Abstract A new procedure for the synthesis of titanium silicate-1 (TS-1) with high Ti (Si + Ti) ratios is being reported. The rationale for the method adopted and the reasons for the incorporation of more Ti (than reported by earlier workers) are discussed based on liquid-phase n.m.r. studies of the precursors and reaction mixture. The influence of various synthesis parameters like temperature, SiO 2 TiO 2 , DH − SiO 2 , and H 2O SiO 2 , ratios, the silica source, and nature of organic additives on the synthesis of TS-1 is discussed. The TS-1 samples have been characterized by XRD, i.r. t.g./d.t.a., and SEM.