Assessment of diffusion coefficients of general solvents by PFG-NMR: Investigation of the sources error

Kato, Haruhisa; Saito, Tetsuya; Nabeshima, Mami; Shimada, Kayori; Kinugasa, Shinichi

doi:10.1016/j.jmr.2006.03.003

Cited by 56 publications

(54 citation statements)

References 59 publications

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“…(1). decays), and hence represents an interesting alternative to other setups designed to avoid these artifacts such as, for instance, post processing corrections [48], Shigemi tubes [50], or slice selective experiments [51].…”

Section: Absolute Gradient Calibrationmentioning

confidence: 99%

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Pulsed field gradient magic angle spinning NMR self-diffusion measurements in liquids

Viel

Ziarelli

Pagès

et al. 2008

Journal of Magnetic Resonance

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Several investigations have recently reported the combined use of pulsed field gradient (PFG) with magic angle spinning (MAS) for the analysis of molecular mobility in heterogeneous materials. In contrast, little attention has been devoted so far to delimiting the role of the extra force field induced by sample rotation on the significance and reliability of self-diffusivity measurements. The main purpose of this work is to examine this phenomenon by focusing on pure liquids for which its impact is expected to be largest. Specifically, we show that self-diffusion coefficients can be accurately determined by PFG MAS NMR diffusion measurements in liquids, provided that specific experimental conditions are met. First, the methodology to estimate the gradient uniformity and to properly calibrate its absolute strength is briefly reviewed and applied on a MAS probe equipped with a gradient coil aligned along the rotor spinning axis, the so-called 'magic angle gradient' coil. Second, the influence of MAS on the outcome of PFG MAS diffusion measurements in liquids is investigated for two distinct typical rotors of different active volumes, 12 and 50 microL. While the latter rotor led to totally unreliable results, especially for low viscosity compounds, the former allowed for the determination of accurate self-diffusion coefficients both for fast and slowly diffusing species. Potential implications of this work are the possibility to measure accurate self-diffusion coefficients of sample-limited mixtures or to avoid radiation damping interferences in NMR diffusion measurements. Overall, the outlined methodology should be of interest to anyone who strives to improve the reliability of MAS diffusion studies, both in homogeneous and heterogeneous media.

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Section: Absolute Gradient Calibrationmentioning

confidence: 99%

“…On one hand, as fast diffusing components, we analyzed by PFG MAS a set of standard solvents exhibiting different viscosities, and for which recent high quality NMR self-diffusion data has been published in the literature [50].…”

Section: Pfg Mas Diffusion Measurementsmentioning

confidence: 99%

Pulsed field gradient magic angle spinning NMR self-diffusion measurements in liquids

Viel

Ziarelli

Pagès

et al. 2008

Journal of Magnetic Resonance

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show abstract

“…One drastic measure to reduce the effects of non-uniformity is to use either slice selection [4,29,30] or a very short sample [31][32][33] to restrict the signals measured to a small volume over which the field gradient variation is small. Unfortunately both involve a major sacrifice in signal-to-noise ratio, as well as introducing problems where the diffusion distance is not small compared to the slice thickness, and their use is probably best limited to experiments where the analysis method used requires strict adherence to the exponential attenuation as a function of gradient squared seen in Eq.…”

Section: Introductionmentioning

confidence: 99%

Improving the accuracy of pulsed field gradient NMR diffusion experiments: Correction for gradient non-uniformity

Connell

Bowyer²,

Bone

et al. 2009

Journal of Magnetic Resonance

118

121

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“…36 Diffusion coefficients (D) were calculated by (eqn. 3) and the hydrodynamic radius (r H ) by (eqn.…”

Section: Resultsmentioning

confidence: 99%

Conformational restriction of flexible molecules in solution by a semirigid bis-porphyrin molecular tweezer

et al. 2013

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Assessment of diffusion coefficients of general solvents by PFG-NMR: Investigation of the sources error

Cited by 56 publications

References 59 publications

Pulsed field gradient magic angle spinning NMR self-diffusion measurements in liquids

Pulsed field gradient magic angle spinning NMR self-diffusion measurements in liquids

Improving the accuracy of pulsed field gradient NMR diffusion experiments: Correction for gradient non-uniformity

Conformational restriction of flexible molecules in solution by a semirigid bis-porphyrin molecular tweezer

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