Microsphere polymeric materials containing beta-cyclodextrin (beta-CD) and poly(acrylic acid) (PAA) with tunable morphologies were prepared in order to improve their sorption characteristics in aqueous solution. The microsphere polymeric materials were prepared using a (water/oil) micro-emulsion-evaporation technique to condense beta-cyclodextrin (beta-CD) with PAA at various comonomer ratios and mixing speeds. The beta-CD microsphere copolymers were characterized using FTIR, TGA, DSC, SEM, elemental (C and H) microanalyses, and solid state 13C-NMR spectroscopy. The sorption properties of the polymeric materials at 295 K in aqueous solution containing p-nitrophenol (PNP) were studied using a dye-based method with UVVis spectrophotometry at pH 4.6 and 10.3. The sorption isotherms of copolymer/PNP systems were evaluated with various isotherm models (e.g., Langmuir, BET, Freundlich, and Sips). The Sips isotherm showed the best overall agreement with the experimental results and the sorption parameters provided estimates of the sorbent surface area (12.0331 m2/g) and the sorption capacity (Qm = 0.3592.20 mmol/g at pH = 4.6; Qm = 0.0700.191 mmol/g at pH = 10.3) for the microsphere copolymer/PNP systems in aqueous solution. The nitrogen adsorption properties of the microporous copolymers in the solid state were obtained at 77K with BET surface areas ranging from 0.275 to 4.47 m2/g. (c) 2012 Wiley Periodicals, Inc. J Appl Polym Sci, 2012