The purposes of this investigation were to study the characteristic properties of bismuthoxynitrate formed by hydrolysis of bismuthnitrate according to various reaction conditions and to propose the property difference between synthesized pearl pigment and bismuthsubnitrate as pharmaceuticals by means of X-ray diffraction, IR, DTA and TGA. The pearl pigment could be obtained by reaction of bismuth nitrate-diluted nitric acid solution with cold water (5.deg.) agitation at lower pH. The pearl pigment was BiO. NO$_{3}$. 2H$_{2}$O. in composition and crystalline form was thin plate of monoclinic system and its combination with water was assumed to be hydrated hydrous form between Bi-H$_{2}$O bond. On the other hand, bismuthsubnitrate was 5BiO.4NO$_{3}$.6H$_{2}$O in composition and crystalline form was pillar of rhombic system and the bond between Bi and H$_{2}$O molecules was assumed to be hydrous form. The different properties between two compounds in structure are presumed to be caused by the hydrolysing conditions of bismuthnitrate respectively.