Chlorinated phenolics analytical methods

Analytical methods for 12 chlorinated phenolics and adsorbable organic halides (AOXs). Samples of air emissions and water discharges from each mill must be tested using the laboratory methods included in the rule. The new methods will enable more timely and accurate measurements of releases of these pollutants to the environment and will be used to ensure compliance with air emission and water discharge permit limits... 

Chlorinated phenolic compounds in air-dried sediments collected downstream of chlorine-bleaching mills were treated with acetic anhydride in the presence of triethylamine. The acetylated derivatives were removed from the matrix by supercritical fluid extraction (SEE) using carbon dioxide. The best overall recovery for the phenolics was obtained at 110°C and 37 MPa pressure. Two SEE steps had to be carried out on the same sample for quantitative recovery of the phenolics in weathered sediments. The SEE unit was coupled downstream with a GC for end analysis . Off-line SEE followed by capillary GC was applied in the determination of phenol in polymeric matrices . The sonication method recommended by EPA for extraction of pollutants from soil is inferior to both MAP and SEE techniques in the case of phenol, o-cresol, m-cresol and p-cresol spiked on soil containing various proportions of activated charcoal. MAP afforded the highest recoveries (>80%), except for o-cresol in a soil containing more than 5% of activated carbon. The SEE method was inefficient for the four phenols tested however, in situ derivatization of the analytes significantly improved the performance . 

Phenols The term phenols is used to designate a series of hydroxyl derivatives of benzene, with phenol as the parent compound. These compounds come from paper mills and cellulose factories as well as from degradation of pesticides such as carbaryl. Disinfecting treatments of chlorine-containing waters produce chlorophenols, which cause a persistent taste. Analytical control of these compounds is commonly performed by chromatographic or photometric methods. 

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