In the present work, CuO/CuFe2O4 nanoparticles were synthesized via a polyacrylamide gel. The produced nanocomposites were utilized as a gas sensor for the detection of H2S gas. The nanoparticles were characterized via XRD, FTIR, SEM and TEM techniques. XRD results revealed that the as-prepared product was amorphous and CuO and CuFe2O4 phases were formed after calcination at 800°C. Microstructural studies showed that the nanoparticles have a particle size distribution ranging from 60 to 120 nm. Most of the particles had a spherical morphology. The polyacrylamide network acted as a template for the formation of the nanoparticles. The H2S gas sensing characteristics of the products were studied at different concentrations and operating temperatures. In addition, the effect of humidity on the gas-sensing response was investigated. The prepared CuO/CuFe2O4 sensors can respond up to 25 when exposed to 10 ppm H2S which is higher than the pure CuO or CuFe2O4 sensors. The sensors reached a detection limit of 0.1 ppm and demonstrated clear sensitivity and quick response and recovery behavior toward H2S gas. The CuO/CuFe2O4 heterogeneous nanostructures also showed proper H2S gas response and selectivity in response to interfering gases like NH3, NO2, HCHO and CO. The gas sensing mechanism of the composites was also discussed.