In this work the laboratory installation for synthesis of powder materials with nanosize grains is presented. Nano-sized zinc and tin were obtained using the spray-pyrolysis (SP method). The zinc oxide was derived from zinc acetate at 300, 430, 580, 800 i 950oC. The tin oxide had been produced by the thermal decomposition of tin tartrate at 500oC. The SP synthesized zinc oxide was used for processing of methane sensor. The methane sensor made of SP derived zinc oxide was characterized with much wider range of operating and substantially (10 times) higher sensitivity when compared to that made of commercially available zinc oxide.