An equimolar mixture of 2.4-dinitrophenylhidrazones (2.4DNPH-ones) providing by acetaldehyde and diacetyl must be analyzed by liquid-chromatographic separation, using the mechanism of repartition with reverse phase; that full papers is for identifi cation the optimal analytical conditions. As mobile phase are utilized various binary mixtures eluent, containing water and methanol, with 0-45% water. By the experimental studies were identified four domains of behavior and two optimal binary mixtures, with 25% and 45% water, thus this is a study on the behavior of binary mixtures mobile phases. The peaks are characterized by values of retention times and by position. The separation processes were appreciated by difference between the retention times of peaks; if the percent of water increase, the values of retention times is higher. When the percent of water is 45%, the difference between the retention times is maxim, associated with a change of peaks position.