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Currently available methods for analyzing haloacetic acids (HAAs) and ketoacids in water generally require the use of diazomethane for sample derivatization. This article proposes methods based on a less toxic, alternative methylating agent. The objectives of this study were to develop and evaluate a liquid-liquid microextraction-acidic methanol derivatization procedure for HAA analysis and a microextraction-PFBHA-acidic methanol derivatization procedure for ketoacid analysis. Includes 23 references, tables, figures.