The development of new adsorbents to separate biocompounds and polyacrylamide monolithic cryogels shows great potential for purifying macromolecules from non‐clarified media. In this work, alternatives for functionalization and characterization of polyacrylamide monoliths grafted with 2‐acrylamide‐2‐methyl‐1‐propanosulfonic acid were explored. Dynamic grafting did not affect swelling capacity, or graft density. Pore size was evaluated by optical microscopy, which presented the same values obtained by scanning electronic microscopy. The method of moments was used to determine porosity, apparent axial dispersion coefficient, and the height of the theoretical plates of the columns, presenting results consistent with those in the literature. The permeability constant was determined by varying the viscosity of a Newtonian fluid at constant pressure, with the value being the same as that obtained by varying the hydrostatic pressure over the column. Results demonstrated these techniques were adequate for characterizing polyacrylamide cryogels, opening new perspectives in this field. POLYM. ENG. SCI., 58:1717–1725, 2018. © 2017 Society of Plastics Engineers