Fe3O4/γ-Fe2O3 nanoparticles (NPs) based thin films were used as active layers in solid state resistive chemical sensors. NPs were synthesized by high temperature solution phase reaction. Sensing NP monolayers (ML) were deposited by Langmuir-Blodgett (LB) techniques onto chemoresistive transduction platforms. The sensing ML were UV treated to remove NP insulating capping. Sensors surface was characterized by scanning electron microscopy (SEM). Systematic gas sensing tests in controlled atmosphere were carried out toward NO2, CO, and acetone at different concentrations and working temperatures of the sensing layers. The best sensing performance results were obtained for sensors with higher NPs coverage (10 ML), mainly for NO2 gas showing interesting selectivity toward nitrogen oxides. Electrical properties and conduction mechanisms are discussed.