This book presents a lucid and systematic exposition of the preparation, characterization, and spectroscopy of carbonaceous namaterials and started with the general introduction to nascience, review of carbon namaterials, and related experimental techniques. This book attempts to highlights to design new, inexpensive, and single step procedure for the bulk synthesis of carbon naparticles. Special attention was made to dispersion of carbon naparticles in variety of solvents, their growth kinetics, and interaction with surfactants, including common, bio and pulmonary surfactants. Interestingly the observation of fluorescent carbon naparticles from organic solvents dispersion without any surface functionalization and their detailed spectroscopic study also presented. This book will be useful for engineers, chemists, and na-scientists interested to work in the area of carbon namaterials for application in their areas and also can be used as a textbook or used by students and carbon research groups on their own as long as they have some basic kwledge of carbon namaterials and fluorescence spectroscopy.