The ultrahistochemical analysis of apical granules in the epithelial cells, i.e., granular cells, of the amphibian urinary bladder using the N,N-naphthaloylhydroxylamine procedure identified the presence of calcium in these structures. Subsequent analytical microscopy employing fresh-frozen ultrathin cryosections for X-ray microanalysis of the granules further confirmed the above histochemical findings. In addition to calcium, elemental analysis indicated the presence of magnesium, phosphorus, sulfur, silicon, potassium, and chlorine either within or in close proximity to the granules. The possibility that these granules function as subcellular compartments for the uptake and storage of calcium ions, in a way similar to mitochondria, and thus function in intracellular calcium homeostasis, is discussed. Additionally, a role for this cation in the secretion of granular glycoproteins, i.e., stimulus-secretion coupling, is hypothesized.