【astm標準】d 2363 - 79 (2011)

1、Designation:D2363?79(Reapproved2011)StardTestMethodsfHydroxypropylMethylcellulose1ThisstardisissuedunderthefixeddesignationD2363thenumberimmediatelyfollowingthedesignationindicatestheyearofiginaladoptioninthecaseofrevisi

2、ontheyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperepsilon()indicatesaneditialchangesincethelastrevisionreapproval.1.Scope1.1Thesetestmethodscoverthetestingofhydroxypropylmethylcellulose.1

3、.2Thetestproceduresappearinthefollowingder:SectionsMoisture4to6Ash(asSulfate)7to10Chlides(asNaCl)11to14Alkalinity(asNa2CO3)15to18Iron19to24HeavyMetals25to29MethoxylContent30to35HydroxypropoxylContent36to41Viscosity42to46

4、pH47Solids48to51Density52to561.3ThevaluesstatedinSIunitsaretoberegardedasthestard.Thevaluesgiveninparenthesesarefinfmationonly.1.4Thisstarddoesnotpurpttoaddressallofthesafetyconcernsifanyassociatedwithitsuse.Itistherespo

5、nsibilityoftheuserofthisstardtoestablishappropriatesafetyhealthpracticesdeterminetheapplicabilityofregulatylimitationspritouse.Faspecifichazardstatementsee33.5.1.2.ReferencedDocuments2.1ASTMStards:2D96TestMethodfWaterSed

6、imentinCrudeOilbyCentrifugeMethod(FieldProcedure)(Withdrawn2000)3E70TestMethodfpHofAqueousSolutionsWiththeGlassElectrode3.PurityofReagents3.1Reagentgradechemicalsshallbeusedinalltests.Unlessotherwiseindicateditisintended

7、thatallreagentsshallconfmtothespecificationsoftheCommitteeonAnalyticalReagentsoftheAmericanChemicalSocietywheresuchspecificationsareavailable.4Othergradesmaybeusedprovideditisfirstertainedthatthereagentisofsufficientlyhi

8、ghpuritytopermititsusewithoutlesseningtheaccuracyofthedetermination.3.2Unlessotherwiseindicatedreferencestowatershallbeunderstoodtomeandistilledwater.MOISTURE4.Scope4.1Thistestmethodcoversthedeterminationofthevolatilecon

9、tentofhydroxypropylmethylcellulosebycommonusagedesignatedmoisture.5.Procedure5.1Transfer2to5gofthesampleweighedtothenearest0.01gtoatareddish(fittedwithalid)dryf2hinanovenat100to105Cwithlidremoved.Removethedishfromtheoven

10、coverwithalidcoolinadesiccatweigh.6.Calculation6.1Calculatethepercentofmoistureasfollows:Moisture%5~AB!3100(1)where:A=masslossonheatingB=sampleusedg.ASH—ASSULFATE7.Scope7.1Thistestmethodcoversthedeterminationoftheamounto

11、fresidueleftfromignitingasampleofhydroxypropylmethylcelluloseafterbeingmoistenedwithsulfuricacid.1ThesetestmethodsareunderthejurisdictionofASTMCommitteeD01onPaintRelatedCoatingsMaterialsApplicationsarethedirectresponsibi

12、lityofSubcommitteeD01.36onCelluloseCelluloseDerivatives.CurrenteditionapprovedJune12011.PublishedJune2011.iginallyapprovedin1965.Lastpreviouseditionapprovedin2006asD2363–79(2006).DOI:10.1520D236379R11.2FreferencedASTMsta

13、rdsvisittheASTMwebsitewww.astm.gcontactASTMCustomerServiceat.FAnnualBookofASTMStardsvolumeinfmationrefertothestard’sDocumentSummarypageontheASTMwebsite.3Thelastapprovedversionofthishisticalstardisreferencedonwww.astm.g.4

14、ReagentChemicalsAmericanChemicalSocietySpecificationsAmericanChemicalSocietyWashingtonDC.FsuggestionsonthetestingofreagentsnotlistedbytheAmericanChemicalSocietyseeAnalarStardsfLabatyChemicalsBDHLtd.PooleDsetU.K.theUnited

15、StatesPharmacopeiaNationalFmularyU.S.PharmacopeialConventionInc.(USPC)RockvilleMD.Copyright?ASTMInternational100BarrHarbDrivePOBoxC700WestConshohockenPA194282959.UnitedStates1S5@~AB30.053!C#3100(5)where:A=H2SO4requiredft

16、itrationofthesamplemLB=nmalityoftheH2SO4C=sampleusedg.IRON19.Scope19.1Thistestmethodcoversthedeterminationoftotalironcontentinsamplesofhydroxypropylmethylcellulose.Theironisconvertedtoferricsulfatewhichreactswiththeindic

17、attofmapinkcolthatcanbequantitativelymeasured.20.Apparatus20.1Photometer—Anyphotoelectricfilterphotometerspectrophotometersuitablefmeasurementsat430nm.20.2KjeldahlFlasks—Calibratedtocontain50mLmadeofheatchemicalresistant

18、glass.21.Reagents21.1AmmoniumHydroxide(spgr0.90)—Concentratedammoniumhydroxide(NH4OH).21.2BufferSolution—Dissolve20gofsodiumbicarbonate(NaHCO3)10gofsodiumcarbonate(Na2CO3)inwaterdiluteto1L.21.3Disodium12Dihydroxybenzene3

19、5DisulfonateSolution—Prepareanaqueoussolutioncontaining25gL.21.4HydrochlicAcid(spgr1.19)—Concentratedhydrochlicacid(HCl).21.5HydrogenPeroxide(30%)—Concentratedhydrogenperoxide(H2O2).21.6IronStardSolution(0.0001gFeml)—Dis

20、solve0.01gofironpowdercontainingnotlessthan99.9%ironinHCl(spgr1.19).Oxidizethesolutionwithbrominewaterexpeltheexcessbyboiling.Diluteto1Linavolumetricflask.21.7PhenolphthaleinIndicatSolution(1g100mL)—Dissolve1gofphenolpht

21、haleinin100mLofethanol(95%).21.8SulfuricAcid(spgr1.84)—Concentratedsulfuricacid(H2SO4).21.9SulfuricAcid(14)—Carefullymix1volumeofH2SO4(spgr1.84)with4volumesofwateraddingtheH2SO4graduallywhilemixing.22.PreparationofCalibr

22、ationCurve22.1FollowingtheproceduregiveninSection23usingvariedamountsofthestardironsolutionpreparedinaccdancewith21.6prepareacalibrationcurveshowingironcontentinpartspermillionthecrespondingphotometerreadings.23.Procedur

23、e23.1Weightothenearest0.01gabout2gofthesample(previouslydriedf1?2hat100to105C).TransferbymeansofafunneltoaKjeldahlflask.Placetheflaskata20angleinthefurnaceat500Cheatuntilsomeringofthesamplehastakenplace.(Caremustbetakenn

24、ottotoomuch.)Removeallowtocool.23.2Add3mLofH2SO4totheflask.Placeonthedigestionrackdigest.CooladdH2O2wiseuntilthesolutionisclear.HeatoveraMekerburnertoavolumeof2mL.Coolwashthesidesoftheflaskwithwater.Add3sofphenolphthalei

25、nindicatsolution.AddNH4OHtoaredendpoint.Washtheneckoftheflask.Thesolutionshouldbeclearnotgreaterthan20mLinvolume.23.3Add2mLofthecolfmingsolutiondescribedin21.3mix.AdjustpHto7.0thendilutetomarkwithbuffer.Transferasmallpti

26、ontoanabsptioncelldeterminethephotometerreadingat480nm.23.4Blank—Makeablankdeterminationusingthesameamountofreagentsthesameprocedureasfthesample.24.Calculation24.1Readtheironcontentinpartspermilliondirectlyfromthecalibra

27、tioncurve(Section22).Subtractthepartspermillionofironduetoironintheblank.HEAVYMETALS25.Scope25.1Thistestmethodcoversthedeterminationofwhethernottheheavymetalscontentofhydroxypropylmethylcelluloseisbelowagivenlevelbasedon

28、aleadstard.26.SummaryofTestMethod26.1Theashresiduefromthesulfatedashtestisdigestedwithdilutehydrochlicacid.Astardcontainingaknownamountofleadispreparedtheheavymetalscontentisdeterminedqualitativelybycomparingthesampletot

29、hestard.27.Apparatus27.1NesslerTubes50mL.27.2VolumetricFlasks50mL.28.Reagents28.1AceticAcid—Glacialaceticacid.28.2AmmoniumHydroxide(spgr0.90)—Concentratedammoniumhydroxide(NH4OH).28.3AmmoniumHydroxide(23)—Dilute400mLofNH

30、4OH(spgr0.90)withsufficientwatertomake1000mL.28.4BufferSolution—Dissolve60mLofaceticacidinabout500mLofwateradd10mLofNH4OHdiluteto1L.28.5HydrochlicAcid(12)—Dilute1volumeofconcentratedhydrochlicacid(HClspgr1.19)with2volume