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TECHNICAL REPORTS

A Solid-Phase Microextraction Chamber Method for Analysis of Manure Volatiles

USDA-ARS, U.S. Meat Animal Research Center, P.O. Box 166, Clay Center, NE 68933. D.N. Miller, current address: USDA, ARS, Soil and Water Conservation Research Unit, 121 Keim Hall, East Campus, Lincoln, NE 68583

^* Corresponding author (dmiller15{at}unl.edu)

Received for publication February 15, 2006. Odors from livestock operations are a complex mixture of volatile carbon, sulfur, and nitrogen compounds. Currently, detailed volatiles analysis is both time consuming and requires specialized equipment and methods. This work describes a new method that utilizes a dynamic flux chamber, solid-phase microextraction (SPME), and gas chromatography–mass spectroscopy (GC–MS) to describe and compare the odorous compounds emitted from cattle and swine feces. Evaluation of method parameters produced a protocol for comparing relative emissions based on fixed sample temperature (20°C) and exposed surface area (approximately 523 cm²), air flow rates (1 L min^–1 or 16 cm s^–1), SPME exposure time (5 min), and chamber cleaning procedures (70% ethanol rinse and drying for 30 min at 105°C) to minimize cross-contamination between samples. A variety of volatile organic compounds (VOCs) including alcohols, volatile fatty acids, aromatic ring compounds, ketones, esters, and sulfides were routinely detected and the relative emissions from fresh and incubated (37°C overnight) swine and cattle feces were compared as a measure of potential to produce odorants during manure storage. Differences in the types and relative quantities of volatiles emitted were detected when animal species (cattle or swine), diet, fecal incubation, or sample storage conditions (20, 4, or –20°C) were varied.

Abbreviations: DM, dry matter • GC, gas chromatography • IC, ion current • MS, mass spectroscopy • OM, organic matter • SPME, solid-phase microextraction • VFA, volatile fatty acids • VOC, volatile organic compounds

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