The quantitative distribution of volatile compounds in the pulp, cloud, and serum of a freshly squeezed orange juice (cv. Naveline) was measured. Juice monoterpene and sesquiterpene hydrocarbons were primarily recovered from the pulp (74.0 and 87.2%, respectively) and cloud (7.3 and 14.9%, respectively). Esters and monoterpene alcohols were mainly found in the serum (90.4 and 84.1%, respectively). Long chain aliphatic aldehydes tend to concentrate in the pulp. The relative proportions of individual volatile compounds were similar in the pulp and cloud. Pulp and cloud alcohol insoluble residues exhibited similar compositions; half of them are made of nonwall proteins, and the rest are made of cell wall materials. Pulp and cloud total and neutral lipids had similar fatty acids distributions, although the cloud was much richer in total lipids than the pulp. No relationship was found between the retention of aroma compounds in the pulp or cloud and their AIR and lipid content or composition.