This study deals with the determination of the relative abundance of the oxide layer in the near-surface volume of aluminum nanoparticles of 50–100 nm in diameter. They are bombarded with a sequence of single projectiles of Au4004+ accelerated to 136 keV. The ionized ejecta from each impact are recorded individually which allows identification of ions emitted from a surface volume of ~10 nm in diameter and 5–10 nm in depth. The mode of analyzing ejecta individually from each single cluster impact is a means to apply mass spectrometry in nanovolumes.