Abstract: This article reports an express determination method of cerium and lead by fluorimetric analysis, based on the characteristics of cerium(Ⅲ) and lead(Ⅱ)in the medium of potassiumchloride. Under the conditions of test with the excitation wave length of 262.5nm, the emissionspectra between 300-520 nm were achieved by scanning at the speed of 120 nm/min,on wiichthe peak height (ΔF)at 352. 4 nm was proportional to 2. 0× 10^-8-2. 0×10^-6 mol/L Ce³⁺andthat at 485. 0 nm proportional to 4. 0× 10^－7-1. 0× 10^－5mol/L Pb²⁺. No significant differencewas found between the results of reference stream sediment sample analysis and the referencevalue. The determination limit was 1.5 × 10^-8 mol/L for Ce³⁺ and 2. 0× 10^－7 mol/L for Pb²⁺。