Polystyrene functionalized at both ends (telechelic polymer) with epoxide groups (epoxy–PS–epoxy) was reacted with carboxylated multiwall carbon nanotubes (COOHMWNT) in solution in order to graft polymer chains at both ends onto the MWNT surface, forming loops. FT‐IR spectroscopy was employed to monitor the formation of aromatic esters and to quantify the amount of telechelic grafted to the nanotube surface as a function of reaction time. When the samples were further annealed in the melt, an increase in the aromatic ester peak was observed, indicating that the unreacted chain ends further grafted to MWNT surfaces to form loops. By reacting the grafted nanotube samples further with monocarboxy terminated poly(4‐methylstyrene) (COOHP4MS), the amount of epoxy–PS–epoxy that had only reacted at one end was determined. Reaction rate analysis indicates that that the grafting of epoxy–PS–epoxy to the nanotube surface is reaction controlled, as the FT‐IR spectroscopy signal grows as a function of approximately t0.3. These studies exemplify how FT‐IR spectroscopy can be used as a novel technique to quantify the amount of grafted polymer, grafting rate, and percent of difunctional polymers that form loops, and provide a method to create loop covered nanoparticles. magnified image