Amylene Hydrate
;)
2-Butanol,2-methyl-.
tert-Pentyl alcohol [75-85-4].
»Amylene Hydrate contains not less than 99.0percent and not more than 100.0percent of C5H12O.
Packaging and storage—
Preserve in tight containers.
Identification—
A:
Mix 2mLwith 15mLof water,5mLof sulfuric acid,and 10g of potassium dichromate,heat the mixture under a reflux condenser for 2hours,and then distil,collecting and reserving the first 2mLof the distillate.Continue the distillation until most of the water has distilled over,render this distillate alkaline with 1Nsodium hydroxide,add 2Nsulfuric acid dropwise until the solution is neutral to litmus,and carefully evaporate to dryness:the residue responds to the tests for Acetate á191ñ.
B:
To 1mLof the reserved distillate obtained in Identificationtest Aadd 5drops of sodium nitroferricyanide TSand 2mLof 1Nsodium hydroxide,then add a slight excess of 6Nacetic acid:a deep red liquid,which develops a violet tint when diluted with several volumes of water,is produced.
C:
To 10mLof a solution (1in 10)quickly add 5mLof a 1in 100solution of vanillin in sulfuric acid:a violet-red color is produced.
Specific gravity á841ñ:
between 0.803and 0.807.
Distilling range,Method Iá721ñ—
It distills completely between 97
and 103,a correction factor of 0.037per mm being applied as necessary.
and 103,a correction factor of 0.037per mm being applied as necessary.
Water—
The relative retention time of water on the gas chromatographic column used in the Assayis approximately 0.2times 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 10mLin a tared porcelain dish on a steam bath to a volume of about 1mL,and allow it to evaporate spontaneously to dryness while protected from dust:the residue,if any,is colorless,and,when dried at 105for 1hour,weighs not more than 2mg (0.02%).
for 1hour,weighs not more than 2mg (0.02%).
Heavy metals,Method Iá231ñ—
Evaporate 5.0mL(4g)on a steam bath to dryness,warm the residue gently with 1mLof dilute hydrochloric acid (1in 120),add water to make 25mL,and filter,if necessary:the limit is 0.0005%.
Readily oxidizable substances—
To 10mLof a solution (1in 20)add 0.10mLof 0.10Npotassium permanganate:the pink color does not completely disappear within 10minutes.
Aldehyde—
To 10mLof a solution (1in 20)add 1mLof silver-ammonium nitrate TS,and heat the mixture on a water bath at 60for 10minutes:no darkening occurs.
for 10minutes:no darkening occurs.
Organic volatile impurities,Method Iá467ñ:
meets the requirements.
Assay—
Inject 0.4µLof Amylene Hydrate into a suitable gas chromatograph (see Chromatography á621ñ)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 50mLper minute.From the area under the curve,calculate the percentage (a/a)of C5H12Oin the Amylene Hydrate taken.
,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 50mLper minute.From the area under the curve,calculate the percentage (a/a)of C5H12Oin the Amylene Hydrate taken.
Auxiliary Information—
Staff Liaison:Catherine Sheehan,B.Sc.,Scientist
Expert Committee:(EMC)Excipients:Monograph Content
USP28–NF23Page 2957
Phone Number:1-301-816-8262