Abstract: Non-aqueous titrimetric determination of DMAA,in the presence of methylamine and dimethylamine,was carried out by using glacial acetic acid as solvent,a mixture of formic acid and acetic anhydride as acylating agent,a 0.1 mol·L-1 glacial acetic acid solution of HClO4 as titrant,and 10 g·L-1 glacial acetic acid solution of crystal violet as indicator.Water contents below 5% in the titration solution cause relative deviations less than 1% but the error increases with the increase of water content.The addition of 10% by volume of chloroform improves the sharpness of color-change of the end-point.The proposed method is comparable to the GC method by the simplicity of operation and accuracy of results.