Nanoparticles have been widely used as vectors for bioactive cargo due to their high therapeutic index. Despite their attractiveness for safe and efficacious drug delivery, nanoparticles are known to suffer from rapid systemic clearance. PEGylation, conjugation of the nanocarrier with polyethylene glycol (PEG) chains, is one of the strategies that has been developed to combat this challenge. PEGylation confers steric stability to the nanoparticle through a “stealth” coating which masks the core of the nanoparticle thereby evading a response from the immune and reticuloendothelial systems. PEG chains are also critical to ensure the stability of the nanoparticles as they prevent aggregation in colloidal suspensions. Due to the crucial role they play in developing an optimal formulation, it is imperative to establish robust analytical tools to characterize the surface topography and morphology of PEGylated nanocarriers. Surface analytical techniques are frequently modified to enable characterization at a nanoscale. This chapter describes the major characterization tools we have at our disposal to effectively analyze critical surface attributes. Examples of each technique are also provided to demonstrate their application, benefits, and drawbacks.