Radioiodine labelled human follicle stimulating hormone has been prepared using chloramine-T, with the approximate labelling yield of 65%. The labelled product is purified by means of a starch gel electrophoresis, and a Sephadex gel filtration, and the separation efficiencies are assessed for the effective use in radioimmunoassay. The results indicate that the gel filtration is efficient in view of the separation time, simplicity and bindability of the labelled hormone to the antibody. In determining the ratio of the free to the antibody bound labelled hormone, a double antibody technique is applied in comparison with a chromatoelectrophoresis. The ratio could be obtained only in the case of applying the double antibody technique.