A method is reported for the sensitive, simultaneous determination of mono-(MFA), di-(DFA), and trifluoroacetates (TFA) by ion chromatography (IC). These species were separated using a Dionex AS17 anion-exchange column employed with a potassium hydroxide gradient (via a Dionex EG40 eluent generator) and suppressed conductivity detection. The fluoroacetates were successfully separated from a range of inorganic and organic species likely to be present in environmental samples, in a total analysis time of 35min (including re-equilibration of the column). Detection limits for mono-, di- and trifluoroacetate were 21, 38 and 36μg/l, respectively, determined using a signal-to-noise ratio of 3, and were obtained using a sample injection volume of 50 l. Precision was less than 0.83% relative standard deviation (RSD) for replicate injections performed over a period of 30 days. The method was applied to the determination of monofluoroacetate in river water samples and also in carrot baits.