Determination of titanium, zirconium, lead and additives in lead zirconate titanate by ICP-AES

A powdered (agate pot and vibrating mixer mill is used) sample (0.2g) is decomposed with a mixed acid solution (15ml of hydrochloric acid +1ml of hydrofluoric acid) in a Teflon bomb. When the resultant solution is diluted directly with water, large quantities of precipitates (consisting of titanium, zirconium and lead compounds etc.) are observed. To avoid this, the following procedure is employed; The solution is transferred into a polyethylene beaker containing 1.5g of citric acid. After pH adjustment to 89, most of the precipitates can be dissolved by the addition of 2.0g of EDTA·2Na. The remaining LaF3 precipitate is dissolved by heating with 1.5g of boric acid and 20 ml of nitric acid. After cooling, this solution is used for rinsing the bomb, and is transferred into a 250ml volumetric flask. An aliquot of 25ml is diluted four times with water and analysed by ICP-AES. The procedure described here provides a rapid and precise (R.S.D.