For orange peel (OP), lemon peel (LP), and banana peel (BP) as adsorbents for removal of heavy metal ions such as Cu2+, Ni2+, Cd2+, Pb2+, and Zn2+ from aqueous solution, a simple FT-IR technique was used and discussed to study the variation in functional groups upon modification. Metal carbon bond formation was witnessed by FT-IR during metal ion adsorption. All of these adsorbents were characterized by FT-IR, BET, and SEM. The presence of carboxylic and hydroxyl groups was confirmed by FT-IR. The FT-IR spectrum of lemon peel cellulose (LPC) showed well resolved peaks for carboxylic acid and hydroxyl groups compared to LP indicating the appreciable contents of carboxylic acid and hydroxyl groups in LPC. The widely used Langmuir adsorption isotherms were used to describe the adsorption equilibrium process. The adsorption capacity of the metal ions such as Cu2+ and Ni2+ was found to be more than those of other metal ions. Upon comparison of the adsorbents, surface modified LPC (LPCACS) was found to show enhanced adsorption activity. A comparative study of adsorption was carried out with commercially available activated carbon (AC) also from which it was inferred that the order of the adsorption capacity is as follows: LPCACS > LPC > AC > LP > OP > BP.