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@ARTICLE{Conte:449,
author = {Conte, P. and Berns, A. E.},
title = {{D}ynamics of {C}ross {P}olarization in {S}olid {S}tate
{N}uclear {M}agnetic {R}esonance {E}xperiments of
{A}morphous and {H}eterogeneous {N}atural {O}rganic
{S}ubstances},
journal = {Analytical sciences},
volume = {24},
issn = {0910-6340},
address = {Tokyo},
publisher = {Japan Society for Analytical Chemistry},
reportid = {PreJuSER-449},
pages = {1183 - 1188},
year = {2008},
note = {P.C. acknowledges Forschungszentrum Julich GmbH (Germany)
for enabling him to perform experimental work as visiting
scientist at the NMR center of the Institute of Chemistry
and Dynamics of the Geosphere, Institute 4: Agrosphere. The
authors are grateful to Dipl.-Ing. H. Philipp (FZJ) for his
assistance in sample preparation. This paper was partially
funded by University of Palermo within a project titled
"Nuovi processi sostenibili per la bonifica di suoli
contaminati".},
abstract = {Nuclear magnetic resonance (NMR) experiments on carbon-13
in the solid state were done with cross polarization (CP)
and magic angle spinning (MAS) in order to overcome the low
NMR sensitivity of C-13 and the chemical shift anisotropy,
respectively. In the present research, CPMAS C-13-NMR
spectra were collected by modulating the contact time needed
for cross polarization (variable contact times experiments,
VCT) on two different humic acids (a soil-HA and a coal-HA).
VCT data were fitted by a model containing either a
monotonic or a non-monotonic cross polarization term. The
non-monotonic model, which fitted the experimental results
better than the monotonic one, provided two
cross-polarization rates, thereby suggesting that two
different mechanisms for the energy transfer from protons to
carbons arise in amorphous and heterogeneous humic
substances. The first mechanism was a fast proton-to-carbon
energy transfer due to protons directly bound to carbons.
The second mechanism was related to a slow transfer mediated
by local segmental motions. Different domains in the humic
acids were identified. Soil-HA was made of rigid domains,
containing mainly aromatic and carboxylic moieties, and fast
moving domains, containing alkyl, C-O and C-N groups.
Coal-HA showed a rigid aromatic domain that was
differentiated from a very mobile domain made of alkyl and
COOH groups.},
keywords = {J (WoSType)},
cin = {ICG-4},
ddc = {540},
cid = {I:(DE-Juel1)VDB793},
pnm = {Terrestrische Umwelt},
pid = {G:(DE-Juel1)FUEK407},
shelfmark = {Chemistry, Analytical},
typ = {PUB:(DE-HGF)16},
UT = {WOS:000259584800019},
doi = {10.2116/analsci.24.1183},
url = {https://juser.fz-juelich.de/record/449},
}