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The polarographic reduction of the 3'-halogen derivatives of N,N-dimethyl-4-aminoazobenzene was studied in mixed water-methanol medium and optimum conditions were found for the determination of these genotoxic substances by tast polarography in the concentration range 1 . 10-4 to 2 . 10-6 mol l-1, differential pulse polarography at a dropping mercury electrode in the range 1 . 10-4 to 2 . 10-7 mol l-1 and fast scan differential pulse voltammetry at a hanging mercury drop electrode in the range 1 . 10-6 to 2 . 10-8 mol l-1. The increase in the sensitivity resulting from adsorptive accumulation of the studied substances on the surface of a hanging mercury drop can be utilized in the determination using the latter method in the concentration range 1 . 10-8 to 2 . 10-9 mol l-1.