A simple and precise potentiometric titration method has been developed for the determination of milligram quantities of alkyl ketene dimer (AKD) in non-aqueous solvents. It involves the addition of chloroform solutions of AKD to an excess of an organic base followed by the titration of excess base with perchloric acid in glacial acetic acid. The method was used to determine non-reacted AKD extracted from hand-sheets: our results agreed with those obtained by capillary gas chromatography. The method was also used to monitor the stability of AKD formulations. Wood resin components and stearone, a hydrolysis product of AKD, do not interfere.