A series of cysteine-stabilized phenolic resin-based polymer and carbon spheres were prepared by the modified Stober method. Cysteine plays a very important role in the proposed one-pot synthesis of the aforementioned spheres; namely, it acts as a particle stabilizer and a source of heteroatoms (nitrogen and sulfur) that can be introduced into these spheres. The diameter of these spheres can be tuned in the range of 70-610 nm by adjusting the cysteine amount and reaction temperature. Since polymer spheres obtained in the presence of cysteine contain sulfur and nitrogen heteroatoms, they were tested for adsorption of copper ions. It is shown that adsorption isotherms recorded for copper ions can be well fitted by Langmuir equation, giving unprecedented adsorption capacities up to similar to 65 mg/g.