Agarose gel entrapping CaCO3 granules is used for the synthesis of bimodal porous CaTiO3 beads by a method that combines a sol-gel process and solid phase reaction, in which CaCO3 (1 05 mu m) performed as both calcium resource and porogen for creating macropores The amount of CaCO3 granules embedded in agarose gel is vaned from 0 to 16 wt %, and the macropores on the surface and in the inner of final CaTiO3 beads are investigated It is found that the addition of 12 wt % of CaCO3 produced CaTiO3 beads that present interconnected macropores of about 745 +/- 20 nm The calcination temperature affects the surface area, mesopore size, phase state, and crystalline Sin of the CaTiO3 beads By calcination at 450 degrees C, the CaTiO3 beads prepared by the addition of 12 wt % CaCO3 are amorphous with an average pore size of 9 nm and possess a high surface area of about 225 m(2) g(-1) With an increase of temperature to 600, 750, and 900 degrees C, the CaTiO3 is transformed Into perovskite in size of about 32, 34, and 37 nm with mesopores of about 20, 23, and 24 nm, respectively, and its specific surface area decreases below 20 m(2) g(-1) The bimodal porous CaTiO3 beads of about 15 mu m are packed into a column for investigating its chromatographic performance The column shows much higher column efficiency than that packed with CaTiO3 beads without removal of the porogen The remarkably high separation performance is attributed to the unique surface property and interconnected macropores present in the CaTiO3 beads