By Anil K. Mukherji, R. Belcher and M. Frieser (Auth.)
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Additional info for Analytical Chemistry of Zirconium and Hafnium
The results are presented in Fig. 3. It was observed that depolymerization increased on standing with increase in acidity from 1 to 3 N with respect I 0 1 2 1 4 1 6 I 8 I 10 I 12 I 14 I 16 I 18 I 20 Time, days FIG. 3. 5 N, N, and 3 N H2S04, curves C, D, and E, respectively. 5 to 3 N with respect to sulfuric acid. The rate of depolymerization was greatest in nitric acid and smallest in sulfuric acid. Therefore, if complete depolymerization is to be affected by ageing, the zirconium solution must be at least 2 N in nitric acid.
Bi 3+ interferes. 2-4 N HCl. 5 to 1. 5 N HC1. -Bromomandelic acid /7-Chloromandelic acid Zr(BrC8H603)4 Zr(ClC8H603)4 S H Zr(BrC8H603)4 Zr(ClC8H603)4 Ppted from dil. HC1. No interferences (82-89, 133-137) Less sol. than Zr mandelate (82,90-97) No advantage over mandelic acid (98, 94-97) 2 o ö in 5 > H o-, m- and /7-Fluoromandelic Zr(FC8H603)4 acid Zr0 2 No advantage over mandelic acid (82, 99) Zr(F3C8H403)4 ZrOo No advantage over mandelic acid (82) Trifluoromandelic acid > < 3 2 o TABLE 2—cont. 6 N H 2 S0 4 .
1 % aqueous) and heat to boiling. 1 M) to a color change from purple to pale orange. Cool, add 10 ml of 7 N NH4OH, and boil to restore the strong purple color. Titrate to a sharp change to lemon yellow. Confirm the endpoint by adding 1-2 ml of the ammonium hydroxide solution and reheating. No further change from lemon yellow color indicates a true endpoint. Excessive use of ammonia changes the indicator color to purple. Note. (1) Loss of volume in the depolymerization digestion is immaterial. Evaporation to fumes is equally effective.
Analytical Chemistry of Zirconium and Hafnium by Anil K. Mukherji, R. Belcher and M. Frieser (Auth.)