This study investigated the adsorption of calcium and gypsum on scheelite and fluorite using micro-flotation, X-ray photoelectron spectroscopy, scanning electron microscope with energy-dispersive spectrometer, and zeta potential measurements. Micro-flotation showed scheelite recovery is more sensitive to calcium, and gypsum shows stronger inhibition than calcium. Stick-shape precipitates as sulfate-bearing are only found on fluorite surface in gypsum solution. Change law of the zeta potentials of scheelite and fluorite in gypsum solution is obviously different from that in calcium solution. Therefore, we concluded that gypsum would make the separation of scheelite from fluorite more difficult than calcium.