Adequately separated signals in the nuclear megnetic resonance spectra of mixtures of cyclocitrals were assigned to the individual components. This assignment allowed direct integration of the signals of interst and calculation of the percentages of α-cyclocitral, β-cyclocitral,para-cymene, and 1-acetyl-4, 4-dimethyl-1-cyclohexene. The rapidity and nondestructive nature of the nuclear magnetic resonance analysis are superior to the fractional crystallization of the semi-carbazones and gas chromatography techniques previously utilized.