This paper studied the problems met in the quantitative analysis of synthetic Mullite phase,which was based on the analysis of various typical Mullite composite scheme. A method of quantitative analysis of Mullite phase (excluding amorphous phase SiO2) by use X-ray diffraction was discussed. The error of the analysis can be verified by chemical analysis of Al2O3 content. The method can effectively improve the accuracy of quantitative analysis of the Mullite phase, the error analysis is less than 3%. The error range can meet the accuracy requirement of Mullite content in the production.Studies show that this method is preliminarily solved how to quantitative the content of mullite phase by X-ray diffraction method .