Site-resolved H-2 relaxation experiments in solid materials by global line-shape analysis of MAS NMR spectra
2016 (English)In: Journal of magnetic resonance (San Diego, Calif. 1997: Print), ISSN 1090-7807, E-ISSN 1096-0856, Vol. 268, 18-24 p.Article in journal (Refereed) PublishedText
We investigate a way one can achieve good spectral resolution in H-2 MAS NMR experiments. The goal is to be able to distinguish between and study sites in various deuterated materials with small chemical shift dispersion. We show that the H-2 MAS NMR spectra recorded during a spin-relaxation experiment are amenable to spectral decomposition because of the different evolution of spectral components during the relaxation delay. We verify that the results are robust by global least-square fitting of the spectral series both under the assumption of specific line shapes and without such assumptions (COmponent-REsolved spectroscopy, CORE). In addition, we investigate the reliability of the developed protocol by analyzing spectra simulated with different combinations of spectral parameters. The performance is demonstrated in a model material of deuterated poly(methacrylic acid) that contains two H-2 spin populations with similar chemical shifts but different quadrupole splittings. In H-2-exchanged cellulose containing two H-2 spin populations with very similar chemical shifts and quadrupole splittings, the method provides new site-selective information about the molecular dynamics.
Place, publisher, year, edition, pages
2016. Vol. 268, 18-24 p.
Solid state NMR, Magic angle spinning, Spectral resolution, Chemical shift, Longitudinal relaxation
IdentifiersURN: urn:nbn:se:kth:diva-189795DOI: 10.1016/j.jmr.2016.04.014ISI: 000378185900003PubMedID: 27152833ScopusID: 2-s2.0-84967017601OAI: oai:DiVA.org:kth-189795DiVA: diva2:949614
QC 201607212016-07-212016-07-152016-07-21Bibliographically approved