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TECHNICAL REPORTS
Waste Management

Characterization of Sewage Sludge Organic Matter Using Solid-State Carbon-13 Nuclear Magnetic Resonance Spectroscopy

^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 November 14, 2002. Six sewage sludges from five sewage treatment plants in Australia were characterized using solid-state ¹³C nuclear magnetic resonance (NMR) spectroscopy. Spectra were acquired both before and after removal of mineral components through treatment with hydrofluoric acid (HF). Carbon mass balance indicated that little organic matter was lost on HF treatment, which significantly improved NMR sensitivity and spectral resolution, and decreased acquisition time and hence cost of NMR analysis. Two NMR techniques were used, the standard cross polarization (CP) technique and Bloch decay (BD). The BD technique had not been applied previously to the analysis of sewage sludge. For each sludge sample, both before and after HF treatment, the BD spectrum contained significantly more alkyl carbon. Spin counting, another technique applied to sewage sludge here for the first time, showed that the BD spectra of the HF-treated sludges were quantitative, while approximately 30% of the CP NMR signal went undetected. The discrepancy between CP and BD spectra was attributed to the presence of alkyl carbon with such high molecular mobility that the efficiency of cross polarization is affected. This study shows that sewage sludge organic matter is significantly different in chemistry to soil organic matter and has implications for the application of sewage sludge to agricultural land.

Abbreviations: BD, Bloch decay • C_obs, proportion of potential carbon-13 nuclear magnetic resonance signal intensity detected in nuclear magnetic resonance spectrum • CP, cross polarization • HF, hydrofluoric acid • NMR, nuclear magnetic resonance • T₁H, proton spin-lattice relaxation rate in the rotating frame

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JEQ 2003 32: 1167-1172. [Full Text]  

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