An experimental study has been conducted to investigate the heat/mass transfer characteristics within a film cooling hole of square cross-section for various blowing ratios and Reynolds numbers. The experiments have been performed using a naphthalene sublimation method and the flow field has been analyzed by numerical calculation using a commercial code. A duct flow enters into a film cooling hole in a cross-direction. For the film cooling hole with square cross-section, it is observed that the reattachment of separated flow and the vortices within the hole enhance considerably the heat/mass transfer around the hole entrance region. The heat/mass transfer on the leading edge side of hole exit region increases as the blowing ratios decrease because the main flow induces a secondary vortex. Heat/mass transfer patterns within the square film cooling hole are changed little with the various Reynolds numbers.