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A New Way to Use Solid-State Carbon-13 Nuclear Magnetic Resonance Spectroscopy to Study the Sorption of Organic Compounds to Soil Organic Matter

School of Earth and Environmental Sciences, The University of Adelaide, Waite Campus, Urrbrae, South Australia 5064, Australia

View larger version (24K): [in a new window]   Fig. 1. (a) Carbon-13 cross polarization (CP) nuclear magnetic resonance (NMR) spectra of HF-treated soil (control soil). (b)–(f) Carbon-13 CP NMR spectra of HF-treated soil spiked with: (b) benzoic acid, (c) benzophenone, (d) naphthalene, (e) phenanthrene, and (f) palmitic acid. (g)–(k) Difference spectra generated by subtracting spectrum (a) from spectra (b)–(f), respectively; these difference spectra represent sorbed (g) benzoic acid, (h) benzophenone, (i) naphthalene, (j) phenanthrene, and (k) palmitic acid. (l)–(p) Carbon-13 CP NMR spectra of neat 13C-labeled compounds: (l) benzoic acid, (m) benzophenone, (n) naphthalene, (o) phenanthrene, and (p) palmitic acid. Spinning sidebands are marked with an asterisk (*).

View larger version (20K): [in a new window]   Fig. 2. Carbon-13 proton spin relaxation editing (PSRE) subspectra of HF-treated soil and HF-treated soil spiked with 13C-labeled compounds.

View larger version (11K): [in a new window]   Fig. 3. Carbon-13 cross polarization (CP) nuclear magnetic resonance (NMR) spectra of HF-treated soil spiked with 13C-labeled palmitic acid acquired with recycle delays of (a) 1, (b) 5, and (c) 20 s.

View larger version (18K): [in a new window]   Fig. 4. Carbon-13 cross polarization (CP) nuclear magnetic resonance (NMR) spectra of melanoidins without (control) and with (spiked) sorbed 13C-labeled naphthalene. Difference spectra were generated by subtracting control spectra from corresponding spiked spectra.

View larger version (31K): [in a new window]   Fig. 5. A selection of 13C inversion–recovery NMR spectra (showing spectra for 8 of the 13 recovery delays used) for the melanoidins and the HF-treated soil, each spiked with 13C-labeled naphthalene.