In this article a method is investigated for the determination of low-valence titanium in slag containing a high titanium content. The residue is dissolved using H2SO4-HF-H3PO4 after tMFe, Fe2O3 and the part of FeO are separated from sample with FeCl3-HCl, and NH4 Fe(SO4)2 is added to oxidate low titanium. Then the standard solution of K2Cr2O7 is used to tit-rat Fe2+ in sample solution. The method possesed with a advantage of simple rapid and good repeatability so that it can be used in the roution determination.