Microdetermination of Fluoride in Vegetation by Oxygen Bomb Combustion and Fluoride Ion Electrode Analysis

Abstract

Classical procedures for the microdetermination of fluoride in vegetation are extremely time consuming. They generally involve ashing, fusion with alkali, distillation, and finally fluoride estimation. Sample size requirements for such procedures are on the order of a gram or more, making the procedure useless for determining low fluoride concentrations in small samples. A procedure for micro-fluoride determination in vegetation is proposed which utilizes the oxygen flask combustion technique (Schoniger flask). The gaseous products of combustion are absorbed in 10.0 ml of 0.05N sodium hydroxide containing 1.00 µg of fluoride. The analysis of the fluoride is performed directly on the absorption solution after addition of a combination complexing-buffer solution, using a specific fluoride ion electrode. The sensitivity of the electrode is such that 0.2 µg of fluoride can be easily detected in this volume. Added oxidant was required in the combustion step for some vegetation samples to completely free the fluoride from its organic matrix. Comparisons with the standard Willard-Winter procedure gave excellent results. Combustion of sodium fluoride standards as well as submicrogram quantities of a fluoro-organic compound showed recoveries greater than 90%. The direct combustion, coupled with fluoride ion electrode determination, reduces analysis time drastically. A complete analysis can be performed in 1/2 hr, with a minimum amount of equipment.