By Anil K. Mukherji, R. Belcher and M. Frieser (Auth.)
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Extra resources for Analytical Chemistry of Zirconium and Hafnium
A survey of direct titration procedures shows that they do not offer both a sharp endpoint and acceptable accuracy. Several indicators have been suggested for EDTA titrations, but xylenol orange (3,3-bis-di(carboxymethyl)aminomethyl-o-cresolsulfonephthalein) seems to provide the sharpest color change in acidic media. 6 N H N 0 3 solutions which Milner and Edwards (21) found to give slow endpoints and low results, however. For most other procedures, reported results are always lower than the theoretical value, and variations in results seem to be dependent on the concentration of zirconium, temperature, and pH of the solution.
Indicator color at the start is brownorange, rather than purple, which is obtained later in the titration on addition of ammonia. 001 N EDTA. Decrease the amount of sulfuric acid to 10 milliequivalents and depolymerize by evaporation to fumes. Cool, add 25 ml of hot water. Boil and titrate as in procedure A, using only 1 ml of 7 N NH4OH near the endpoint. Re-boil to confirm the endpoint. Interferences The above procedures may not be free from interferences, especially because of the change in pH near the endpoint.
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