Irradiation at elevated temperatures of V(Cr) alloys is known to create a near-surface layer of nonequilibrium Cr enrichment. Highly reproducible RBS spectra were accumulated from a V-15%Cr alloy irradiated at 750°C, and from unirradiated portions of the same specimen. Differences between these spectra are used to demonstrate the high sensitivity of conventional RBS techniques for determining near-surface segregation behavior. Sensitivities obtained utilizing differences in the acquired spectra are much higher than those typically assumed for RBS measurements. Using 1.8 MeV 4He, and conventional RBS equipment and scattering geometries, segregation of < two atomic layers of 52Cr in 51V- 15at.%Cr over a depth of ∼5 nm has been observed.