This present work aimed to synthesis Ni doped WO3 nano particles with different doping concentration by hydrothermal method and examined as effective gas sensing materials for detecting VOC’s. The physio chemical properties and the effect of ammonia sensing characteristics of prepared nano particles were investigated and confirmed by XRD, SEM, TEM, UV– Vis and FTIR. The results proposed that 0.75wt%Ni doped WO3 (NW3) exhibited excellent response towards ammonia gas at the calcining temperature of 550 °C with good response time of 36 sec also with rapid response – recovery time of 36–100 s even at room temperature.