Formation of tungstic acid was investigated in the presence of an alkylammonium chloride surfactant, C16H33N(CH3)(3)Cl Or C12H25N(CH3)(3)Cl, by titrating Li6W2O9 . 4/7H(2)O aqueous solution with HCl. Alkylammonium intercalated layered tungstic acids with expanded interlayer spacings of 2.58 nm or 2.20 nm were precipitated in a low surfactant concentration of 3.2 wt. % depending on the kind of surfactant, respectively. They thermally decomposed to WO3 at 600 degrees C through layered compounds with contracted interlayer spacings. MCM-41 like mesostructured product with hexagonal a = 4.48 nm was obtained in a high surfactant concentration of 33 wt. %. The mesostructure was difficult to preserve in its thermal treatment converting to WO3 even below 270 degrees C.