The incorporation of triple crystal x-ray diffraction (TCD) under conditions of a nearly grazing incident x-ray beam provides a unique capability to characterize surface and subsurface structural damage. The effects of bromine-methanol chemical-mechanical (CM) polishing on the surface quality of GaAs were investigated by inclined Bragg plane triple crystal x-ray diffraction. GaAs samples polished under varying conditions of Br2 concentration, total polish time, polish wheel rotation speed, and force exerted on the samples were analyzed using TCD profiles from inclined (220) planes, with the samples oriented at both the exact Bragg condition, θB, and at deviations from the exact Bragg condition. As the deviation from the 220 reciprocal lattice point was increased, multiple peaks corresponding to both the dynamic and the kinematic components were observed. The peak positions and the relative intensities of the various peaks were used to characterize the effects of the CM polishing variables on the GaAs surfaces.