The proposed approach relies on successive dilution of a solution containing a sample with standard addition and on titration of the solutions obtained until receiving a signal lower than the signal measured for the sample alone. Equations are derived for subsequent dilution factors for the automatic flow injection system applied. The overall calibration strategy including the possibility of prediction of the number of required standard solutions and of positioning the sample signal within the calibration range is presented. The method has been tested on the spectrophotometric determination of hydrochloric acid at two concentration levels (0.193 and 1.21 mol L-1) with sodium hydroxide as titrant. The results of accuracy better than |3.9|% (RE) and repeatability better than 1.3% (RSD) were obtained. The method has been applied to the determination of total acidity in vinegars and soft drinks. The average time necessary to analyze one sample is about 10 min.