The dissolution of intermetallic phases in AA 2024-T3 aluminum alloy sheet was investigated during a coating pretreatment sequence. The atomic emission spectroelectrochemistry (AESEC) technique was used to quantitatively measure the dissolution rates of individual alloying elements during a complete pretreatment sequence. The results demonstrate the significant selective dissolution of Al in 1.25 M NaOH, leading to the enrichment of alloying elements such as Cu. Subsequent 2.8 M HNO 3 treatment contributes toward dissolving the excess residual layer and passivates the alloy matrix, however the presence of a residual Cu layer at the alloy surface was evidenced. The real-time alloy dissolution profiles are presented herein, and discussed in the context of the surface morphology via microscopy. The surface treatment of aluminum (Al) alloys is required prior to the application of corrosion protective coatings.1 Protective coatings are essential in order to allow microstructurally complex alloys, which are nominally prone to localized corrosion, 2-7 to be used in service; particularly in aerospace applications.8 Coatings for Al-alloys are nominally multilayered coating 'systems', with the first coating being a chemical conversion coating. The surface treatment prior to this chemical conversion coating is as important as the coating itself, since it determines the efficacy of any conversion coating.1,9 Such surface treatment, often termed pre-treatment, generally involves alkaline etching and acid pickling. Sodium hydroxide (NaOH) is often used to remove any organic residue and also to remove several micrometers of the alloy surface.10 This is followed by acid pickling, usually performed in nitric acid (HNO 3 ) to remove any residue, products, films, or particles remnant from -or caused by -the prior alkaline step. The purpose of surface pretreatment is to provide a chemically homogeneous surface chemistry prior to subsequent coating processes. The chemical heterogeneity of the Al-alloy surfaces is due to the many alloying elements present, such as copper (Cu), magnesium (Mg), iron (Fe) and manganese (Mn). Cu improves the mechanical properties of AA 2024-T3 11 however decreases corrosion resistance due to stimulating various phases which serve as local electrochemical entities, in addition to raising the alloy potential to above the pitting potential of the matrix phase 7,[12][13][14][15][16] . This element is considered to be a major contributor to the localized corrosion of Al 2,17,18 and its elimination is one of primary goals of aluminum alloy surface pretreatment.Knowledge of the elementary dissolution kinetics during the pretreatment sequence would be very useful for the development of surface treatment formulations, however, this information is often very difficult to obtain. In situ monitoring of the corrosion reactions during surface treatment is difficult as the corrosion reactions occur within a relatively short time with large reaction rates and may involve extensive precipitation of dissolution products a...