Abstract: Nano-Bismuth ferrate (BiFeO3) was prepared by the sol-gel method and used as Fenton reagent in the fluorophotometric determination of phthalates (PAEs) in atmospheric microparticles.The hydrolysate was neutralized with HCl (1+1) solution and its acidity was controlled at pH 7 with 0.03 mol·L-1 phosphate buffer solution.Bismuth ferrate (0.050 0 g) and H2O2 were added to render to concentration of H2O2 attained to 0.02 mol·L-1 in a total volume of 100 mL.The solution was irradiated under a high-pressure mercury lamp for 3.5 h to carry out the photocatalytic heterogeneous Fenton′s reaction.Determination of PAE′s was performed by measuring the fluorescence intensity (IF) at 417 nm.Taking diethylphthalate (DEP) as example,linear relationship between values of IF and concentration of DEP was kept in the range of 3.8×10-7-4.8×10-5mol·L-1,with its detection limit (3S/N) of 5.43×10-8mol·L-1.Values of recovery found by standard addition method were in the range of 90.8% to 108%,with values of RSD′s (n=7) ranged from 2.1% to 8.3%.