A sensitive spectrophotometric method for the determination of trace amounts of hydrogen sulphide (H2S) after fixing in a modified zinc acetate-disodium ethylenediaminetetraacetate-sodium hydroxide solution is described. The fixed H2S is stable for 3 d. The reaction of iodate with H2S in the presence of acid and an excess of chloride leads to the formation of ICI which is stabilised as ICI2-. The species formed reacts with 2',7'-dichlorofluorescein to form 2',7'-dichloro-4',5'-diiodofluorescein which is extracted into a mixture of 15% isoamyl acetate in isoamyl alcohol. The colour system obeys Beer's law in the range 0-2.5 micrograms of H2S. The coefficient of variation is 4.5% for ten determinations of 2.0 micrograms of H2S. The effect of interfering gases on the determination is discussed. The method was applied to the determination of residual amounts of H2S present in a laboratory fume cupboard and the results obtained were compared with those given by the widely used Methylene Blue method. The method can be used to determine down to 0.3 micrograms of H2S.