Two novel fibrous framework titanium phosphates having a similar formula, Ti2O(PO4)(2) . H2O, and a layered titanium phosphate, Ti2O3(H2PO4)(2) . 2(H)2, were synthesized and their properties were characterized with physicochemical methods, such as elemental analysis, thermogravimetry, nitrogen adsorption, X-ray diffraction, and P-31 solid-state NMR. Nitrogen adsorption isotherms were measured on synthesized titanium phosphates in order to characterize their surface and structural properties. The specific surface area and total pore volume of the titanium phosphates studied were determined, The low-pressure nitrogen adsorption isotherms were used to evaluate surface heterogeneity of the synthesized materials by employing an advanced numerical procedure based on the regularization method.