The electro-oxidation of water-immiscible liquid aliphatic acids (RCO₂H) leading to decarboxylation to afford a hydrocarbon (R–R) may be achieved using an emulsion formed via insonation so that the organic phase continuously extracts the products; in complete contrast to conventional monophasic electrolyses, the type and yield of products obtained from this biphasic Kolbe electrolysis are independent of the electrode material used.