Thiobenzoylphenylhydroxylamine (TBPHA) quantitatively precipitates iron(III) in 1 F acid solution as Fe(C13H10NSO)3; the complex is ignited to Fe2O3. Aluminium, chromium, manganese and a number of common accompanying elements do not interfere. TBPHA can be used to separate copper from iron and to determine iron directly in the filtrate from the copper precipitation. Results obtained for iron standards, copper-iron mixtures, and steel and ore analyses are tabulated. © 1969.