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The mass attenuation coefficients (μ/ρ) of a natural material, i.e., olive peat, were measured at photon energies of 0.059, 0.356, 0.662, 1.17, and 1.332 MeV and compared with those of concrete and Pb. The experimental samples were irradiated with 214Am, 133Ba, 137Cs, and 60Co point sources using a transmission arrangement. The olive peat samples were obtained from different areas in Jordan, namely Mafraq (sample M), Kerak (sample K), Ajloun (sample A), and Irbid (sample I), and photon energies were measured using a NaI(Tl) scintillation detector with an energy resolution of 7.6% at 662 keV. The differences in the μ/ρ of olive peat samples and the calculated μ/ρ of concrete were consistently within 0.7% at photon energies of 0.356–1.332 MeV. This finding indicates that olive peat can be used in radiation applications in the field of medical physics. Finally, the half-value layer (HVL) of the exper-imental samples was measured, and results were compared with those of concrete and Pb. Pb and concrete exhibited minimal HVL values due to their high density, and the HVL of olive peat revealed lower shielding effectiveness than that of concrete.