The phosphorylation of cross-linked polystyrene resins has been previously described. As seen by their interaction with lupus antibodies, these polymers were found to mimic either DNA or phospholipid antigens, depending on the degree of substitution by phosphate groups. When an alkyl spacer was included between phosphate groups and macromolecular chains, difficulties in synthesis and desorption of the biological species from the resins were seen. In this article, kinetic aspects of the synthesis of phosphorylated polymers, possessing sulfamide spacers, are discussed. The characterization of these phosphorylated polymers by acidimetric titration is extensively described. This technique differentiates and quantifies the grafted phosphate groups, which can be either phosphomonoester or phosphodiester in nature. We demonstrate that these polymers form complexes with calcium ions, and that the affinity of the ions is closely associated with the type of phosphate groups.