Electroanalytical techniques are a group of analytical practices that primarily focuses on electrical and chemical parameters. It usually studies the response of an analyte under a specific applied potential or current in an electrochemical cell. These techniques proved their efficiency and cost effectiveness. Electromotive materials can be analyzed accurately even at nano or picomolar levels. Electroanalytical peculiarities of nanomaterials especially nanoscale carbon materials opened new avenues in the current research. The first part of this chapter is an introduction of different electroanalytical techniques available. The second part briefly explains the electrochemical characterization techniques used particularly for carbon-based nanomaterials; namely carbon nanotubes (CNTs), carbon nanomaterials, graphene, carbon-based quantum dots, etc. Electroanalytical sensing applications are mainly focused throughout the chapter and giant biomolecules as well as tiny environment pollutants like heavy metal ions, dyes, pesticides, and organic molecules.