An HPLC procedure for the determination of linear alcohol polyethoxylates in surface water, waste water, and detergents is described. After extraction of the alcohol ethoxylates into an organic phase the alcohol ethoxylates are derivatized with phenyl isocyanate to apply an UV detection. A reversed-phase HPLC procedure is used to separate different ethoxylate species by their different alkyl chain length. A normal phase procedure is employed to separate alcohol polyethoxylates by their different number of ethoxylate groups in the molecule.