The determination of zirconium in fluoride-containing solutions

In the recommended procedure the zirconium is first precipitated from solution as the insoluble barium fluozirconate. After separation, the precipitate is dissolved in a mixture of nitric and boric acids and the zirconium is then precipitated as its hydroxide. This precipitate is separated, dissolved in hydrochloric acid and this solution is evaporated to fumes of perchloric acid to remove completely fluoride ions. The zirconium content is then determined volumetrically by adding a slight excess of a standard solution of ethylenediaminetetra-acetic acid and back titrating with a standard iron solution at pH 2.3 using potassium benzohydroxamate as indicator and the photometric technique for end-point detection. This method is applicable to the determination of milligram amounts of zirconium in fluoride-containing nitric or hydrochloric acid solutions provided that the concentration of these acids is below 3N. It is also suitable for the determination of zirconium in the presence of any of the following elements - uranium, titanium, niobium, tantalum, molybdenum, tungsten, lead, iron, copper and tin.