Optimization of a microwave-assisted derivatization-extraction procedure for the determination of chlorophenols in ash samples

A procedure for the determination of 17 chlorophenolic compounds in ash samples obtained from the incineration of waste materials is described. Analytes were simultaneously derivatized with acetic anhydride in presence of triethylamine (TEA), and extracted from the sample in a mixture of n-hexane acetone using a microwave system equipped with closed extraction vessels. Influence of five experimental parameters (volume of TEA and acetic anhydride, extraction time and temperature, as well as the volume of n-hexane acetone) on the yield of the derivatization-extraction procedure was systematically studied using a uniform experimental design at four levels, followed by a conventional factorial design at two levels. Under optimal extraction conditions, recoveries from 72 to 94% were obtained for a spiked ash sample with a carbon content of 8.7%. Quantification limits of the proposed procedure ranged from 2 to 5 ng/g using GC-MS as detection technique. The proposed method was applied to the determination of chlorophenols in three ash samples obtained from different incineration plants. Total chlorophenol contents of 423 and 135 ng/g were found in two of these samples. (C) 2003 Elsevier B.V. All rights reserved.