The invention relates to a method for measuring the content of calcium sulfate in desulfurized gypsum of a coal-fired power plant, which comprises the following steps: (1) drying the desulfurized gypsum in the sun, grinding, sieving and drying, adding hydrogen peroxide, demineralized water and cation exchange resin, stirring to adjust the pH value, stirring, filtering with filter paper, and fixing the volume to obtain a desulfurized gypsum oxidation solution; (2) transferring the desulfurized gypsum oxidation solution, adding absolute ethyl alcohol and an alizarin red S indicator, uniformly mixing, titrating with a barium chloride standard solution, slowly generating turbid substances in a yellow solution, shaking while titrating, determining the titration end point when reddish color appears, and recording the volume of the consumed standard solution; and (3) substituting the volume of the consumed standard solution into a calculation formula, and calculating to obtain the content of calcium sulfate. The method has the advantages of simple operation steps, good repeatability of detection results, high accuracy, high efficiency, rapidness, low pollution, low drug consumption and low cost, meets the requirements of thermal power plant detection laboratories, and has a wide application range.