Calcium was localized by in situ precipitation with potassium antimonate during epididymal maturation of the mouse and guinea pig sperms. In caput epididymis the calcium in mouse sperm head was mainly localized on the inner surface of tha outer acrosomal membrane (OAM) in preacrosomal region. During the passage from the caput epididymis to the cauda epididymis the calcium amount of mouse sperm did not undergo apparent changes. In comparison with mouse sperm, there were a few fine calcium deposite granules on the inner surface of the guinea pig sperm OAM on the abdomen side at the caput epididymis stage, but these granules disappeared at the cauda epididymis stage. The microvilli of columnar cell in columnar epithlium lining the epididymal duct are probably involved in regultion of Ca2+ concentration of the intraluminal fluid. The calcium precipitation granules distributing in the microvilli were observed. An abundance of Ca2+ were present in the intraluminal fluid of the corpus epididymis and they might have some important functions during the process of sperm maturation. Calcium in sperm tail was mainly distributed in the mitochondria. Compared with the mouse sperm, the mitochondria of guinea pig sperm possessed more calcium.