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 13C and the chemical shift anisotropy, respectively. In the present research, CPMAS 13C-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 nonmonotonic 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.

Conte, P., Berns, A.E. (2008). Dynamics of cross polarization in solid state nuclear magnetic resonance experiments of amorphous and heterogeneous natural organic substances. ANALYTICAL SCIENCES, 24, 1183-1188.

Dynamics of cross polarization in solid state nuclear magnetic resonance experiments of amorphous and heterogeneous natural organic substances

CONTE, Pellegrino;
2008-01-01

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 13C and the chemical shift anisotropy, respectively. In the present research, CPMAS 13C-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 nonmonotonic 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.
2008
Conte, P., Berns, A.E. (2008). Dynamics of cross polarization in solid state nuclear magnetic resonance experiments of amorphous and heterogeneous natural organic substances. ANALYTICAL SCIENCES, 24, 1183-1188.
File in questo prodotto:
File Dimensione Formato  
2008_Conte&Berns_Anal_Sci_24_1183-1188_(2008).pdf

Solo gestori archvio

Dimensione 720.16 kB
Formato Adobe PDF
720.16 kB Adobe PDF   Visualizza/Apri   Richiedi una copia

I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.

Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/10447/35843
Citazioni
  • ???jsp.display-item.citation.pmc??? ND
  • Scopus 16
  • ???jsp.display-item.citation.isi??? 16
social impact