In this chapter, the current status of various key technologies for nanoscale characterization and analysis that are indispensable for dealing with nanoethics issues is discussed. Such advanced analytical methodologies include not only the precise shape and size measurements but also the in-depth characterization of various properties of nanomaterials in the bulk states and at the interfaces and surfaces. Especially, nanoscale physicochemical characterization technologies for manufactured and engineered nanomaterials that can be useful for nanoethics assessments have been focused on. Starting from the introduction of the history and status of nano-characterization, major microscopies or spectroscopic imaging tools with the nanoscale spatial resolution are introduced. Interesting applications of such nano-characterization and nano-analysis methods to nanomaterials research are introduced. Besides the major nano-characterization players such as scanning tunneling microscopy and atomic force microscopy, emerging techniques such as helium ion microscopy and tip-enhanced Raman spectroscopy are also introduced. Since some of the nano-characterization techniques are semi-quantitative, the establishment of quantitative methodologies and the standardization of nano-characterization technologies are the next steps toward reliable assessments for nanoethics. Another important direction based on the industrial application needs for engineered nanomaterials is to develop dynamic observation techniques involving operando spectroscopy for physicochemical properties at the nanoscale.