M. Roux et al., Structural investigation by multinuclear solid state NMR and X-ray diffraction of as-synthesized, dehydrated, and calcined AlPO4-SOD, J PHYS CH B, 105(38), 2001, pp. 9083-9092
AlPO4-SOD, a microporous aluminophosphate, was synthesized in a quasi-nonaq
ueous medium using dimethylformamide as solvent and template. The as-synthe
sized, dehydrated, calcined materials and the corresponding rehydrated phas
es were investigated by various solid-state nuclear magnetic resonance (NMR
) and powder X-ray diffraction techniques. Structural data from the NMR stu
dy are in a very good agreement with the as-synthesized AlPO4-SOD structure
refined from powder synchrotron data. P-31 homonuclear correlation and P-3
1/Al-27 3QHETCOR experiments allowed the complete assignment of P-31 and (2
1)AI resonances to the corresponding crystallographic sites. P-31 and Al-27
NMR spectra are drastically modified after dehydration at 200 degreesC and
calcination at 800 degreesC. A possible structural rearrangement of the te
mplate molecules is proposed that explains NMR and XRD data of the dehydrat
ed material. The structure of the calcined material solved by powder XRD is
in agreement with the NMR data.