ANALYSIS OF TRANSITION METAL IN ZRF4 OR HFF4

摘要

PURPOSE:To enable analysis in ppb in a short time with a simple device by performing a wet type high pressure analysis on ZrF4 or HfF4 using hydrofluoric acid. CONSTITUTION:About 5g of ZrF4 as sample is placed into a wet type high pressure analysis container and 3ml in total capacity and after closed, it is kept at 150 deg.C with a thermostatic cell. After the container is allowed to cool, the content liquid is moved to a flask and diluted by water to 50ml in total capacity. Then, the solution is batched off by 10ml and 80ml of a reagent (H3Bo3-APDC solution) and 2-3 drops of a methyl orange indicator are added thereto and aqueous ammonia is dropped until the solution turns yellow slightly. 3ml of MIBK is added to the solution and, then, allowed to stand for about one hour. A water layer is thrown away and a MIBK layer is shifted to a solvent volatalizing container. 1.5ml of nitric acid is added thereto and the mixture is heated up to about 100 deg.C to volatilize MIBK. The residual liquid is diluted by water to 2ml in total capacity. Absorbance is measured from 20mul of the solution by frameless atomic absorption method. Then, an amount of each metal is determined by a calibration curve prepared preliminarily to calculate the content thereof by a specified formula.