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Issue 37, 2011
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Structural characterisation of phosphate materials: new insights into the spatial proximities between phosphorus and quadrupolar nuclei using the D-HMQC MAS NMR technique

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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 31P/S through-space two-dimensional correlation NMR spectra providing unreported structural information on (i) a sodium alumino-silicate glass doped with only 3% of P2O5, (ii) a potassium boro-phosphate glass containing BO3 and BO4 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.

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

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Publication details

The article was received on 31 Mar 2011, accepted on 03 Aug 2011 and first published on 18 Aug 2011


Article type: Paper
DOI: 10.1039/C1CP20993K
Citation: Phys. Chem. Chem. Phys., 2011,13, 16786-16794
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    Structural characterisation of phosphate materials: new insights into the spatial proximities between phosphorus and quadrupolar nuclei using the D-HMQC MAS NMR technique

    G. Tricot, O. Lafon, J. Trébosc, L. Delevoye, F. Méar, L. Montagne and J-P. Amoureux, Phys. Chem. Chem. Phys., 2011, 13, 16786
    DOI: 10.1039/C1CP20993K

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