The ATRP (atom-transfer radical polymerization) process was used to synthesize C-60 end-capped polystyrene. GPC data demonstrated that fullerene (C-60) was chemically bonded to polystyrene, and C-60 was most likely monosubstituted. Matrix-assisted laser desorption/ionization-time of flight (MALDI-TOF) mass spectrometry (MS) analysis (with 1,8-dihydroxy-9(10H)-anthracenone (dithranol)/silver trifluoroacetate as the matrix) of this copolymer proved that C-60 was monosubstituted.