The research investigates the liberation size of composite particles in Iperindo lode deposit at Ilesha goldfield in Osun state, Nigeria. The sample of the gold ore was sourced from Iperindo and 3 kilograms of gold ore was prepared by crushing and grinding to 100% passing 710µm sieve. 300 grams of the prepared ore was charged into set of sieves arranged in √2 i.e from 500 µm to-45 µm mounted on automated sieve shaker and operated for 20 minutes. Atomic Absorption Spectrometry (AAS) and X-ray Fluorescence (XRF) were used to determine the elemental and chemical composition of the ore. The chemical analysis of the crude sample via X-ray Fluorescence Spectrometry (XRF) revealed that the crude sample contain high content of Fe, Ti, Mn and K. The traces of K, Ba and Rb, shows that composite particles in Iperindo gold-bearing rock ore was formed as a result of hydrothermal alteration and the characterization of the sieve fractions by Atomic Absorption specteometey shows-63µm +45µm has the highest gold content when compare to other seive fraction. This indicates that the optimum liberation size of gold in Iperindo gold-bearing rock is 45µm. Processing of gold, which is economical viable from the ore deposit using froth flotation is desirable. Hence, efficient flotation of the mineral particle at the optimum liberation size of 45µm which lies favorably within the range of 10-150µm sighted from literature, will lead to good recovery of the gold particle.