Currently, there has been a growing interest of zeolite materials for industrial and scientific purpose. Synthetic zeolites are more often used than natural ones due to its higher purity and more uniform particle sizes. Numerous investigations are conducted in searching of inexpensive raw materials suitable for zeolite synthesis. Moreover, the temperature, pressure, times and SiO 2 /Al 2 O 3 ratio are the most important parameters which play key roles in the synthesis processes. Due to such a large number of factors that affect the process, zeolite synthesis has been undergoing constant development. Nowadays, researchers focus on the methods of synthesizing zeolites at ambient temperature and pressure. Metakaolin and tuff are natural raw materials which can be turned into a brand new class of synthetic zeolites. However, each requires different method of synthesis in order to obtain a material with best physical properties. This paper discusses the process of alkaline activation of synthetic zeolites from natural raw materials: volcanic tuff excavated in Filipowice and metakaolin obtained from Rominco company. Two methods: fusion and low-temperature synthesis, were used in the presented research. Moreover, the physical properties of raw materials and zeolites obtained were shown. Based on the XRD analysis, it was verified that materials after the synthesis process contained zeolites A, Na-X and faujasite-Na. Furthermore, the dehydration and thermal decomposition phenomena of the tuff and metakaolin before and after the synthesis process were determined by coupled TG/MS techniques.