3D correlation NMR spectrum between three distinct heteronuclei for the characterization of inorganic samples: Application on sodium alumino-phosphate materials

We report here an original NMR sequence allowing the acquisition of 3D correlation NMR spectra between three distinct heteronuclei, among which two are half-integer spin quadrupolar nuclei. Furthermore, as two of them exhibit close Larmor frequency, this experiment was acquired using a standard trip...

Full description

Saved in:
Bibliographic Details
Published in:Solid state nuclear magnetic resonance 2017-07, Vol.84, p.164-170
Main Authors: Nagashima, Hiroki, Tricot, Grégory, Trébosc, Julien, Lafon, Olivier, Amoureux, Jean-Paul, Pourpoint, Frédérique
Format: Article
Language:English
Subjects:
Alumino-phosphate
Chemical Sciences
Close Larmor frequencies
HMQC
INEPT
or physical chemistry
Theoretical and
Citations: Items that this one cites
Items that cite this one
Online Access:Get full text
Tags: Add Tag
No Tags, Be the first to tag this record!
Description
Summary:We report here an original NMR sequence allowing the acquisition of 3D correlation NMR spectra between three distinct heteronuclei, among which two are half-integer spin quadrupolar nuclei. Furthermore, as two of them exhibit close Larmor frequency, this experiment was acquired using a standard triple-resonance probe equipped with a commercial frequency splitter. This NMR technique was tested and applied to sodium alumino-phosphate compounds with 31P as the spin-1/2 nucleus and 23Na and 27Al as the close Larmor frequencies isotopes. To the best of our knowledge, such experiment with direct 31P and indirect 27Al and 23Na detection is the first example of 3D NMR experiment in solids involving three distinct heteronuclei. This sequence has first been demonstrated on a mixture of Al(PO3)3 and NaAlP2O7 crystalline phases, for which a selective observation of NaAlP2O7 is possible through the 3D map edition. This 3D correlation experiment is then applied to characterize mixing and phase segregation in a partially devitrified glass that has been proposed as a material for the sequestration of radioactive waste. The 31P-{23Na,27Al} 3D experiment conducted on the partially devitrified glass material conclusively demonstrates that the amorphous component of the material does not contain aluminum. The as-synthesized material thus presents a poor resistance against water, which is a severe limitation for its application in the radioactive waste encapsulation domain. [Display omitted]
ISSN:0926-2040
1527-3326
DOI:10.1016/j.ssnmr.2017.03.002