The preparation of 17 kinds of ceramic standard samples(CSS) is introduced briefly in the present paper, and the experimental results of the sintered CSS by using EPMA and XRF are discussed in detail. The conclusions can be mainly drawn that the CSS, which have high density, low water absorption and good homogeneity of element distribution, have similar phase structure (or matrix) to the bodies of ancient ceramics, and perfectly meet the requirements of being used as ceramic standard samples. This set of CSS are expected to play an important role in x-ray fluorescence spectrometric quantitative analysis of Na2O, MgO, Al2O3, SiO2, K2O, CaO, TiO2 and Fe2O3 in the body of ancient ceramics and can provide accurate and reliable data for study and identification of ancient ceramics.