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Matrix isolation spectroscopy is a powerful tool for investigation of the structure and dynamics of fundamentally important small radicals with numerous implications for different areas of the free radicals research. In particular, the HOCO radical, a key intermediate in atmospheric chemistry and combustion, was first observed in low temperature matrices, which stimulated extensive experimental and theoretical investigations of this species, both in gas phase and in solids. It is worth noting that the radiation-induced formation and intrinsic reactivity of HOCO at low temperatures is of specific interest in view its possible role in pre-biotic astrochemistry. Meanwhile, the mechanism of formation and reactions of this radical in matrices is still poorly understood and direct experimental evidences are quite limited. Here we report a systematic study on the formation of HOCO radical in the radiation-driven processes, occurring in H2O/CO2/Ng and HCOOH/Ng systems (Ng = Ne, Ar, Kr, or Xe, in typical excess of 1000).