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The optimization procedure for the reversed-phase HPLC separation of 1-naphthyl isocyanate derivatives of linear alcohol polyethoxylates (LAEs) is reported. Using a C 1 8 -bonded silica stationary phase and acetonitrile-water mixtures as mobile phase, different trends in the chromatographic separation of selected 1-tetradecanol polyethyleneglycol ether ethoxymers were observed. In the investigated range of acetonitrile-mobile phase volume ratio ( ), the elution order of the ethoxymers was inverted by increasing the organic solvent content of the mobile phase, and the mobile phase composition was found which provides the co-elution of the tested compounds. On the basis of the trends of capacity factor logarithm (log k ) versus the number of ethoxy units (n) at different , an increased retention by increasing was also predicted for higher ethoxymers. The separation under the same chromatographic conditions of a C 1 2 -C 1 8 LAE mixture with an average number of 10 ethoxy units, confirmed the strong variability of LAE chromatographic behaviour in the investigated range. The isoeluting conditions found for the C 1 4 LAE ethoxymers were also applied successfully to the homologue-by-homologue separation of the C 1 2 -C 1 8 LAE mixture.
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