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TECHNICAL REPORTS

Organic Compounds in the Environment

Studying Organic Matter Molecular Assemblage within a Whole Organic Soil by Nuclear Magnetic Resonance

^a Dep. of Chemistry, Louisiana State Univ., Baton Rouge, LA 70803
^b Gordon A. and Mary Cain Dep. of Chemical Engineering, Louisiana State Univ., Baton Rouge, LA 70803
^c School of Plant, Environmental and Soil Sciences, Louisiana State Univ., Baton Rouge, LA 70803
^d Dep. of Chemistry, Southern Univ., Baton Rouge, LA 70813

^* Corresponding author (rlcook{at}lsu.edu).

Received for publication March 19, 2007. This work shows the applicability of two-dimensional (2D) ¹H-¹³C heteronuclear correlation (HETCOR) nuclear magnetic resonance (NMR) spectroscopy to the characterization of whole soils. A combination of different mixing times and cross polarization (CP) methods, namely Lee-Goldberg (LG)-CP and Ramp-CP are shown to afford, for the first time, intra- and inter- molecular connectivities, allowing for molecular assemblage information to be obtained on a whole soil. Our results show that, for the brackish marsh histosol under study, two isolated domains could be detected. The first domain consists of O-alkyl and aromatic moieties (lignocellulose material), while the second domain is comprised of alkyl type moieties (cuticular material). The role of these domains is discussed in terms of hydrophobic organic compound sorption within soil organic matter (SOM), including the possible effects of wetting and drying cycles.

Abbreviations: 1D, one-dimensional • 2D, two-dimensional • CP, cross polarization • FSLG, frequency-switched Lee-Goldberg • HETCOR, heteronuclear correlation • HOC, hydrophobic organic compound • LG-CP, Lee-Goldberg cross polarization • MAS, magic angle spinning • NMR, nuclear magnetic resonance • NOM, natural organic matter • Ramp-CP, ramped amplitude cross polarization • r.f., radio frequency • SOM, soil organic matter • SPINAL, small phase incremental alternation