On-line flow injection solid sample introduction, leaching and potentiometric determination of fluoride in phosphate rock

Abstract

A flow injection method with on-line solid sample dissolution was developed for the determination of fluoride in phosphate rock. The fluoride was selectively leached (98–102.4 % recovery) from a 50-mg powdered phosphate rock sample with 0.50 M citric acid. Using the zone sampling technique the fluoride in the buffered leachate was determined by injecting 87 μL into the carrier stream using a fluoride ion-selective electrode detector. The sensing element of the electrode was housed in a home-made sleeve-type flow-through cell. On-line solid sample digestion with 0.50 M citric acid at 55 °C resulted in minimum dissolution of interfering iron and aluminum ions with improved accuracy and calibration linearity. The incorporation of relatively high level of fluoride in the carrier stream (40 μg mL −1) facilitated the determination of high levels of fluoride in phosphate rock (up to 4.1%) with out the need for excessive on-line dilution. The optimized flow system was applied for the determination of fluoride in phosphate rocks samples and a reference material at a rate of nine samples per hour with a relative standard deviation ( n = 5) of 2.95–4.0 %. Comparison of the proposed flow injection method with the standard method, which involves steam distillation from sulfuric acid solution and manual titration with thorium nitrate, showed no evidence of bias at the 95% confidence level.