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Two-dimensional Ca-43-H-1 correlation solid-state NMR spectroscopy

Wong, Alan and Laurencin, Danielle and Dupree, Ray and Smith, Mark E. (2009) Two-dimensional Ca-43-H-1 correlation solid-state NMR spectroscopy. Solid State Nuclear Magnetic Resonance, 35 (1). pp. 32-36.

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Abstract

Calcium-43 (nuclear spin, S = 7/2) is an NMR insensitive low-gamma quadrupolar nucleus and up until recently only one-dimensional solid-state Ca-43 NMR spectra have been reported. Through-space correlation experiments are challenging between spin-1/2 and low-gamma quadrupolar nuclei because of the intrinsically weak dipolar interaction and the often-low natural abundance of the quadrupolar nucleus. Rotary-resonance recoupling (R-3) has recently been used to re-introduce hetero-nuclear dipolar interactions for sensitive high-gamma quadrupolar nuclei, but has not yet been applied in the case of low-gamma half-integer quadrupolar nuclei. Here an effective and robust 2D H-1-Ca-43 NMR correlation experiment combining the R-3 dipole-recoupling scheme with 2D HMQC is presented. It is demonstrated that the weak Ca-43-H-1 dipolar coupling in hydroxyapatite and oxy-hydroxyapatite can be readily re-introduced and that this recoupling scheme is more efficient than conventional cross-polarization transfer. Moreover, three Ca-43-H-1 dipolar coupled calcium environments are clearly resolved in the structurally unknown oxy-hydroxyapatite. This local information is not readily available from other techniques such as powder XRD and high resolution electron microscopy. R-3-HMQC is also a desirable experiment because the set-up is simple and it can be applied using conventional multi-resonance probes. (C) 2008 Elsevier Inc. All rights reserved.

Item Type: Article
Journal or Publication Title: Solid State Nuclear Magnetic Resonance
Uncontrolled Keywords: Ca-43 NMR, Low-gamma, Hetero-nuclear correlation NMR spectroscopy, Dipolar interaction, R-3-HMQC, Hydroxyapatite, Oxy-hydroxyapatite
Subjects:
Departments: VC's Office
ID Code: 52835
Deposited By: ep_importer_pure
Deposited On: 28 Feb 2012 13:55
Refereed?: Yes
Published?: Published
Last Modified: 09 Apr 2014 23:09
Identification Number:
URI: http://eprints.lancs.ac.uk/id/eprint/52835

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