Accurate quantification of aromaticity and nonprotonated aromatic carbon fraction in natural organic matter by 13C solid-state nuclear magnetic resonance

Environ Sci Technol. 2004 May 1;38(9):2680-4. doi: 10.1021/es034770x.

Abstract

An improved approach for accurately determining the aromatic carbon fraction (fa) and nonprotonated aromatic carbon fraction (faN) in natural organic matter by solid-state 13C NMR is described. Quantitative peak areas are obtained from direct polarization 13C nuclear magnetic resonance (NMR) under high-speed magic angle spinning (MAS). The problem of overlap between aromatic and alkyl carbon resonances around 90-120 ppm in 13C NMR spectra is solved by a 13C chemical shift anisotropy (CSA) filter technique. After correction for residual spinning sidebands, an accurate value of the aromaticity fa is obtained. To obtain a quantitative faN fraction, dipolar dephasing was adapted for high-speed MAS 13C NMR; the separation of the signals of nonprotonated alkyl and aromatic carbons was achieved by CSA filtering plus dipolar dephasing. The method is demonstrated on a peat humic acid, yielding fa = 45 +/- 2% and faN = (0.64 +/- 0.07) x 45%.

Publication types

  • Evaluation Study
  • Research Support, U.S. Gov't, Non-P.H.S.

MeSH terms

  • Carbon / analysis*
  • Carbon Isotopes / analysis
  • Environmental Pollutants / analysis*
  • Hydrocarbons, Aromatic / analysis*
  • Magnetic Resonance Spectroscopy
  • Organic Chemicals
  • Reproducibility of Results

Substances

  • Carbon Isotopes
  • Environmental Pollutants
  • Hydrocarbons, Aromatic
  • Organic Chemicals
  • Carbon