Herein, we report a general voltammetric method to characterize the electrochemical nucleation rate and nuclei of single nanobubbles. Bubble nucleation is indicated by a sharp peak in the current in the voltammetry of gas-evolving reactions. In contrast to expectations based on the stochastic nature of nucleation events, the peak current signifying a stable nucleus is extremely reproducible over hundreds of cycles (∼3% deviation). By applying classical nucleation theory, this seemingly deterministic behavior can be not only understood but also used to quantify the nucleation rate and size of bubble nuclei. A statistical model is developed whereby properties of single critical nuclei (contact angle, the radius of curvature, activation energy, and Arrhenius pre-exponential factor) can be readily measured from the narrow distribution of peak currents (mean, standard deviation) from hundreds of voltammetric cycles at a nanoelectrode. Single nanobubbles formed from gas-evolving reactions (H 2 from H + reduction, N 2 from N 2 H 4 oxidation, O 2 from H 2 O 2 oxidation) are analyzed to find that their critical nuclei have contact angles of ∼150, ∼160, and ∼154°for H 2 , N 2 , and O 2 , respectively, corresponding to ∼50, ∼40, and ∼90 gas molecules in each nucleus. The energy barriers for heterogeneous nucleation of H 2 , N 2 , and O 2 bubbles are, respectively, 2, 0.4, and 0.7% of those required for homogeneous nucleation under the same supersaturation.