Packaging and storage—
Preserve in tight containers.
Identification—
A:
Mix 2 mL with 15 mL of water, 5 mL of sulfuric acid, and 10 g of potassium dichromate, heat the mixture under a reflux condenser for 2 hours, and then distil, collecting and reserving the first 2 mL of the distillate. Continue the distillation until most of the water has distilled over, render this distillate alkaline with 1 N sodium hydroxide, add 2 N sulfuric acid dropwise until the solution is neutral to litmus, and carefully evaporate to dryness: the residue responds to the tests for
Acetate 
191
.
B:
To 1 mL of the reserved distillate obtained in
Identification test
A add 5 drops of
sodium nitroferricyanide TS and 2 mL of 1 N sodium hydroxide, then add a slight excess of 6 N acetic acid: a deep red liquid, which develops a violet tint when diluted with several volumes of water, is produced.
C:
To 10 mL of a solution (1 in 10) quickly add 5 mL of a 1 in 100 solution of vanillin in sulfuric acid: a violet-red color is produced.
Water—
The relative retention time of water on the gas chromatographic column used in the
Assay is approximately 0.2 times that of Amylene Hydrate. From the area under the curve obtained in the
Assay, calculate the percentage (a/a) of water in the Amylene Hydrate taken: not more than 0.5% is found.
Limit of nonvolatile residue—
Evaporate 10 mL in a tared porcelain dish on a steam bath to a volume of about 1 mL, and allow it to evaporate spontaneously to dryness while protected from dust: the residue, if any, is colorless, and, when dried at 105
for 1 hour, weighs not more than 2 mg (0.02%).
Heavy metals, Method I 231—
Evaporate 5.0 mL (4 g) on a steam bath to dryness, warm the residue gently with 1 mL of dilute hydrochloric acid (1 in 120), add water to make 25 mL, and filter, if necessary: the limit is 0.0005%.
Readily oxidizable substances—
To 10 mL of a solution (1 in 20) add 0.10 mL of 0.10 N potassium permanganate: the pink color does not completely disappear within 10 minutes.
Aldehyde—
To 10 mL of a solution (1 in 20) add 1 mL of silver-ammonium nitrate TS, and heat the mixture on a water bath at 60
for 10 minutes: no darkening occurs.
Assay—
Inject 0.4 µL of Amylene Hydrate into a suitable gas chromatograph (see
Chromatography 621) equipped with a thermal conductivity detector. Under typical conditions, the instrument contains a 4-mm × 2-m glass column packed with chromatographic support S2. The column is maintained at a temperature of 190
, the injection port is maintained at about 200
, the detector block is maintained at about 200
, and helium is used as a carrier gas at a flow rate of about 50 mL per minute. From the area under the curve, calculate the percentage (a/a) of C
5H
12O in the Amylene Hydrate taken.
;)
