The polarographic reduction of methylmercury in aqueous medium takes place in two steps, each of which involves the transfer of a single electron. The first reduction step proceeds reversibly both in direct current and in sinusoidal alternating current. Since the polarograms corresponding to this step are well defined, they can be successfully used to determine methylmercuric compounds by phase-sensitive sinusoidal a.c. polarography, in the concentration range 1 × 10−7−1 × 10−4mole.dm.−3