We have investigated the structural and electrical properties of GaInP/GaAs epilayers that we have implanted with Fe atoms (190 keV) to produce a shallow high resistivity layer. SIMS, PIXE-channeling and EXAFS were used to provide a structural characterization. Current–voltage analyses as a function of temperature indicate the activation of an efficient and stable electrical compensation process, that we have ascribed to the interplay between a deep donor and a deep acceptor, located at EC−0.50 eV and EV+0.74 eV, respectively. We have focused our attention on the latter deep level, attributed to the Fe2+/3+ related acceptor trap, that we have directly identified and characterized by spectral photocurrent analyses and by capacitance transient spectroscopy carried out under below band gap illumination that stimulated the direct emission/trapping of carriers from the deep trap.