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Weigh, to the nearest 0.1 mg, 0.25 g of the sample, previously
dried at
105º for 3 h. Dissolve in 36 ml of glacial acetic acid and 4 ml
acetic
anhydride in a 250-ml glass-stoppered flask, warming to effect
solution.
Cool to room temperature, add 2 drops of crystal violet TS and
titrate
with 0.1 N perchloric acid in glacial acetic acid to a blue-green end
point
which persists for at least 30 sec. Perform a blank determination
and
make any necessary correction. Each ml of 0.1 N perchloric acid is
equivalent to 15.02 mg of C6H7KO2.
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