Polyacrylamide (PAA) cryogels were prepared by freezing monomer solution of acrylamide with cross-linker N,N-methylenebis(acrylamide) and polymerizing initiated by N,N,Nʹ,Nʹ-tetramethyl ethylene diamine and ammonium peroxodisulfate at sub-zero temperatures. Iron hydroxide oxide particles were formed by stepwise penetration of iron(III) chloride solution (FeCl₃) and alkaline aqueous solution into cryogel wall. The particles formed were observed on the surface of the cryogel wall. The amount of the particles was changed by the concentration of FeCl₃ and the kind of alkaline aqueous solution. The polyacrylamide cryogel containing iron hydroxide oxide particles successfully adsorbed a large amount of As(V) at both low and high concentrations. The adsorption of As(V) with the cryogel containing iron particles was not affected by the pH value of the aqueous solution. The cryogels containing iron particles prepared using sodium carbonate had larger amount of iron than that prepared using sodium hydroxide. The adsorption amount of As(V) on the cryogel had a tendency with the contents of iron in the cryogels.