The invention discloses a method for analyzing of occurrence forms of Hg and Pb in desulphurization gypsum in a coal-fired power plant. A solid mercury analyzer is used for analyzing the total mercurycontent, namely, input SHg of mercury, in a desulphurization gypsum sample, a liquid analyzer is used for analyzing content of acid extraction form, reduction form, oxidation form and residual form mercury content of mercury and lead in an extraction liquid, SHg1+SHg2+SHg3+SHg4 are output of mercury, a reference system with analytical data of Hg as reference is established, meanwhile, and a groupof prepared Hg and Pb standard solutions with the content of 10 ppb can be added in the extraction process of each step to serve as check standard of each step. The recovery ratio of lead in the method can reach 95% or above, and the occurrence forms of mercury and lead in the desulphurization gypsum in the coal-fired power plant can be obtained more accurately.