Abstract: In order to improve the teaching level of X-ray diffraction (XRD) analysis application, a XRD comprehensive analysis experiment is designed. Taking the XRD pattern of cubic crystals Cu and Cr as an example, the Bravais lattice, index of crystal face and lattice parameters are derived mathematically. Taking the XRD pattern of TiO₂ as an example, its phase compositions are analyzed by Jade software. The quantitative analysis of phase is obtained by K-value method, peak fitting and Rietveld whole pattern fitting. The results show that Rietveld whole pattern fitting has the advantages of being independent of RIR value compared with peak fitting; the quantitative analysis results of phase composition with the same crystal model and different RIR value are consistent; it is convenient to obtain accurate crystal cell parameter values. Mathematical derivation of crystal structure and quantitative calculation of phase, qualitative analysis of phase by software and comparative use of different software and different methods in quantitative analysis of phase can effectively improve students’ XRD theory and practice level.