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In this paper, researchers from Indiana University, US demonstrate superior correlative characterization method compared to conventional spectroscopic techniques to detect CTAB on the surface of Au nanocubes (Au NCs) under hydrated conditions. The presence of residual CTAB on nanoparticle surfaces can significantly impact nanoparticle applications, such as catalysis and sensing. In situ force–distance (FD) spectroscopy and Kelvin probe force microscopy (KPFM) measurements on Park NX10 AFM was used to characterize adsorbed CTAB, while correlative in situ AFM and scanning electron microscopy (SEM) measurements were used to evaluate sequential steps of CTAB removal from Au NCs across hydrated and dehydrated environments, respectively.