined as δ 11 ≥ δ 22 ≥ δ 33 . Presently, most 2D experiments measuring tensor data display the 1D isotropic spectrum along one axis and the tensor patterns for each resonance along the second dimension. Experiments most frequently used are two‐dimensional phase‐adjusted spinning sideband (2D PASS), phase corrected magic angle turning (PHORMAT), FIREMAT (five π replicated magic angle turning), RAI (recoupling of anistropic information), SUPER (separation of undistorted powder patterns by effortless recoupling), and CSA (chemical shift anisotropy) amplification. Very few simple relationships exist between principal values and structure, thus comparison with model structures from computational methods has become important. Recently, these computational methods have been used to predict structure in solids that are intractable to traditional methods. Tensor data have also been found to be extremely sensitive to crystal structure and can therefore be used to further refine some structures, including single crystal structures. The prospect of predicting entire crystal structures from 13 C tensor data and computational methods is now realistic, and a few structures have recently been determined without diffraction data.

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Two-Dimensional Sideband Separation in Magic-Angle-Spinning NMR

Cited by 289 publications

References 0 publications

High‐resolution ¹H NMR spectroscopy in organs and tissues using slow magic angle spinning

High‐resolution ¹H NMR spectroscopy in organs and tissues using slow magic angle spinning

Solid‐State NMR Spectroscopy

C‐13 Chemical‐Shift Tensors in Organic Materials

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Two-Dimensional Sideband Separation in Magic-Angle-Spinning NMR

Cited by 289 publications

References 0 publications

High‐resolution 1H NMR spectroscopy in organs and tissues using slow magic angle spinning

High‐resolution 1H NMR spectroscopy in organs and tissues using slow magic angle spinning

Solid‐State NMR Spectroscopy

C‐13 Chemical‐Shift Tensors in Organic Materials

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High‐resolution ¹H NMR spectroscopy in organs and tissues using slow magic angle spinning

High‐resolution ¹H NMR spectroscopy in organs and tissues using slow magic angle spinning