Citrus aurantifolia essential oils are volatile phytochemicals obtained from various part of the plant which has found wide range of domestic, medicinal and industrial applications. The research seeks to investigate the effect of time of harvest on the yield and phytochemical composition of Citrus aurantifolia leaf oil. Pulverized leaves of Citrus aurantifolia harvested in the morning (7a.m) and afternoon (2p.m) on the same day were separately subjected to hydro-distillation which yielded 0.4 and 0.5% (v/w) of the volatile oil respectively. Analyses of the oil harvested in the morning (7am) revealed the predominance of oxygenated terpenes which constituted 58.3%  of the oil. The principal constituents were; isolimonene (22.2%), neral (22.2%), citral (21.5%), caryophyllene (4.3%), and α-geranyl acetate (4.1%). Furthermore, the leaf oil from the afternoon (2pm) harvest also showed predominance of oxygenated terpenes which constituted 57.7%. The principal constituents in the oil were; limonene (20.2%), neral (24.5%), citral (10.3%), caryophyllene (5.4%), and α-geranyl acetate (3.3%). This study established   that there was compositional variation in the leaf essential oil obtained from the different time of harvests.