The detection of the dry alcoholate corrosion of aluminium is vital to design a corrosion resistive aluminium alloy for the storage and transportation of biofuel (methanol or ethanol). By synthesizing an Al³⁺ fluorescent probe operable in an alcoholic medium, we quantified the alcoholate corrosion in terms of the fluorometrically estimated soluble alkoxide (Al(OR)₃) generation under nitrogen atmosphere. With time, a linear increase in corrosion with specific aluminium dissolution rate constants ∼2.0 and 0.9 μg per day per cm² were estimated for aluminium and Al-7075 alloy, respectively. During open atmosphere monitoring, the adsorbed moisture converted small extent of Al(OR)₃ to the insoluble Al(OH)₃ at the alloy surface which retarded the alcoholate corrosion appreciably.