The preparation of CaSO4 nanoparticle by vesicles formed spontaneously in cationic OTAC and anionic ADS mixed surfactant solution whose ratio is 0.3/0.7 is investigated. Added electrolytes for preparing nanoparticles reduce vesicle size about 200-300 nm comparing with that of pure vesicle whose size is 700-800 nm by DLS. The core of vesicles has 200 nm size and acts as nanoreactors which same size of monodisperse CaSO4 nanopaticles are formed. Although CaSO4 particles are formed at the outer of vesicles, they are very large and amorphous. The formed particles are identified with XRD analysis after separation due to coinciding with CaSO4 particles.