A new method is developed for the extractive separation of mercury from associated elements. Mercury is quantitatively extracted from 0.5 M acetic acid solution by aliquat 336 S, which acts as a liquid anion exchanger. The metal ion from the organic phase is stripped with sodium hydroxide solution and determined in the aqueous phase complexometrically. The extracted species is [2(R4N+), Hg(OAc)4−2]. A working procedure for the selective separation of mercury from zinc, cadmium, nickel, cobalt, copper, bismuth and manganese is described.