SUMMARY: The aldehydes, ketones and esters in the volatile portion of Valencia orange oil have been isolated and identified. Seventeen aldehydes and ketones and three esters are included, 10 of which have never been identified as constituents of Valencia oil. Cis‐ and trans‐limonene oxide have also been found to occur in the same fraction. This is the first time that these compounds have been identified in cold‐pressed orange oil. A series of five homologous α,β‐unsaturated aldehydes were isolated and partially characterized. Copyright © 1969, Wiley Blackwell. All rights reserved