RI 6314 Fluorine Analyses. Control Method for Various Compounds

Defluorination studies on refractory fluoride - bearing compounds and minerals , particularly on partly defluorinated residues from high - temperature pyrohydrolysis , required a dependable and reasonably accurate analyticalcontrol method for the analysis of fluorine . The difficulty in liberating fluorine from the fluorides of metallic elements such as aluminum, zirconium , and rare earths by steam- distillation can be largely overcome if the distillation is made from a sulfuric - phosphoric acid solution of a sodium carbonate fusion of the sample material and if the distillation temperature is maintained at about 155 ° C. The data presented in this paper show that liberation of fluorine by this method is more complete and proceeds more rapidly than by usual distillations from perchloric or sulfuric acid alone or a mixture of phosphoric and perchloric acids . Fluorine in amounts ranging up to about 140 mg can be recovered by collecting only about 300 ml of distillate . Determination of fluoride in the distillate is made by the usual thorium nitrate titration .