A simple method for the determination of nitrilotrioacetic acid (NTA) and ethylene-diaminetetraacetic acid (EDTA) beside other aminepolycarboxylic acids in surface water and waste water by gas chromatography is described. First, water samples were dried by evaporating. The free acids were esterified by the mixture of n-butyl alcohol and acetyl chloride. The prepared n-butyl esters were identified by the cappillary GC-MS and then determined by the cappilary GC-FID. n-Butyl esters of aminepolycarboxylic acids NTA, EDTA, CDTA and DTPA were characterized by retention times under the chosen conditions.