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This work aimed to compare the adsorptive removal of diclofenac from ultrapure and wastewater by different adsorbents. Batch kinetic and equilibrium experiments were carried out using two different activated carbons (GPP20 and WP70, from Chemviron Carbon) and a non-ionic polymeric resin (SP207, from Resindion). The pseudo-second-order equation fitted the kinetic experimental results and the corresponding k2 (g mg−1 min−1) determined for the activated carbons was one order of magnitude higher than for the polymeric resin. The equilibrium results were fitted by the Langmuir–Freundlich isotherm. The determined maximum adsorption capacity (Qm, mg g−1) and the adsorbent–adsorbate affinity parameter (KLF, mg g−1 (mg L−1)−1/n) were one order of magnitude higher for the activated carbons than for the polymeric resin. With respect to the influence of the aqueous matrix, both the k2 and the Qm remained the same in ultrapure as in wastewater. Differently, the KLF showed one order of magnitude higher values i...