In this paper, a novel and sensitive method based on Rayleigh light scattering technique (RLS) wasproposed for the determination of sulfate using a conventional spectrofluorometer. Sulfate wastransformed to BaSO
4 particles, which displayed intense light scattering in aqueous solutions. Theeffects of factors such as wavelength, acidity, stabilizers and interferents were studied in detail. TheRLS intensity of the BaSO
4 suspension was obtained in 0.1 mol L
-1 of [H
+] and the addition of 2 mLof cationic polyacrylamide (CPAM) with 7.05 × 10
-3 mmol mL
-1 charged cations and 1.0 mL of BaCl
2·2H
2O (5.0%) at 510 nm. In the range of 8-400
g mL
-1, RLS intensity was linear to the concentrationof BaSO
4, and the detection limit was 0.3
g mL
-1. To determine the feasibility of the proposedmethod, some samples of water, drinks, and vegetables digests were analyzed, and the results werein agreement with the standard turbidimetric method. Good recovery results were also obtained inthe range of 94-105%. Although this method was limited in stability, it was characterized withsimplicity, sensitivity, reliability, and little interference.Keywords: Sulfate determination; Rayleigh light scattering; barium sulfate