For the efficient preconcentration of azo compounds – products of the interaction of 4-nitrophenyldiazonium with thymol, a system 4-nitroaniline (4-NA) – NO2 - – Triton X-100 – NaOH – ethanol has been proposed. The optimal conditions for the formation of micellarsaturated phases of the system under study have been established: 3. 10-4 M 4-NA – 3. 10-4 M NO2 - – 5% Triton X-100 – 2.8 M NaOH – 10 vol. % С2Н5ОН. A spectrophotometric study of the above system has been carried out.