The following details are discussed in the present paper, after high titanium slag and H3PO4 is put in the closed system,the .reaction takes place under controlled temperature conditions, and the gas produced is collected. The two phases of gas liquid attain kinetic equilibrium, ihe gas above the liquid is used to make GC analysis with the aid of chromatographic column of 5A molecular sieve, TCD and N2 30ml/min. Satisfactory quantitative results can be achieved with simple instruments and uncomplicated operation technique.