A fluorometrjc method for the determination of F(superscript -) is developed. The fluorescence of calcein in pH=8.9 buffer solution can be quenched when the calcein reacts with Al(superscript 3+)The complex of F(superscript -) and Al(superscript 3+) is more stable than that of calcein-Al(superscript 3+) When F reacts with calcein-Al(superscript 3+), the fluorescence of calcein can be recovered. The changes of fluorescence has a linear relationship with the concentration of F(superscript -) in the range of 1.0×10^(-4)-1.0×l0^(-3)mol/L.