A process for treating spent pickle liquor has the steps of mixing the spent pickle liquor with sulfuric acid, introducing oxygen into the mixture of spent pickle liquor and the sulfuric acid for a period of time, and producing diiron(II) tetrachlorosulfate from the oxygen-introduced mixture of sulfuric acid and spent pickle liquor. The spent pickle liquor and the sulfuric acid are introduced into a column. The oxygen is passed under pressure into the column. The intimate mixture of spent pickle liquor, sulfuric acid and oxygen are maintained under pressure for a period of time.