【astm標準】d 1301 - 91 (2014)

1、Designation:D1301?91(Reapproved2014)StardTestMethodsfChemicalAnalysisofWhiteLeadPigments1ThisstardisissuedunderthefixeddesignationD1301thenumberimmediatelyfollowingthedesignationindicatestheyearofiginaladoptioninthecaseo

2、frevisiontheyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperepsilon()indicatesaneditialchangesincethelastrevisionreapproval.ThisstardhasbeenapprovedfusebyagenciesoftheU.S.DepartmentofDefense

3、.1.Scope1.1Thesetestmethodscoverproceduresfthechemicalanalysisofbasiccarbonatewhiteleadbasicsulfatewhitelead.NOTE1—IfitisnecessarytoseparatethesepigmentsfromothersrefertoPracticeD215.1.2Theanalyticalproceduresappearinthe

4、followingder:SectionPreparationofSample6BasicCarbonateWhiteLead:SmallAmountsofIron7TotalLead8MoistureOtherVolatileMatter9CarbonDioxide(EvolutionMethod)10CarbonDioxideCombinedWater(CombustionMethod)11LeadCarbonate12TotalM

5、atterInsolubleinAceticAcid13TotalMatterInsolubleinAcidAmmoniumAcetate14TotalImpuritiesOtherThanMoisture15CoarseParticles16BasicSulfateWhiteLead:SmallAmountsofIron17TotalLeadMoistureOtherVolatileMatter19TotalSulfate20Zinc

6、Oxide21BasicLeadOxide22TotalImpurities23CoarseParticles241.3ThevaluesstatedinSIunitsaretoberegardedasthestard.Thevaluesgiveninparenthesesarefinfmationonly.1.4Thisstarddoesnotpurpttoaddressthesafetyconcernsifanyassociated

7、withitsuse.Itistheresponsibilityoftheuserofthisstardtoestablishappropriatesafetyhealthpracticesdeterminetheapplicabilityofregulatylimitationspritouse.2.ReferencedDocuments2.1ASTMStards:2C25TestMethodsfChemicalAnalysisofL

8、imestoneQuicklimeHydratedLimeD185TestMethodsfCoarseParticlesinPigmentsD215PracticeftheChemicalAnalysisofWhiteLinseedOilPaints(Withdrawn2005)3D280TestMethodsfHygroscopicMoisture(OtherMatterVolatileUndertheTestConditions)i

9、nPigmentsD1193SpecificationfReagentWaterD2371TestMethodfPigmentContentofSolventReduciblePaintsD2372PracticefSeparationofVehicleFromSolventReduciblePaintsD3280TestMethodsfAnalysisofWhiteZincPigmentsE11SpecificationfWovenW

10、ireTestSieveClothTestSieves3.SignificanceUse3.1Thesetestmethodsaresuitablefdeterminingthelevelofpurityfdeterminingthelevelsofvariousimpurities.Theymaybeusedtoestablishcompliancewithspecificationrequirements.4.Reagents4.1

11、PurityofReagents—Reagentgradechemicalsshallbeusedinalltests.UnlessotherwiseindicateditisintendedthatallreagentsshallconfmtospecificationsoftheCommitteeonAnalyticalReagentsoftheAmericanChemicalSociety1Thesetestmethodsareu

12、nderthejurisdictionofASTMCommitteeD01onPaintRelatedCoatingsMaterialsApplicationsarethedirectresponsibilityofSubcommitteeD01.31onPigmentSpecifications.CurrenteditionapprovedDec.12014.PublishedDecember2014.iginallyapproved

13、in1953.Lastpreviouseditionapprovedin2008asD1301–91(2008).DOI:10.1520D130191R14.2FreferencedASTMstardsvisittheASTMwebsitewww.astm.gcontactASTMCustomerServiceat.FAnnualBookofASTMStardsvolumeinfmationrefertothestard’sDocume

14、ntSummarypageontheASTMwebsite.3Thelastapprovedversionofthishisticalstardisreferencedonwww.astm.g.Copyright?ASTMInternational100BarrHarbDrivePOBoxC700WestConshohockenPA194282959.UnitedStates1withwater.Neutralizethesolutio

15、nwithNH4OHthenmakeslightlyacidwithaceticacidaddingabout3mLexcess.Filteroffanyinsolubleresiduewashthoughlywithhotwater.8.3.3Unitethefiltratewashingsheattoboilingadd15mLofK2Cr2O7solution.Stirheatuntiltheyellowprecipitateas

16、sumesanangecol.LetsettlefilteronaweighedGoochcrucible.Washbydecantationwithhotwateruntilthewashingsarecolless.Finallytransferalltheprecipitatefromthebeakertothecruciblewashwithethylalcohol(95%).Dryat10562C(22064F)f1h.Coo

17、linadesiccatweighasPbCrO4.8.4Calculation:PbO%5~P30.691S!3100where:P=PbCrO4precipitategS=specimeng0.691=PbOPbCrO4=223.19?323.18.9.MoistureOtherVolatileMatter9.1Procedure—DeterminemoistureothervolatilematterinaccdancewithM

18、ethodAofTestMethodsD280.10.CarbonDioxide(EvolutionMethod)10.1Apparatus—KnrtypeofCO2evolutionapparatuswithpingfunnelcondensersuitablepurifyingtrain.NOTE3—AdeionofasuitablepurifyingtrainisfoundintheCarbonDioxideStardMethod

19、sectionofTestMethodsC25.10.2Reagent:10.2.1NitricAcid(119).10.3Procedure—Transferabout2gofthesampleweighedto10mgtoacleandryevolutionflask.ConnecttheevolutionflasktotheabsptiontrainwhichpreviouslyhasbeenflushedfreeofanyCO2

20、add100mLofHNO3(119)throughaseparatyfunnel.WhenalloftheHNO3hasbeenintroducedintotheflaskclosethestopcockfromtheseparatyfunnel.Heatthesolutionintheflasktogentleboilingboilf5min.TurnofftheheataspirateCO2freeairthroughthesys

21、temf20min.Removetheabsbingtubefromthesystemsealcoolinadesiccatweigh.TheincreaseinweightisCO2.10.4Calculation—Calculatethepercentofcarbondioxideasfollows:CO2%5~C1S1!3100where:C1=CO2gS1=specimeng.11.CarbonDioxideCombinedWa

22、ter(CombustionMethod)11.1Apparatus—CombustionTrainconsistingofthefollowingpartsconnectedinthederspecifiedtankofpurifiedcompressednitrogenpurifyingjarsincludingaCO2absptionjardryingtubecombustiontubetubefurnaceprovidedwit

23、hsuitablecontrolstomaintainthetemperaturefrom450to550C(840to1020F)absptionbulbfwateranabsptionbulbfCO2.11.2Procedure:11.2.1Heatthefurnacewithoutthecombustiontubefrom450to550C(840to1022F).Connectthecombustiontubebesidethe

24、furnaceconnecttheabsptiontubestothenitrogensupplypassaslowstreamofnitrogen(about30mLmin)throughthemtoclearoutanyresidualmoistureCO2.Accuratelyweightheabsptionbulbsreconnecttheminthetrain.Transfer1gofthespecimenweighedto1

25、0mgtoacombustionboatthathasbeenpreviouslyignitedcooled.11.2.2Withthenitrogenstillflowingdisconnectthetrainplacetheboatcontainingthespecimeninthedleofthetubewiththeaidofahookedwire.Flushthecombustiontubethoughlywithnitrog

26、enreconnectwiththetrain.Placethetubeinthefurnace.11.2.3Continuethecombustionf30minuntilthewaterthatcondensesintheinletarmofthefirstabsptionbulbhasbeencompletelysweptintothebulb.Disconnecttheabsptionbulbsfromthecombustion

27、tubeafterclosingallstopcocksplaceinadesiccattocoolthenweigh.11.3Calculation:Carbondioxide%51003C1Combinedwater%5100W12MCombinedwaterasPb~OH!2%5~100W12M!313.39where:C1=CO2gW1=totalwatergM=freemoisture%13.39=Pb(OH)2H2O=241

28、.20?18.015.12.LeadCarbonate12.1Calculation—CalculatethepercentofPbCO3fromtheCO2contentasfollows:PbCO3%5C136.071S23100where:C1=CO2(10.411.3)gS2=specimenweightusedintheCO2determinationg6.071=PbCO3CO2=267.20?44.01.13.TotalM

29、atterInsolubleinAceticAcid13.1Apparatus—GoochCruciblepreparedweighedpritouse.13.2Reagent—AceticAcid(32).13.3Procedure—Transfer10gofthesampleweighedto10mgtoa250mLbeakeradd40mLofaceticacid(23).Heatuntilsolutioniscompletefi