Direct determination of fluoride in aluminium reduction materials by using an ion-selective electrode

Macro amounts of fluoride in aluminium reduction materials are successfully determined with a fluoride electrode. Except for anhydrous aluminium fluoride, which requires fusion with sodium hydroxide, samples are dissolved in aqueous media. Cryolite and sodium fluorosilicatc are dissolved in boiling sodium hydroxide solution. Other materials containing fluoride, such as fluorspar and the reduction cell bath and pot-lining, require dissolution in a hydrochloric acid solution of aluminium chloride. Potential interference from large amounts of aluminium (and calcium, if present) is eliminated and pH control attained by using ammoniacal sulphosalicylate (and EDTA). The procedures are reasonably rapid. Relative errors of less than 2% and a relative standard deviation of 1% are achieved.