Impurities may affect structural alloy compatibility in both indirect- and direct-fired supercritical CO2 (sCO2) cycles for high efficiency power generation with peak temperatures above 700°C. Using a new multi-pump gas control system, experiments with controlled impurity additions were compared to baseline results in research- or industrial-grade CO2 at 750°C/300 bar. Low level impurities, 50 ppm O2 and 50 ppm H2O, were not found to affect mass change or reaction products after 2,500 h exposures. However, in RG sCO2+1%O2+0.25%H2O, higher reaction rates were observed for both Ni- and Fe-based alloys, but especially Fe-based alloys were strongly affected by these high impurity levels. Analytical TEM was used to characterize the reaction products on alloy 625.