A method for activating ISE is proposed that can allow determination of the fluoride concentration at ng mL(-1) level with good precision and accuracy. Fluoride ISE is activated in 0.5 mol L(-1) HClO4 medium and then fluoride is determined in the same medium. The linear range for the determination of fluoride is between 1.00 x 10(-2)-1.00 x 10(-7) mol L(-1), and the detection limit of the method is 1.0 ng mL(-1). The advantage of this method is that it is free from the use of TISAB solution while being, time-saving and labor-saving. A mechanism study of the activation of FISE in HClO4 medium is explained. The method has been used for the determination of trace fluoride in milk and flour with satisfactory results.