Abstract
A solution containing zirconium, iron and copperis treated with EDTA, the reaction is adjusted to pH 1.5 and heated with cupferron for masking of zirconium and precipitation of iron and copper, then the precipitate is extracted with ethyl ether for separation of iron and copper (Table 2). Also, titanium and tin are separated by this method. Quantitative determination of zirconium was possible by adjusting the solution to pH 3.0 and titrating the excess EDTA with a standard copper sulfate solution, using α-pyridyl-β-azonaphthol as an indicator (Table 1). Zirconium in ferro-zirconium alloy was determined by this method and good results were obtained as indicated in Table 3. The time required for analysis was about 30 min. The procedure is carried out as follows: The sample (0.5g) is decomposed with a mixture of 50ml HCl (1+1), 2g NH4F and 2 ml conc HNO3, evaporated by heating after addition of 20ml 60% HClO4, heated for 5 min at white fuming temperature for driving off the F, the residue is tranferred into a 250ml measuring flask and filled up to the mark with water, 2025ml portion of the solution is treated with an excess EDTA and NH4Ac to pH 1.5 and the titration is carried as above for quantitative determination of zirconium.
