Volatile compounds oils play a significant role in perfumery, cosmetic, medicinal and pharmaceutical industries. In our protracted research for new useful essential oils, a volatile oil from Aloe ferox was obtained by prolonged hydrodistillation. This volatile oil was subjected to GC/MS analysis to identify the major constituents of the oil. The major constituents identified were as follows: 3, 6 octatriene (23.86%), 3-cyclohexane-1-hetanol (7.31%), Bornylene (5.24%), 1, 3-cyclopentadiene (4.07) and 5-methyl- 3-heptanol (3.92%). A significant number of other volatiles were also identified but in minor concentrations.