Hydroxy sodalite (HS) is reported as high-temperature water separating zeolite membrane because of its small β-cage structure (pore size=2.8Å). HS zeolite particles were synthesized using various experimental set-ups including water bath, oil bath, refluxing and hydrothermal method using a gel composition of 5SiO2:1Al2O3:50Na2O:1000H2O. The morphology, crystallinity and purity of HS particles by changing silica source, temperature and synthesis time were studied. The products were characterized by X-ray diffraction (XRD), and scanning electron microscopy (SEM). Particle sizes were increased with increase of temperature (90 °C - 180 °C) and time (2 – 24 h). Pure HS particles were obtained by using conventional hydrothermal synthesis at 120°C for 2h.