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The temperature- and pH-sensitive poly(N-isopropylacrylamide-co-acrylic acid) hydrogels, poly(NIPAM-co-AA), were synthesized by radical polymerization. The characterizations of hydrogels based on N-isopropylacrylamide (NIPAM) and acrylic acid (AA) before and after adsorption of heavy metal ions was performed by Fourier transform infrared spectroscopy and scanning electron microscopy. Heavy metal ions (Cr, Mn, Pb) adsorbed onto poly(NIPAM-co-AA) hydrogels were identified using the energy-dispersive X-ray spectroscopy. The mechanism of the water transport within the matrix of synthesized poly(NIPAM-co-AA) hydrogels at pH 4.5 is Super Case II diffusion, and at pH 6.8 corresponds to the non-Fickian diffusion mechanism. The effect of pH, temperature, contact time, and the initial concentration of heavy metals on the adsorption process of Cr(VI), Mn(II), and Pb(II) ions from aqueous solutions …