A new diffusion-multiple technique was used for mapping the phase diagram in the pseudoquaternary Fe 3 Al-Cr-Mo-C system at 800°C. The following five carbide phases were formed in an Fe 3 Al matrix phase (B2) with composition gradients of Cr, Mo, and C in the diffusionmultiple samples: j-Fe 3 AlC, M 5 C, M 6 C, Cr 7 C 3 , and M 2 C (M: Mo, Cr, Al, and Fe). It was assumed that B2 phase is in equilibrium with j, M 5 C, M 6 C, and Cr 7 C 3 but not with M 2 C phase at 800°C. Complex phase equilibria among those phases were efficiently mapped by the diffusion-multiple technique. The results from the technique were consistent with those obtained from the conventional bulk alloy method.