The free ion concentrations of Na+, K+ and Cl- have been measured in the cells and intercellular spaces of developing amphibian embryos using ion-sensitive microelectrodes. Ca2+, H+ and buffering capacity have also been measured in the intercellular spaces. The free intracellular Na+ and K+ concentrations in the early cleavage stages remain approximately constant at 21 mM and 90 mM respectively. The free intracellular Cl- concentration, approximately 60 mM during the egg to 4-cell stage, falls during development to around 30 mM by the 128-cell stage. Embryos from different batches show a wide variation in intracellular free ion content. A strong correlation was observed between the ion content, particularly of K+, and the viability of the embryo. If the intracellular K+ concentration was less than 60 mM, embryos invariably died between late blastula and early gastrula stages; if greater than 80 mM the embryo generally survived. The intercellular free Na+, K+, Cl- and Ca2+ concentrations in Xenopus mid-blastula embryos are 91 mM, 4 mM, 59 mM and 1.5 mM respectively. The intercellular potential at late neurula stages is +3.5 mV when the embryo is bathed in 5% Ringer solution; changing to Ringer solution reduced the potential to -4 mV. Before gastrulation the intercellular Ca2+ concentration in Xenopus falls to approximately 0.5 mM, where it remains throughout gastrulation before returning to its mid-blastula value during neurulation. In Xenopus, the intercellular Na+ concentration falls to around 75 mM and the intercellular K+ concentration rises to around 17 mM at the end of gastrulation. These changes are not maintained and both Na+ and K+ concentrations return to their earlier values. In Ambystoma, the intercellular K+ concentration falls steadily from 7 mM at the mid-blastula stage to 2 mM at the end of neurulation. The Na+ concentration is constant at approximately 93 mM up to stage 14; between stages 14 and 16 the measurements show some scatter (minimum value 60 mM, maximum value 100 mM), and beyond stage 16 the Na+ concentration increases to 123 mM.