The photo degradation of n-hexacosane (n- C26H54) by coupled ZnO -Sb2O3 was investigated. The coupled ZnO-Sb2O3 was prepared by using pure solid materials of ZnO -Sb2O3( 1: 1 ) then calcend in suitable furnace for five hours The photodegradation of n-hexacosane using coupled ZnO-Sb2O3, which is achieved by the irradiation of suspended solution consists of 1x10-4Mn-hexacosane dissolved in 100 cm3 of n-nonane with 0.1 g of coupled ZnO-Sb2O3 by using tungsten lamp from external source of a Pyrex photo reaction cell of 100 cm3 at 298.15 K.. Several experiments were carried out at various conditions to reach the best degradation of n-hexacosane using coupled ZnO-Sb2O3. These experiments include the amount of n- hexacosane on fixed mass of ZnO-Sb2O3, the amount of coupled ZnO-Sb2O3, and the temperature effects .The main photolytic products of n-hexacosane photo degradation processes were heptane, octane, nonane, dodecane and tetradecane. Gas chromatographic using FID and IR, UV-Visible spectrophotometric techniques were used to identify the photocalalytic degradation products. Also the coupled ZnO - Sb2O3 studied by using X-Ray Diffraction spectrometric technique.