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Tricot G, Lafon O, Trébosc J, et al. Structural characterisation of phosphate materials: new insights into the spatial proximities between phosphorus and quadrupolar nuclei using the D-HMQC MAS NMR technique. Phys Chem Chem Phys. 2011;13(37):16786-94doi: 10.1039/c1cp20993k.
Tricot, G., Lafon, O., Trébosc, J., Delevoye, L., Méar, F., Montagne, L., & Amoureux, J. P. (2011). Structural characterisation of phosphate materials: new insights into the spatial proximities between phosphorus and quadrupolar nuclei using the D-HMQC MAS NMR technique. Physical chemistry chemical physics : PCCP, 13(37), 16786-94. https://doi.org/10.1039/c1cp20993k
Tricot, G, et al. "Structural characterisation of phosphate materials: new insights into the spatial proximities between phosphorus and quadrupolar nuclei using the D-HMQC MAS NMR technique." Physical chemistry chemical physics : PCCP vol. 13,37 (2011): 16786-94. doi: https://doi.org/10.1039/c1cp20993k
Tricot G, Lafon O, Trébosc J, Delevoye L, Méar F, Montagne L, Amoureux JP. Structural characterisation of phosphate materials: new insights into the spatial proximities between phosphorus and quadrupolar nuclei using the D-HMQC MAS NMR technique. Phys Chem Chem Phys. 2011 Oct 06;13(37):16786-94. doi: 10.1039/c1cp20993k. Epub 2011 Aug 18. PMID: 21853181.
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Phys Chem Chem Phys. 2011 Oct 06;13(37):16786-94. doi: 10.1039/c1cp20993k. Epub 2011 Aug 18.

Structural characterisation of phosphate materials: new insights into the spatial proximities between phosphorus and quadrupolar nuclei using the D-HMQC MAS NMR technique.

Physical chemistry chemical physics : PCCP

G Tricot, O Lafon, J Trébosc, L Delevoye, F Méar, L Montagne, J-P Amoureux

Affiliations

  1. Université Lille Nord de France, CNRS UMR 8181, Unité de Catalyse et de Chimie du Solide, Université Lille 1, Ecole Nationale Supérieure de Chimie de Lille, Villeneuve d'Ascq, France. [email protected]

PMID: 21853181 DOI: 10.1039/c1cp20993k

Abstract

We show in this article how the spatial proximity between phosphorus and quadrupolar nuclei can be efficiently and easily investigated with the D-HMQC (Dipolar Hetero-nuclear Multiple-Quantum Coherences) NMR technique. Compared to the commonly used CP-HETCOR (Cross-Polarisation HETero-nuclear CORrelation) sequence, the D-HMQC pulse scheme exhibits a higher sensitivity and a better robustness with respect to spinning frequency, electronic shielding and quadrupole interaction, and thus does not require time-consuming and complicated optimisation procedures. The advantages of the D-HMQC are demonstrated in this article through the acquisition of (31)P/S through-space two-dimensional correlation NMR spectra providing unreported structural information on (i) a sodium alumino-silicate glass doped with only 3% of P(2)O(5), (ii) a potassium boro-phosphate glass containing BO(3) and BO(4) groups and (iii) a crystalline zirconium vanado-phosphate. All these systems, representative of the most important mixed phosphate network materials, cannot be correctly investigated with the conventional CP-HETCOR NMR technique.

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