Water-soluble arabinoxylans from wheat flour were purified and fractionated by graded ethanol precipitation. Six fractions were obtained at 20% (F20), 30% (F30), 40% (F40), 50% (F50), 60% (F60), and 70% (F70) saturation with ethanol. Neutral sugars and (1)H NMR analyses revealed differences in structural characteristics. The Ara/Xyl ratio and the amount of Xylp residues disubstituted increased with ethanol concentration. Ferulic acid content was higher in fractions precipitated at low ethanol percentage. Fractions were refractionated by SEC, leading to 46 subfractions with low polydispersity index. Substitution degree was apparently linearly related to the amount of disubstituted Xylp. Macromolecular characteristics (M(w), [eta], R(G), q, nu) determined by multiangle laser light scattering and viscosimetry were similar among all fractions. A rather flexible conformation was determined for the arabinoxylans, in conflict with the admitted rodlike conformation. The substitution degree had no influence on the conformation or on the rigidity of the polymers. Evidence for the presence of ferulic acid dimers in the water-soluble arabinoxylans is provided, which probably explains the unexpected conformation and macromolecular characteristics.