Effective determination for enrichment of the uranium materials in heavy shielding is technically difficult to solve. Various technical methods so far have been proposed to deal with this problem. With the time-correlated coincidence measurement method, 14 MeV neutrons and fission spectrum neutrons are chosen to interrogate the uranium samples with different masses and enrichments. The fission spectrum neutrons are obtained by slowing down the 14 MeV neutrons. Results have shown that a good linear relationship exists between masses of the uranium materials (≤10% enriched 235U) that possess the same enrichment. A linear relationship also exists between enrichments of the uranium materials that possess the same mass.