X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectrometry (ToF-SIMS) were used to analyse the surface modifications of AA-2024-T3 induced by model pre-treatment baths such as H2SO4, HNO3, and in a mixture of both acids. These acids are commonly used for pickling treatment, applied before conversion coating deposition.ToF-SIMS and XPS measurements showed a significant copper enrichment in metallic and oxidised states, localised at the oxide/metal interface. The sulphuric acid treatment led to the highest Cu enrichment. A lower dissolution rate of AA-2024 was observed by inductively coupled plasma optical emission spectroscopy (ICP-OES). It was concluded that the surface enrichment in Cu is mainly associated with dealloying of intermetallic particles by selective dissolution of the less noble elements.