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TECHNICAL REPORTS
Waste Management

Advanced Solid-State Carbon-13 Nuclear Magnetic Resonance Spectroscopic Studies of Sewage Sludge Organic Matter

Detection of Organic "Domains"

^a Dep. of Soil and Water, Waite Agricultural Research Institute, Univ. of Adelaide, Glen Osmond, South Australia 5064, Australia
^b Environment Agency, National Centre for Ecotoxicology & Hazardous Substances, Wallingford, Oxfordshire, OX10 8BD, UK

^* Corresponding author (ronald.smernik{at}adelaide.edu.au)

Received for publication December 29, 2002. Two novel solid-state ¹³C nuclear magnetic resonance (NMR) spectroscopic techniques, PSRE (proton spin relaxation editing) and RESTORE [Restoration of Spectra via T_CH and T₁H (T One Rho H) Editing], were used to provide detailed chemical characterization of the organic matter from six Australian sewage sludges. These methods were used to probe the submicrometer heterogeneity of sludge organic matter, and identify and quantify spatially distinct components. Analysis of the T₁H relaxation behavior of the sludges indicated that each sludge contained two types of organic domains. Carbon-13 PSRE NMR subspectra were generated to determine the chemical nature of these domains. The rapidly relaxing component of each sludge was rich in protein and alkyl carbon, and was identified as dead bacterial material. The slowly relaxing component of each sludge was rich in carbohydrate and lignin structures, and was identified as partly degraded plant material. The bacterial domains were shown, using the RESTORE technique, to also have characteristically rapid T₁H relaxation rates. This rapid T₁H relaxation was identified as the main cause of underrepresentation of these domains in standard ¹³C cross polarization (CP) NMR spectra of sludges. The heterogeneous nature of sewage sludge organic matter has implications for land application of sewage sludge, since the two components are likely to have different capacities for sorbing organic and inorganic toxicants present in sewage sludge, and will decompose at different rates.

Abbreviations: BD, Bloch decay • CP, cross polarization • NMR, nuclear magnetic resonance • PSRE, proton spin relaxation editing • RESTORE, Restoration of Spectra via T_CH and T₁H (T One Rho H) Editing • T₁H, proton spin-lattice relaxation rate in the static frame • T₁H, proton spin-lattice relaxation rate in the rotating frame • T_CH, rate of transfer of polarization from ¹H to ¹³C nuclei during the contact time of the cross polarization experiment • VCT, variable contact time • VSL, variable spin lock

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