The effect of giant injection magnetoresistance (GIMR) was recently observed in a granular SiO2/(54–75 at. % Co) film on a semiconductor GaAs substrate in a temperature range near T = 300 K. The magnetoresistance coefficient reaches a value of 105% in a magnetic field of 1.9 T and at a voltage of 90 V. A structural model of the film was proposed based on the results of the grazing-incidence small-angle scattering (GISAXS) and x-ray reflectivity, which showed a specific interface layer 70–75 A thick separating bulk SiO˚ 2(Co) granular film from the semiconductor substrate. This layer is formed by a monolayer of flattened Co particles which are laterally spaced apart much further than the particles in the bulk film. In the present work, using polarized neutron reflectometry (PNR), we study both the structural and magnetic properties of SiO2(Co) film separately in the bulk and in the interface layer, which is possible due to the depth resolution of the method. Temperature-dependent PNR and magnetization measurements performed by Superconducting Quantum Interference Device (SQUID) revealed the occurrence of two types of magnetic nanoparticles with different blocking temperatures and magnetization. The magnetization hysteresis curve demonstrated specific two-loop structure in fields 0.5–2 T. Thus our selfconsistent results of PNR, GISAXS, and SQUID measurements emphasize the role of the interface features in the SiO2(Co)/GaAs heterostructures and show a direction for further development of the GIMR theory