Ultrafast NMR T1 relaxation measurements

Probing molecular properties in real time

Pieter E.S. Smith, Kevin J. Donovan, Or Szekely, Maria Baias, Lucio Frydman

    Research output: Contribution to journalArticle

    Abstract

    The longitudinal relaxation properties of NMR active nuclei carry useful information about the site-specific chemical environments and about the mobility of molecular fragments. Molecular mobility is in turn a key parameter reporting both on stable properties, such as size, as well as on dynamic ones, such as transient interactions and irreversible aggregation. In order to fully investigate the latter, a fast sampling of the relaxation parameters of transiently formed molecular species may be needed. Nevertheless, the acquisition of longitudinal relaxation data is typically slow, being limited by the requirement that the time for which the nucleus relaxes be varied incrementally until a complete build-up curve is generated. Recently, a number of single-shot-inversion-recovery methods have been developed capable of alleviating this need; still, these may be challenged by either spectral resolution restrictions or when coping with very fast relaxing nuclei. Here, we present a new experiment to measure the T1s of multiple nuclear spins that experience fast longitudinal relaxation, while retaining full high-resolution chemical shift information. Good agreement is observed between T1s measured with conventional means and T1s measured using the new technique. The method is applied to the real-time investigation of the reaction between D-xylose and sodium borate, which is in turn elucidated with the aid of ancillary ultrafast and conventional 2D TOCSY measurements. Mobility observed: A new experiment is presented to measure the T1s of multiple nuclear spins that experience fast longitudinal relaxation, while retaining full high-resolution chemical shift information. Good agreement is observed between T1s measured with conventional means and T 1s measured using the new technique. The method is applied to the real-time investigation of the reaction between D-xylose and sodium borate.

    Original languageEnglish (US)
    Pages (from-to)3138-3145
    Number of pages8
    JournalChemPhysChem
    Volume14
    Issue number13
    DOIs
    StatePublished - Sep 16 2013

    Fingerprint

    Xylose
    molecular properties
    Chemical shift
    Nuclear magnetic resonance
    nuclear magnetic resonance
    xylose
    Spectral resolution
    retaining
    borates
    Agglomeration
    nuclear spin
    Experiments
    nuclei
    chemical equilibrium
    Sampling
    Recovery
    sodium
    high resolution
    spectral resolution
    shot

    Keywords

    • longitudinal relaxation
    • molecular mobility
    • real-time NMR
    • T
    • ultrafast 2D NMR

    ASJC Scopus subject areas

    • Atomic and Molecular Physics, and Optics
    • Physical and Theoretical Chemistry

    Cite this

    Smith, P. E. S., Donovan, K. J., Szekely, O., Baias, M., & Frydman, L. (2013). Ultrafast NMR T1 relaxation measurements: Probing molecular properties in real time. ChemPhysChem, 14(13), 3138-3145. https://doi.org/10.1002/cphc.201300436

    Ultrafast NMR T1 relaxation measurements : Probing molecular properties in real time. / Smith, Pieter E.S.; Donovan, Kevin J.; Szekely, Or; Baias, Maria; Frydman, Lucio.

    In: ChemPhysChem, Vol. 14, No. 13, 16.09.2013, p. 3138-3145.

    Research output: Contribution to journalArticle

    Smith, PES, Donovan, KJ, Szekely, O, Baias, M & Frydman, L 2013, 'Ultrafast NMR T1 relaxation measurements: Probing molecular properties in real time', ChemPhysChem, vol. 14, no. 13, pp. 3138-3145. https://doi.org/10.1002/cphc.201300436
    Smith, Pieter E.S. ; Donovan, Kevin J. ; Szekely, Or ; Baias, Maria ; Frydman, Lucio. / Ultrafast NMR T1 relaxation measurements : Probing molecular properties in real time. In: ChemPhysChem. 2013 ; Vol. 14, No. 13. pp. 3138-3145.
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