Analysis of Phenolic residues in soil as free and acetylated derivatives by capillary gas chromatography equipped with fid, ECD and MSD

Abstract
A multiresidue method was developed to analyse phenol, cresols, xylenols and chlorophenols in soil or sediment. Soil samples were extracted with acetone in an ultrasonic bath and the extracts were divided into two fractions for free and acetylated compounds. Extract fractions were then analysed in a GC‐FID with DB‐1 capillary column and in a GC‐ECD with HP‐5 capillary column. Confirmation of phenol identity was carried out by GC‐MSD in the selected ion monitoring (SIM) mode. Recoveries of phenol were almost at the same level 92.4 and 97.6% for free and acetylated derivatives respectively. Recoveries of cresols were lower at 62.3–65.2% and were increased after acetylation up to 81.9–96.6%. Recoveries of 2,3‐, 2,4‐, 2,5‐, and 2.6‐ xylenols also increased from a level of 65.2–72.9% for free compounds to 73.6–95.8% for their acetates. On the contrary, recoveries of 3,5‐ and 3,5‐ xylenols seem to decrease slightly after acetylation from 102.5–125.3% to 97.7–107.5%. Finally, recoveries of tri‐ tetra‐ and pentachlorophenols were strongly increased by the acetylation from 91.3–116.4% to 109.3–130.2%.

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