D橡膠品的化學(xué)測(cè)試

1、DesignatioB):297-93(Reapproved002)StandarTesMethodforRubbeProductsChemicAnalyslsThisstandasdssueuhderhe?xeddesignatO297thenumbenmediatfelyowinthedesignationicateseyeaoforiginsaldoptionjnthecasefrevisiothieyeaoflastevisioA.numbinrparentheinelicatthBsyeaoflasteapproAal.superscepsilon)indicataseditoric

2、hangencehelasrevisioorreapproval.ThisetandOnaSoeeapproviedfus(byagencieStheDepartmenDefense.eNoTSecti03s.,5.1.5,.5,7.7.an(X2.4.1Wer(editoriaiupdatedJanuary2003.Sections11-1314and1516 17-26 27-33 34-4041-5152-581. Scope1.1 Thesfesstmethoacoverhequalitativeidquantita-tiveanalyso

3、sthecompositofmubberroducosthe"R"famiiyseeL1)Manofthestesmethodsay)eapplieotheanalysofnatursandsyntheticudeubbers.1.1.1 PartAconsisofgeneraesmethodsrusenthedeterminatiofrsomeorallofthemajoiconstitueotsarubbeproduct.1.1.2 PartBcoveithedeterminatofispecicpolymerspreseintarubbeproduct.1.1.3 r

4、hetestnetho(as)peamthefollowinorder:PartA.GeneraTesMethods:RubbeP01ymeConterbythelndiredMethodDeterminatiomdReporortheGeneraMethodDensityExtraoAnalysisSulfuAnalysisFillerAnalysisAshAnalysisPariB.DeterminatiofRubbePolymers1.2 ThevaluestatednSIunitsaretoberegardedsstandarTheinch-poununitsgiveninparent

5、hesesforinformationly.1.3 ThisstandardoejnotpurportoaddresslofthesafetyDroblemif,any,associatedithitsuse.ltistheresponsibiotyheuseofthisstandatoestablisippro-priatesafetylndhea1tlpracticesrddetermirl®eapp1ica-bilityofregulatormitatiorpriortouse.Specicprecau-tionary>tatemeat®givenin31.4.

6、531.6,.2,45.1.34.4.2vnc56.5.3;ncX1.3.ancX.2. ReferencDocuments2.1ASTMStandards:D982TestMethoforOrganiNitrogennPapeand2Paperboard1 ThestesmethodsreundehejurisdictioniASTMDommittDe1onRubberndarethedirecresponsibiotySubcommiDd0.1onChemicalAnalysis.CurreneditioapprovDtec.10,2002

7、Publishednua2)003Originallyapprovirdl1928_asprevioleditiompprovind199sD297-93(1998).2 Discontinuse；982nnuBooOfASTIStandarPal20.D1416TesMethodorRubberomSyntheSourcesChemicanalysisD1418PracticeforRubberandRubberLatticesNomenclatureD1646TesMethocforRubbeViscositStresRelax-atioran(Pre-Vu1canizCtharacter

8、iSMBoneys-cometer)D3156PracticerRubbeChromatographaysofAntidegradanrtsoxidanAntiozonanisdStabiliz-ersD3452PracticforRubberden?icationbyPyrolysis-GaChromatographyD3677TesMetho<dorRubberden?ication)ylnfra-redSpectrophotometryD4483Practi(cerDeterminiPrecisiooirTesMethodStandardstheRubberncCarboBlack

9、ndustrtesE11SpecicationorWire-ClothievesorTestinPur-posesE131TerminolcRelatintoMoleculSpectroscopyE200PracticforPreparati0ntandardizaOInd,Stor-ageofStandardndReagerSolutionsorChemicalAnalysisE422TestMethodorMeasurinlgeatFluxUsingaWater-CooCadorimgterE443TesMethodorSulfurnOrganiCompounbsOxygeFilasCom

10、bus6ion3. Terminology3.1 DePnitionsThenomenclatainelabbreviatiasedfornaturaandsyntheticubberareinaccordanwethPracti1418.4. Reagents4.1 PurityfReagenReagegradehemicasallbeusednalltestsUn1esstherwiigdicateidisintendedat3AgguBooOfASTIStagdarde109.01.4AgguBooOfASTIStagdards114.02.5AgguBooOfASTIStagdarde

11、103.06.6AgguBooOfASTIStagdarde115.05.7AgguBooOfASTIStagdarde115.03.Copyrig?ltASThgtematiog1-)0BarlHarbODrivepOBoXC7OOW/esCogshohoelPA1,9428-29U91iteStates.1.061.421.701.840.90allreagenStSalConfontothespeCicationsftheCommit-teeorAnalyticReagenOStheAmericanhemicSiOciety,whersuchspeCication

12、sreavaila由Othegrademay)eusedprovidedtis?rstascertainthatthereagensofsufficientiyghpurittopermiittsusewithoulfessenittgeaccuracythedetermination.4.2PurityofWaterUnlesstherwisedicatere,ferencestowaterhalbeunderstotocheadistilleWateorwateofequapurity.5. ConcentratiofiReagents5.1 ConcentraAcdandAmmoniui

13、lydroxidW/henacidsandammoniunydroxiderespeCiedbynameorchemicaormulaonly,itisunderstoddatconcentratedreagentsfthefollowingdensitieorconcentratioarsintended:Density,Mg/m/ceticacid,HGHC2(99.7%)FormiacidHCOOHHydrochloaicidHClHyd?)uori(acidHF(49%)NtricacidHNOPhosphoacidHPO(85%)Sjlfuri(acidH2SQAmmoniuhydr

14、oxideHOHThedesiretfensitieffconcentratio同0theconcen-trate(acidarestateWhenevthearespeCied.8ReageCthemicaAmericaChemicaBocietSpeccationAmericanChemicSbcieWashingDCForsuggestionsietestingfreagentetlistecbytheAmericaChemicSocietyeeAnalaStandaridsLaboratoryChemicaBDHLtd.pooleJorseU.K.andheUniteStateshar

15、macopeiaandNationaormulaty.SPharmaceiCicaventionlUSPGRockville,MD.5.2 DilutedAcidsandAmmoniumHydroxideConcentrationsCilutecacidsandammoniutTydroxide,excepwhenstandardiza3dspeciedasaratiostatinthenumbofvolumeftheconcentrareagenObeaddetOagivennumbeofvolumesfwaterasinthefollowingexamplHCl(1+9)meansvolu

16、mofconcentrated(density.19mixedwith9volumefwateAcidsshalbeaddetowateslowlywithstirring.5.35 tandaSolutionConcentrationstandasolu-tionsreexpressasnormalitiesasvolumofsolutiothatreactwithorcontairasgivennassfmateribleingjseordetermineorexample：1NNaS>O3solutionsCuSO3solutioncm=0.00gCu).5.36 Nonstand

17、ardiZedutioniConcentratioofsnon-StandardizsBC：lutionseparelydissolvilaggivennasSlasolveratrespeciedingramofthereagenasweighted3out)/dmofsolutionanditisunderstothdatwatersthesolveninlesotherwiseDecied,forexamplNaOH(10g/dmimeans。gofNaOFdissolvedwateanddiluted3wthwateto1dm(Note).Inthecasefcertaneagerth

18、3sconcentratmaybespeciedasapercentabyemasspr&ample:thano50%)meanessolutiocontaining)gofethan(per100gofsolutioiOthenonstandardsoedtionsmaybespeciedbynamonlyandtheconcentrationuchsolutionwillbegovernedttheinstructiofiostheiiprepa-ration.Ndte1Whenevarhydrateslaltisusednthepreparatioonareagenforexam

19、plB,aC22HO)thepreparationthereagensdescribeddetaiWheiananhydrcsustisusedhprepariiagjimpleaqueosolutionhereagenslistedbytitleonlyanddetailofthepreparatarenotgiven.PARAGENERALESTMETHODS6. ScopandApplication6.1Thejenertesmethodtescribedveheanalysosmanyypesfrubbeproductodetermirnheamounindtypeofnonrubbs

20、onstitueatstocalculailndirectiyomthesdatetheamoundfrubbeconstituent.6.2Theapplicatio8rndllimitatiolcfthetestmethodoanalysOfspe?ictypeofrubberroducasregiveriinthescopesfthevariousestmethodApplicatiototypesofrubbeproductsotspeciedinthescopofaparticulfesstmethodhalbeve?edbyapplicatitoiacontroofknownand

21、similacomposition.6.3SpeciaiestmethocforanalysBsregiverforrubberproduccontaininguefreecarboantimoneadmineraloil,waxynydrocarbcansbariuraarbonate.6.4Fo4hedeterminatooheamouofarubberolymerpreserrtarubbsJ,roductnindire(testneth(CSIgivebywhichthenonrubbernstitueatsdetermineidlividuallyoringroupsi1ndheru

22、bberolymerontensdetermineddifferencSections-13)f,inusinthistesmetho?,llersaredeterminbyltheashingpstnethoCBectiOn50r36),satisfactorysultwillbeobtaineexcepwhereherearefounctobepresendecomposaOlmpoundingredientssuchascarbona1thatdecompoSlej5c,clayasbestos,asbestintajc,hydratedilica,antimonyu?de,haloge

23、n-containicgmponeatssiliconeolymeNotesmethodof?llerdeterminatiOereindescribewillgiveaccurateresultsth中resencfelayasbestosicatalcorany?therhydratedllerunlesscorrectioanbemadeorlossesfwateofhydratioaashinThis:orrecticarbenadenlyifthenatureandquantityofthese?llersareknownTheindirectestmethodvillnotgive

24、accurateesultsnthepresenofhalogen-contailoirmDoneortsiliconleJbber.Inthepresenofantimosy?deorcarbonadecomposingat550C:butintheabsenoetheabovinterfering)nstitu-entsapproximatorrectioanbemadbymeanofdeter-minatiooftotalantimonySectior50)orofthemetalassociatedhthedecomposcbrbonausualcalcium,Sectio45)or(

25、Sectio49)andcalculatiooftheoriginalcompositOfnthecompoundingredienrOmtheseata.6.5Iffacticeorhighpercentagifsminerailubbearepreserr0accuratestnethoiSknowrordetermina00nrubberonteorforcompleanalysiistherubbeproduct.6.6ForthedeterminatiofhtherubbecontenOfhardrubbeproductsoaccuratesmethOddescribedreif?l

26、lersdecomposabie5(Carepresent.7. BlankDeterminations7.1 Blankshalberunonalldeterminationshecthepurityofthematerialssedanddeductionsallbemadeaccordingly.8. ChecAnalyses8.1 DuplicadeterminatishnsbemadancshalcheckwithinthelimitsspeciedinthetestmethoWhenhesarestated.9. PreparatioonSamples9.1 Beforprepar

27、iasampforanalystheanalyshall,byinspectiGassuhemselhatthasiotbeenontaminated.ThesampltebeanalyzedialbeselectedytakingpiecesfromvarioupartoftheoriginasampandseparatinhemfromforeigmatteBecausethevarietofrubberroductstowhicrthistestmetho(dahbeapplie(h,osingle)rocedureforreducingesamptotherequirednenessa

28、pplicabeallsampleiherefosseverallternativeocedufesthispurposeredescribedZogiTheanalyssexpectedselecheonemosSuitabtethesampllhaheisanalyzingandtheequipmenVailable.9.2 Forvulcanizsoftrubbeunvulcanizebbecruderubbeandmanyamplefreclaimdbbetjspreferabletomixthesampan(grindtbypassirigtwoorthreeimesthroughc

29、learcoldlaboratorybbeinill.Therubbewillcomeromthemillintheformofacoarspowderraroughsheelf.theproductintheermGfasheetheadjustmentthemillshalbesuclthatthelhickneoSthe?nalsheesnogreatethanD.5mmIfthesamplisstickyitshalberolledinalinermateriahaWillnotadheiteorcontaminattiesamplf.themilledampleapowdershal

30、betransferredtoaNo.14(l/D-mmeveandrubbetihrougthesieve.Grindingshallbecontinuedntiltheentiresamplpassesthrougthesieve.9.3 IntheabsenoemillingmachineryesampmayDepreparejycuttingwithscissossthattwillpasaNo.141D-(1.4D-mlSieveThesampmay)eculintelong>tripShatare?neenouglepasSreelyhrouglhesievenclhestr

31、ipsfedthrougbyhandorthesamplmaybecutintosmallfragmerahdshakelhrougthesievehecuttincshalbecontinueditiltheentire>amplpassesrougthesieveIfnecessaoprevesticking,ffererrtagmeeslhesievedsampmayDesegregabywrappingalinematerithatwillnotadheiteorcontamintrtesample.9.4 CertaiiveryglutinousampleBaybeprepar

32、eforextracticamalysassfollowsPlacaweighed-gsampofthemateribetwedwepiecQsfashleSSlterpapelhatasbeenextractenaccordanwehSectio21.Thepapers9.5 Detaileelquirementtheseiev的egivennSpecicatioE11.9.6 Acompreevel:Umeeheimtlealmeetheeequiremehae/ailablefromC.W.Brabehdletrumehfrc.5DE.Weeldjyt.,SoutHackehea>

33、ck,07606.shouldeapproximatjfl'Dby1DDmm(2Dby4in.)andhesamp曲ouldeplaceheaoneendFlattethesampahdspreatthroughohelengto代he?代erpaperypassinge“sandvl(HrtgthWiSerougacoldcloseleeteven-speedrubbecalenderhegrossthicknesftheresultingheetshouldotbegreatehanl.Dmm.Ifarubberalendernotavailable,similarsheemayb

34、eobtainedyplacinghesamplinahydraulpresoraviseJnthelattecasethesampmayeroughlypreaoyhandhrougheUtelengthofthe?代erpapeanqpressuapplietosmaareaatatimeuntilthewholsamphasoee?attened.9.7 Samplesrubberizelothwhoseverathicknessnogreaterhan1.0mm,maybeprepareoranalysisycuttinthennntepiece1s.5mmequaahdlhennix

35、ingvell.Ifthefabriiseasilysmovedshoulbeseparatedlesananalysiofthewholelothisdesired.9.65 amplesfrubbeicementshallbeevaporateddrynesnavacuumvenatatemperathe-lhigherhan3DC.TheesidumaNhenbeanalyzeeanunvulcanizedsamplAseparasamplofthecemenshallbedistilledundeleducexlressUfexaminatGGthesolveredesired.9.7

36、Samploehardubberhabereducdepowddormby?lingcleanedithamagneindsievethrouca)No.3D10(500-71Lsieve.ResiduEetaineonthissieveshallbereducedltiltheentire,ampl|easseerougthesieve.10. PreliminaryxaminatiojfSamples10.65.1 Theprocedureiverin1D.1.1-1D.ar9foruseindeterminingenumbeandkindofteststhatshouldbeconduc

37、tedobtairthedesiredlformatioencernihgerubberroduct.1D.1.CarbonaldSropasmalpieceofsamplintoatestubecontainilhCeaturatwiihbromind.astreaefbubblesgivenoff,carbonatarepresenT.hetestisnotapplicabtelIRproducts.1D.1.2ntimolahdLeadAshaD.2loD.3-cspecimeh3accordanweth35.4or36.4Dissolvtheashn10cmof3HClbyheatin

38、g).iluteoabol40cmanddecaer?ltertheeolutiorfromtheresidue?asSHSintothesolutiorlfared-oran|grecipita:OrmeantimorrypreseahdmayedetermineldarubberpecimehaccordahcehSection50.OrganeulfushalbedetermiriedlCCordarCeh27.3.3Dlutewithwatetoabou400cmandagaipasmH2S.Ifablaclprecipitaaippearleadispreseandorganisnd

39、inorganeulfuehalbedeterminihdaccordarwdh28.3and.3 CarboiBlackHeataportioofthesampwithHNOuntitheresnomorerothingftheliquidsblackitindicatdSepreseneecarbohlackTheteslisnotappli-cableollRproducts.10.1.43 ariunSaltefthesampcentainerbonaaehasmaspecimehgeeheashndiluteHClcooland?lter.Addafewdropso

40、fdiluteH2SOtothe?ltrateAwhiteprecipitatesolubleexcesHClindicatesepresenceacid-solubariunsaltsThepresenoeacid-solublariumsaltsrequirethatorganisulfuishallbedeterminbylthefusionnethe(Sectieh2).RubberAdDerisitMg/mNR94/970.940.9AIR1.001.000.95sbR1.000.920.94BR1.001.000.90IIR1.001.000.92"raodL.A.,va

41、loeshysicConstai osRubbeiRubberrhemisandTABLE FactorSorCalculationsTechnologyol.12,1939p. 130.BWakeWV.C., <<TIAelalys(sfRubb6andRubbet-LPelymetSMaCLaten andSonsLtd.LondorEngland958Pp.42 to45.CContainin23.5% bcunstyten®ncnctcil-extended.10.1.44 axyHydrocart)otfswaxyhydrocarbonsepresentheyw

42、illsolidifyit-5Cintheacetoredractsawhite?occuleptecipitacengintpthesideofthe?ask.10.1.45 lueExtractportionfthesampleithamixturecf32%acetonand68%chloroforbyvolumeor8hinaccordancehSectionlDrythespecimanGtligesorlhwithhotwateFiltercoolandaddafewdropofafreshly3ptepareBClutiC(nftanniClCic(20g/dm)tothe?lt

43、rateandallowtostandorafewminutesfthesolutiobecomesturbicgluespreseortcshouldedeterminasdescribieidSectionO.10.1.46 acticeDigestherubberemainifg:)mthetestforgluewithNaOFsolutionl75j/dm).Decanheliquid,dilute,andacidifywithHCl.Anycloudinessprecipitateindicatesnepresencffacticeandthealcoholipotashextrac

44、tSection2)shalbedetermined.10.1.80 therFillersAnHCl-solubleshindicatetheabsencofclay,silica,silicatestitaniumdioxidebariumsulfatendithoponenHCl-insoluashrndicattiseneedforacompleteshanalysiifcompositiontheashisrequired.10.1.81 berolymdden?icationIfaniden多cationofthetypecfrubbetolymeJtesehrtthesampie

45、desired,proceenaccordancehSection2-58.Rubbbyvolum%5GEF(4)where:A=factoristednTable,B=sumofpercentagjesotaextracalcoholpotashextractcombinedulfur,inorgani?llers,carbonblackandglueasdeterminedaccordanwethSecti02s(or19anc20)22,2822i4.138(TestMethoA)or39(TesMethoB),and40.C=rubbepolyme%D=factorstednTable

46、,E=densitofprodu(atsdeterminind16.1,F=densitofrubbelrstednTable,andG=rubbeascompound%d,RUBBEROLYMERONTENTYTHEINDIRECTESTMETHOD11.ScopeDETERMINATICANDRERORTORGENERALTESTMETHOD14.DeterminationsRequired11.1Therubbecontenofaproductscalculated/subtractinhesunofthenonrubbonstituefrom100%.14.1Acompleteanal

47、ysiofarubberproductfortheacetoiesxtradbjaseonrubbGascompounded,5A/B3100purposewhere:determiningA=percentageicetorextracandqualityndtsB=percentaofeubbeascompounded.specic14.1.2SulfuBasednRubbetsCompoundlCdlculateThistestmethods applicabto NR, IR, SBR,andBRcompositionhepercentagfesulfurbaseonrubbeasco

48、mpoundaid,follows:productstcanalsobeapplied)IIRproductstheyareextractedthmethyithyketoneathethanwithacetone.requirein,additiotoSulfubasednrubbet9dompounc%d>A/B!3100rubbepolymercontent,ewhere:determina-A=percentageotasulfuandB=percentaofeubbeascompounded.tionofother14.1.3norganidillersThenorgan?dl

49、lersmayede-valuesstedntermineasaunitormaybedetermininodividualand14.1.1-14.1reporteisinItem$18to(28of.4DombustibieersCarb0nlaclncgluearethe14.1.1combustibleerswhichmaybedeterminiedividually.Acetone14.1.5dditiveAdditivesuchasfacticeotherubberExtract,substitutesdsoftenetBenotaccurate:letermin

50、TdleirBasedpresencndanestimatefthequantitiesreserrtiaybeon(6)RubberasCompoundedCalculathe12.Terminologypercentaogfeacetoneextract,baseodnrubbearscompounded,asfollows:12.1De?nitions:12.1.1 rubbeprolymetrhecharacterisatnicdmajorcom-ponenotfanaturaolrsynthetcicruderubber.12.1.2 rubberascompoundaepdprox

51、imatelqyuivalenttothenonextendruebdbeursedinthemanufactuorfearubberproducItt.differsfromtherubbeprolymebrytheamounotfnonrubbmerateriaplresenintthecruderubberF.orsyntheticrubbertshequantityvarieswiththetypeofrubbearndthemanufactuarenrdnode?nitepercentacgaenbegivenT.here-fore,forsynthetircubberr,ubbea

52、rscompoundsehdallbeconsiderteodbeequatlorubbeprolymeerxcepfotrSBR(seeTable1).12.1.3 rubbeprolymebryvolumethepercentabgyevol-umeofarubbeprroducotccupiebdytherubbeprolymer.12.1.4 rubbebryvolumeisthepercentabgyevolumoefarubbeprroducotccupiebdytherubbearscompounded.13.Calculation13.1 Calculatheepercenta

53、ogfersubbearsfollows:(1)Rubbeprolyme%r,5A1002B!(2)(3)Rubbearscompound%ed5,C/DRubbeprolymebryvolume%,5CE/FDetermined bySection0.9973AA2B2C!3DDensi0t25C inMg/m5(8)foundbydeterminateOacetonehloroforandalcoholicpotasextractsnsapOnEiblenattewaxyiydrocarband,mineraoil,andthesvalueshalbereportedacompletean

54、alysis.15. Report15.1 ThereportnayincludanyorallofthefollowingItemsi)to(17ifadetailedlleranalysiisnotdesirethepurposoftheanalysshadetermittenaturo代h&eport.Therepomayalsoncludenyorallofthefollowingems(18to(28ifadetailednalysofinorganicllerisdesired.(1)Acetonextraccorrected18.1and19(2)Waxyiydrocar

55、bons24(3)Mineraoil25(4)Chloroformtract18(5)Freesulfur29(6)Combinesulfur28.2.2(7)Totasulfur28.2.3(8)Fillersinorganic34.1(9)Carboblack38or39(10)Glue40(11)Rubbepolymer11-13,r52-58(12)Rubbepolymeryvolume11to13(13)Rubbeascompoundndiiuraorsyn-11to13thetic(14)Rubbetoyvolumenaturabrsynthetic11to13(15)Percen

56、tageacetonextractnrubberascompounded14.1.1(16)Percentagesulfuonrubbeascom-14.1.2pounded(17)Density16(18)Silicodioxidondnsolublmatter42(19)Silicodioxide42(20)Leacoxide43(21)Ironandaluminuioxides44(22)Calciumxide45(23)Magnesiumxide46(24)Zincoxide47(25)Bariumarbonate49(26)Bariursulfate48(27)Antimonyl?d

57、e50(28)Titaniumoxide51PercentageDENSITY16.Density16.1Determirthedensity)yuseofapycnometbyhydrostaWeighingsrbycompresvedumeensimeter.Takemeasurementtsatemperatubetwee24.5and25.5C,unlessthecoefficienfexpansiooftherubberproductknownnwhiccasmakthedeterminaaanyconvenieemperatandcorreco25C.16.2PycnomeMeethod16.2.1 Procedureeterminthedensityusingthepyc-nometwithalcohonplacefwatetoeliminatsrorduetoairbubbles.16.2.2 DalculatioCalculalfeedensitasfollows:B=masofpycnome?elrecwithspecimendalcohol,g,C=