Chemical derivatization analysis of phenols. Part VI. Determination of chlorinated phenolics in pulp and paper effluents.

Based on the in-situ acetylation procedure, a method for the determination of 31 chlorinated phenols, guaiacols, catechols, syringols, and vanillins in pulp and paper effluent samples has been successfully developed. Except for 4-chlorocatechol, this procedure provided satisfactory recovery for all phenols at 3 levels of fortification, namely, 400, 40, and 4 micrograms/L. The acetyl derivatives were analyzed by gas chromatography using a 30 m DB-5 capillary column interfaced to an electron-capture detector. Mass spectral abundance data for the characteristic ions of the acetyl derivatives were used for confirmation of compound identities. By operating a mass selective detector in the selected ion monitoring mode, this procedure was further extended to the monochlorinated phenolics. Using a 50 mL effluent sample, the method detection limit was 0.5 micrograms/L for all except the monochlorinated compounds, which had a detection limit of 1 microgram/L. Several effluent samples from a Canadian paper mill were analyzed by this procedure and the results are presented.