Optimum conditions were found for the determination of 4-nitrobiphenyl by fast scan differential pulse voltammetry at a hanging mercury drop electrode in the concentration range 1 . 10-5 to 2 . 10-7 mol l-1. A further increase in sensitivity was attained by adsorptive accumulation of this substance on the surface of the working electrode, permitting determination in the concentration range (2 – 10) . 10-8 mol l-1 with one minute accumulation of the substance in unstirred solution or (2 – 10) . 10-9 mol l-1 with three-minute accumulation in stirred solution. Linear scan voltammetry can be used to determine 4-nitrobiphenyl in the concentration range (2 – 10) . 10-9 mol l-1 with five-minute accumulation in stirred solution, with the advantage of a smoother baseline and smaller interference from substances that yield only tensametric peaks.