Abstract.A complexo-titrimetric method for the determination of mercury (II) in the presence of other metal ions is described, based on the selective masking ability of sulphite ion towards Hg(II). Mercury in a given sample solution is initially complexed with a known excess of EDTA and the surplus EDTA titrated with zinc sulphate solution at pH 5.0-6.0 (hexamine), using xylenol orange (or methylthymol blue) as indicator. An excess of solid sodium sulphite is then added to decompose the Hg(II)-EDTA complex and the released EDTA is titrated with standard zinc sulphate solution. Reproducible and accurate results are obtained for 9.9-99 mg Hg with relative errors < 0.35% and standard deviations < 0.05 mg. The effects of various cations and anions are studied.Key words: mercury determination, EDTA titration, complexometry, masking, sodium sulphite.Mercury(II) is not normally determined by direct EDTA titration, particularly in the presence of other ions. Instead, Hg(II) and other metals are complexed with EDTA, followed by selective decomposition of the Hg-EDTA complex with a masking agent such as thiosemicarbazide and titration of the liberated EDTA [1]. Cu(II) interferes severely in the above method. In alkaline medium, potassium iodide may be used as a masking agent for the estinaation of Hg(II) in the presence of Cu(II), but several other cations interfere [2]. With thiourea [3] as masking agent, interference by copper was avoided by controlling the pH at 5.5 and cooling below 15~ good results are obtainable provided that thiourea is in only slight excess over the stoichiometric proportions. Obviously, this is difficult to ensure in the case of unknown concentrations of mercury. In the determination of Bi(III) at pH 1.0, thiocyanate is used to mask Hg(II). The mercury thiocyanate complex is then decomposed by silver ions and the liberated mercury(II) titrated with EDTA at * Present address: