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A method for the separation and identification of aldehyde isomers depends upon the separation of an isomer approximately 90% pure b y large volume gas-liquid partition chromatography. The separated aldehyde is examined by nuclear magnetic resonance to determine the number of a-hydrogens, CHa-, CHx-, and CHgroups and by infrared spectroscopy to establish the presence or absence of -(CH2)3-or -(CH2)n-groups, where R is equal to or greater than 4. Finally, the aldehyde is reduced to a hydrocarbon by the Wolff-Kishner reaction and the hydrocarbon identified b y comparison with API standards by gasliquid partition chromatography. The combined information from nuclear magnetic resonance, infrared spectroscopy, and the reduction step makes possible the identification of separated aldehyde isomers. This method has been used for the separation and identification of several isomers in an octyl aldehyde mixture derived from the oxo process. HE separation and identification of