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Acidityoralkalinity—
Phenolphthaleinsolution—Dissolve0.1gofphenolphthaleinin80mLofalcohol,anddilutewithwaterto100mL.
Procedure—To20mLofalcohol,add20mLoffreshlyboiledandcooledwaterand0.1mLofPhenolphthaleinsolution.Thesolutioniscolorless.Add1.0mLof0.01Nsodiumhydroxide.Thesolutionispink(30ppm,expressedasaceticacid).
Ultravioletabsorption—RecordtheUVabsorptionspectrumofthetestmaterialfrom200to400nmina5-cmcell:maximumabsorbance0.40at240nm,0.30between250and260nm,and0.10between270and340nm.Examinebetween235and340nm,ina5-cmcell,usingwaterasthecompensationliquid.Theabsorptioncurveissmooth.Volatileimpurities—
TestsolutionA:substancetobeexamined.
TestsolutionB—Add150Lof4-methylpentan-2-olto500.0mLofthesubstancetobeexamined.
StandardsolutionA—Dilute100Lofmethanolwiththesubstancetobeexaminedto50.0mL.Dilute5.0mLofthesolutionwiththesubstancetobeexaminedto50.0mL.StandardsolutionB—Dilute50Lofmethanoland50Lofacetaldehydewiththe
substancetobeexaminedto50.0mL.Dilute100Lofthesolutionwiththesubstancetobeexaminedto10.0mL.
StandardsolutionC—Dilute150Lofacetalwiththesubstancetobeexaminedto50.0mL.Dilute100Lofthesolutionwiththesubstancetobeexaminedto10.0mL.
StandardsolutionD—Dilute100Lofbenzenewiththesubstancetobeexaminedto100.0mL.Dilute100Lofthesolutionwiththesubstancetobeexaminedto50.0mL.Chromatographicsystem(see)—Thegaschromatographisequippedwithaflame-ionizationdetector,maintainedatabout280,anda0.32-mm30-mfusedsilicacapillarycolumnbondedwitha1.8-mlayerofphaseG43.Thecarriergasisheliumwithalinearvelocityofabout35cmpersecondandasplitratioof1:20.Thecolumntemperatureismaintainedat40forthefirst12minutesafteraninjectionismadeandisincreasedfrom40to240from12to32minutesafterinjection.Duringtheperiodof32to42minutesafteraninjectionismadethecolumntemperatureismaintainedat240.Theinjectionporttemperatureismaintainedat200.ChromatographStandardsolutionB,andrecordthepeakresponsesasdirectedforProcedure:theresolution,R,betweenthefirstmajorpeak(acetaldehyde)andthesecondmajorpeak(methanol)isnotlessthan1.5.
Procedure—Separatelyinjectequalvolumes(1.0L)of
TestsolutionA,TestsolutionB,
StandardsolutionA,StandardsolutionC,andStandardsolutionDintothe
chromatograph,recordthechromatograms,andmeasurethemajorpeaks.CalculatetheconcentrationofmethanolinTestsolutionA:notmorethanhalftheareaofthe
correspondingpeakinthechromatogramobtainedwithStandardsolutionA(200ppm).Calculatethesumofthecontentsofacetaldehydeandacetal,expressedas
acetaldehyde,usingthefollowingformula:
[(10AE)/(AT–AE)]+[(30CE)/(CT–CE)]
inwhichAEistheareaoftheacetaldehydepeakinthechromatogramobtainedwithTestsolutionA;ATistheareaoftheacetaldehydepeakinthechromatogramobtainedwithStandardsolutionB;CEistheareaoftheacetalpeakinthechromatogramobtainedwithTestsolutionA;andCTistheareaoftheacetalpeakinthechromatogramobtainedwithStandardsolutionC:notmorethan10ppm,expressedasacetaldehydeisfound.Calculatethecontentofbenzeneusingthefollowingformula:
(2BE)/(BT–BE)
inwhichBEistheareaofthebenzenepeakinthechromatogramobtainedwithTestsolutionA,andBTistheareaofthebenzenepeakinthechromatogramobtainedwithStandardsolutionD:notmorethan2ppmisfound.Ifnecessary,theidentityofbenzenecanbeconfirmedusinganothersuitablechromatographicsystem(stationaryphasewithadifferentpolarity).
ThetotalofallotherimpuritiesinthechromatogramobtainedwithTestsolutionBisnotmorethantheareaofthepeakdueto4-methylpentan-2-olinthechromatogramobtainedwithTestsolutionB(300ppm).Disregardanypeaksthatare0.03timestheareaofthepeakcorrespondingto4-methylpentan-2-olinthechromatogramobtainedwithTestsolutionB(9ppm).
Limitofnonvolatileresidue—Evaporate100mLinatareddishonawaterbath,anddryat100to105for1hour:theweightoftheresiduedoesnotexceed2.5mg.
AuxiliaryInformation—Pleasebefo
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