USP乙醇内容及相关附录.docVIP

Alcohol (al ka hol). C2H6O46.07 Ethanol;????Ethyl alcohol????[64-17-5]. DEFINITION Alcohol contains NLT 92.3% and NMT 93.8%, by weight, corresponding to NLT 94.9% and NMT 96.0%, by volume, at 15.56, of C2H5OH. IDENTIFICATION ???A. It meets the requirements of the test for Specific Gravity 841. ???B. Infrared Absorption 197For197S: Neat IMPURITIES Inorganic Impurities? ???Limit of Nonvolatile Residue: Evaporate 100 mL in a tared dish on a water bath, and dry at 100–105 for 1 h: the weight of the residue is NMT 2.5 mg. Organic Impurities? ???Procedure Sample solution A:?Alcohol (substance under test) Sample solution B:?300 ppm of 4-methylpentan-2-ol in Sample solution A Standard solution A:?200 ppm of methanol in Sample solution A Standard solution B:?10 ppm of methanol and 10 ppm of acetaldehyde in Sample solution A Standard solution C:?30 ppm of acetal in Sample solution A Standard solution D:?2 ppm of benzene in Sample solution A Chromatographic system? (See Chromatography 621, System Suitability.) Mode:?GC Detector:?Flame ionization Column:?0.32-mm × 30-m fused silica capillary column bonded with a 1.8-μm layer of phase G43 Split ratio:?20:1 Temperature? Detector:?280 Injector:?200 Column:?See the temperature program table below. Initial Temperature () Temperature Ramp(/min) Final Temperature () Hold Time at Final Temperature (min) 40 0 40 12 40 10 240 10 Linear velocity:?35 cm/s Carrier gas:?Helium Injection size:?1.0 μL System suitability? Sample:?Standard solution B Suitability requirements? Resolution:?NLT 1.5 between the first major peak (acetaldehyde) and the second major peak (methanol) Analysis? Samples:?Sample solution A, Sample solution B, Standard solution A, Standard solution B, Standard solution C, and Standard solution D Methanol calculation? Result = (rU/rS) rU = = peak area of methanol from Sample solution A rS = = peak area of methanol from Standard solution A Acetaldehyde and Acetal calculation?