The total mass attenuation coefficients (μ m ), for Cr, Fe, Ni and Fe x Ni 1− x (x=0.8, 0.7, 0.6, 0.5, 0.4, 0.3 and 0.2), Fe x Cr y Ni 1−( x + y ) (x=0.7, y=0.1; x=0.5, y=0.2; x=0.4, y=0.3; x=0.3, y=0.3; x=0.2, y=0.2 and x=0.1, y=0.2) and Ni x Cr 1− x (x=0.8, 0.6, 0.5, 0.4 and 0.2) alloys were measured at 22.1, 25.0, 59.5 and 88.0 keV photon energies. The samples were irradiated with 10mCi Cd-109 and 100mCi Am-241 radioactive point source using transmission arrangement. The γ- and X-rays were counted by a Si(Li) detector with a resolution of 160eV at 5.9keV. Total atomic and electronic cross-sections (σ t and σ e ), effective atomic and electron numbers (Z eff and N eff ) were determined experimentally and theoretically using the obtained mass attenuation coefficients for investigated 3d alloys. The theoretical mass attenuation coefficients of each alloy were estimated using mixture rule. The experimental values were compared with the calculated values for all samples.