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

Alan Wong¹, Danielle Laurencin, Ray Dupree

¹Department of Physics, University of Warwick, Coventry CV4 7AL, UK.

Solid State Nuclear Magnetic Resonance

|January 2, 2009

Summary

This summary is machine-generated.

This study introduces a new 2D (1)H-(43)Ca NMR method using rotary-resonance recoupling (R(3)) to overcome challenges with low-gamma quadrupolar nuclei. The technique effectively reveals distinct calcium environments in materials like oxy-hydroxyapatite.

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Area of Science:

Solid-state Nuclear Magnetic Resonance (NMR) spectroscopy.
Materials characterization.
Calcium-43 (43Ca) NMR.

Background:

Calcium-43 (43Ca) is an NMR-insensitive, low-gamma quadrupolar nucleus, limiting its use in solid-state NMR.
Previous studies primarily focused on one-dimensional (43)Ca NMR spectra.
Through-space correlation experiments involving low-gamma quadrupolar nuclei are difficult due to weak dipolar interactions and low natural abundance.

Purpose of the Study:

To develop an effective and robust 2D (1)H-(43)Ca NMR correlation experiment for low-gamma quadrupolar nuclei.
To demonstrate the application of rotary-resonance recoupling (R(3)) for re-introducing hetero-nuclear dipolar interactions in (43)Ca NMR.
To resolve distinct calcium environments in structurally complex materials.

Main Methods:

Implementation of a 2D (1)H-(43)Ca NMR correlation experiment.
Combination of the rotary-resonance recoupling (R(3)) dipole-recoupling scheme with 2D Heteronuclear Multiple Quantum Coherence (HMQC).
Application of the method to hydroxyapatite and oxy-hydroxyapatite samples.

Main Results:

Successful re-introduction of weak (43)Ca-(1)H dipolar coupling in hydroxyapatite and oxy-hydroxyapatite.
Demonstration that R(3)-HMQC is more efficient than conventional cross-polarization transfer.
Clear resolution of three distinct (43)Ca-(1)H dipolar coupled calcium environments in oxy-hydroxyapatite.

Conclusions:

The R(3)-HMQC technique provides an effective means to study low-gamma quadrupolar nuclei like (43)Ca.
This method offers local structural information not easily obtainable by techniques like powder X-ray diffraction (XRD) or high-resolution electron microscopy.
The R(3)-HMQC experiment is user-friendly, applicable with standard multi-resonance probes, and enhances the utility of (43)Ca NMR.