In this chapter we describe the synthesis of iodinated homopolymeric radiopaque nanoparticles of 28.9 ± 6.3 nm diameter prepared by emulsion polymerization of 2‐methacryloyloxyethyl(2,3,5‐triiodobenzoate) (MAOETIB). These nanoparticles dispersed in aqueous continuous phase tend to agglomerate in concentration above 0.3%. The agglomeration rate increases as the concentration of the nanoparticles in the aqueous phase rises, and prevents thereby the in vivo use as contrast agent for medical X‐ray imaging. This limitation was solved by synthesis of copolymeric iodinated nanoparticles of 25.5 ± 4.2 nm diameter, via emulsion copolymerization of MAOETIB in the presence of a low concentration of glycidyl methacrylate (GMA). The surface of the resulting copolymeric nanoparticles is far more hydrophilic than that of the polyMAOETIB (PMAOETIB) nanoparticles. Therefore, P(MAOETIB‐GMA) nanoparticles are significantly more stable against agglomeration in aqueous continuous phase. After intravenous injection of the P(MAOETIB‐GMA) nanoparticles dispersed in 5% dextrose aqueous solution into rats and mice (including those with a liver cancer model) CT‐imaging revealed a significant enhanced visibility of the blood pool for 30 min after injection. Later, lymph nodes, liver and spleen strongly enhanced due to nanoparticles uptake by the reticuloendothelial system. This favorably enabled the differentiation of cancerous from healthy liver tissue and suggests our particles for tumor imaging in liver and lymph nodes.