Various factors affecting the demulsification rate of emulsion were examined by means of an electrostatic coalescence method using emulsion which consisted of an organic phase containing tri-n-octhylamine (TNOA) and Span 80 or ECA 4360J and an internal aqueous phase containing Na₂CO₃. Increases in applied voltage, Na₂CO₃ concentration, and W_I/O ratio result in an increase in demulsification rate, while increases in surfactant (including Span 80 and ECA 4360J) concentration, agitation speed of homogenizer and homogenizing time cause a decrease in demulsification rate. Changes in TNOA concentration do not have a significant effect. The regeneration of emulsion was examined using organic solution recovered from a Mo(VI) extraction circuit. It was found that the regeneration of emulsion containing Span 80, is generally difficult, while that containing ECA 4360J is relatively easy.