A new electrochemical technique is presented for the investigation of aggregation phenomena in solution over a wide range of solution conditions. Developed nominally for dyes, the method is, in principle, applicable to any electroactive compound. The method employs microelectrodes to measure the change in the diffusion limited current, with concentration, of the aggregating species of interest. At the onset of aggregation, the relationship between this limiting current and concentration deviates from linearity. This deviation, due to the slower rate of diffusion of aggregates, is related to the degree of association of the molecule, assuming a molecular weight distribution of aggregates and using an established relationship between the effective diffusion coefficient and molecular weight. The technique is contrasted with an existing spectroscopic method.