1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS ISO 12965:2000 ICS 83.
2、060 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Butadiene rubber Determination of microstructure by infra-red spectrometryThis British Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was published under the authority
3、of the Standards Committee and comes into effect on 15 December 2000 BSI 12-2000 ISBN 0 580 36736 3 BS ISO 12965:2000 Amendments issued since publication Amd. No. Date Comments National foreword This British Standard reproduces verbatim ISO 12965:2000 and implements it as the UK national standard. T
4、he UK participation in its preparation was entrusted to Technical Committee PRI/23, Chemical test methods for rubber, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals f
5、or change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement internationa
6、l or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include all
7、 the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. Summary of pages This document comprises a front cover, an inside front cover, the ISO titl
8、e page, pages ii to iv, pages 1 to 7 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued.Referencenumber ISO12965:2000(E) INTERNATIONAL STANDARD ISO 12965 Firstedition 2000-09-15 ButadienerubberDeterminationof microstructurebyinfra-redspe
9、ctrometry CaoutchoucbutadineDterminationdelamicrostructurepar spectromtrieinfrarougeISO12965:2000(E) ii ISO12965:2000(E)iii Contents Page Foreword.iv 1 Scope1 2 Normativereferences1 3 Principle1 4 Reagent.1 5 Apparatus.1 6 Sampling.2 7 Procedure.2 8 Precision.5 9 Testreport7ISO12965:2000(E) iv Forew
10、ord ISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISO memberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnical committees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhas theri
11、ghttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnon-governmental,in liaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnical Commission(IEC)onallmattersofelectrotechnicalstandardization. InternationalStandardsaredraftedinaccordancewi
12、ththerulesgivenintheISO/IECDirectives,Part3. DraftInternationalStandardsadoptedbythetechnicalcommitteesarecirculatedtothememberbodiesforvoting. PublicationasanInternationalStandardrequiresapprovalbyatleast75%ofthememberbodiescastingavote. AttentionisdrawntothepossibilitythatsomeoftheelementsofthisIn
13、ternationalStandardmaybethesubjectof patentrights.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights. InternationalStandardISO12965waspreparedbyTechnicalCommitteeISO/TC45,Rubberandrubberproducts, SubcommitteeSC2,Testingandanalyses.INTERNATIONALSTANDARD ISO12965:2000(E)1 Butadienerubb
14、erDeterminationofmicrostructurebyinfra-red spectrometry WARNINGPersonsusingthisInternationalStandardshouldbefamiliarwithnormallaboratorypractice. Thisstandarddoesnotpurporttoaddressallofthesafetyproblems,ifany,associatedwithitsuse.Itis theresponsibilityoftheusertoestablishappropriatesafetyandhealthp
15、racticesandtoensurecompliance withanynationalregulatoryconditions. 1 Scope ThisInternationalStandardspecifiesamethodforthedeterminationofthemicrostructureofbutadienerubber(BR) byinfra-redspectrometryusingacastfilm. 2 Normativereferences Thefollowingnormativedocumentscontainprovisionswhich,throughref
16、erenceinthistext,constituteprovisionsof thisInternationalStandard.Fordatedreferences,subsequentamendmentsto,orrevisionsof,anyofthese publicationsdonotapply.However,partiestoagreementsbasedonthisInternationalStandardareencouragedto investigatethepossibilityofapplyingthemostrecenteditionsofthenormativ
17、edocumentsindicatedbelow.For undatedreferences,thelatesteditionofthenormativedocumentreferredtoapplies.MembersofISOandIEC maintainregistersofcurrentlyvalidInternationalStandards. ISO1407:1992,RubberDeterminationofsolventextract. ISO1795:2000,Rubber,rawnaturalandrawsyntheticSamplingandfurtherpreparat
18、iveprocedures. ISO/TR9272:1986,RubberandrubberproductsDeterminationofprecisionfortestmethodstandards. 3Principle 3.1 Asmallquantityofextractedrubberisdissolvedinmethylenechlorideandcastonasaltplate. 3.2 Aspectrumisobtainedovertherange2000cm 1 to600cm 1 .Fromtheabsorbancesatfixedwavelengths, thecis,t
19、ransandvinylcontentsarecalculated. 4 Reagent 4.1 Methylenechloride. 5 Apparatus 5.1 Double-beaminfraredspectrophotometerorFourier-transforminfra-red(FTIR)spectrophotometer, with2cm 1 resolution.Theinstrumentshallbecapableofscaleexpansionalongtheabsorbanceortransmittance axisoverthespectralregionof20
20、00cm 1 to600cm 1 .ISO12965:2000(E) 2 5.2 Saltplate. 5.3 Balance,weighingto0,1mg. 5.4 Vacuumoven,operatingat50Cto60C. 6 Sampling SampletherawrubberinaccordancewithISO1795. 7 Procedure 7.1 Millthetestsampletoasthinasheetaspossible.ExtracttherubberinaccordancewithISO1407using ethanol/tolueneazeotrope(E
21、TA).Drytheextractedrubberundervacuumintheovenat50Cto60C. 7.2 Takeapproximately100mgofextractedsampleanddissolveitinaround20mlofmethylenechloride.Ifgel ispresent,filterthesolution. 7.3 Ensurethatthesaltplateislevelledhorizontallybeforethefilmiscast.Place3or4dropsofthesolutionon theplateandspreadevenl
22、yoverthebeamarea.Allowthesolventtoevaporate,preferablyatroomtemperature. 7.4 Checkthatthetransmittanceoverthemeasurementrangeliesbetween50%and30%.Ifgrosslyoutside theselimits,cleanthesaltplateandrepeatstep7.3withmoreorlesssolution. 7.5 When7.4issatisfied,scanovertherange2000cm 1 to600cm 1 . 7.6 Draw
23、abaselinefrom2000cm 1 to600cm 1 ,takingcarethatnopeaksarecut(seeFigures1,2and3for medium-,low-andhigh-cispolybutadiene). 7.7 Measuretheabsorbancesat965cm 1 (A 965 ),909cm 1 (A 909 )and728cm 1 (A 728 ).Theseareanindication ofthetrans(A 965 ),vinyl(A 909 )andcis(A 728 )contents. 7.8 Normalizetheabovea
24、bsorbancesusingthefollowingequations: 965 965 965 909 728 % 100 A A AAA 909 909 965 909 728 % 100 A A AAA 728 728 965 909 728 % 100 A A AAA 7.9 Calculatethecontentsofthedifferentisomers,c cis ,c trans andc vinyl ,ing/dm 3 ,usingthefollowingequations: 728 965 909 1,7896 % 0,0253 % 0,0085 %cAAA cis 96
25、5 728 909 0,3971% 0,0502 % 0,0142 %cAAA trans vinyl 909 728 965 0,2954 % 0,0075 % 0,0065 %cAAAISO12965:2000(E)3 7.10Determinethemicrostructureoftherubber,inpercent,usingthefollowingequations: vinyl 100 % c ccc cis cis cis trans vinyl 100 % c ccc trans trans cis trans vinyl vinyl vinyl 100 % c ccc ci
26、s trans Figure1SampleA(medium-cispolybutadiene)ISO12965:2000(E) 4 Figure2SampleB(high-cispolybutadiene) Figure3SampleC(low-cispolybutadiene)ISO12965:2000(E)5 8 Precision 8.1 Theprecisioncalculationstoexpressrepeatabilityandreproducibilitywereperformedinaccordancewith ISO/TR9272.Consultthisforprecisi
27、onconceptsandnomenclature. 8.2 Atype1interlaboratorytestprogrammewasorganizedin1994.Threepolybutadienematerials(A,BandC) withdifferentmicrostructures(seeFigures1,2and3)weresenttotheparticipatinglaboratorieswheretheywere analysedusingthetestprocedure. 8.3 Theprecisionresultsfortheciscontentaregivenin
28、Table1,theprecisionresultsforthetranscontentare giveninTable2,whileTable3showstheprecisionresultsforthevinylcontent. Foralldata,p=6,q=3andn=5. 8.4 Repeatabilityforciscontent:Therepeatabilityrfortheciscontentofpolybutadienehasbeenestablished as1,00percentagepoints.Twosingletestresults(ordetermination
29、s)thatdifferbymorethan1,00percentage pointsshallbeconsideredsuspectanddictatethatsomeappropriateinvestigativeactionbetaken. 8.5 Reproducibilityforciscontent:ThereproducibilityRfortheciscontentofpolybutadienehasbeen establishedas1,86percentagepoints.Twosingletestresults(ordeterminations),obtainedinse
30、parate laboratories,thatdifferbymorethan1,86percentagepointsshallbeconsideredsuspectanddictatethatsome appropriateinvestigativeactionbetaken. 8.6 Repeatabilityfortranscontent:Therepeatabilityrforthetranscontentofpolybutadienehasbeen establishedas0,72percentagepoints.Twosingletestresults(ordeterminat
31、ions)thatdifferbymorethan 0,72percentagepointsshallbeconsideredsuspectanddictatethatsomeappropriateinvestigativeactionbe taken. 8.7 Reproducibilityfortranscontent:ThereproducibilityRforthetranscontentofpolybutadienehasbeen establishedas0,94percentagepoints.Twosingletestresults(ordeterminations),obta
32、inedinseparate laboratories,thatdifferbymorethan0,94percentagepointsshallbeconsideredsuspectanddictatethatsome appropriateinvestigativeactionbetaken. 8.8 Repeatabilityforvinylcontent:Therepeatabilityrforthevinylcontentofpolybutadienehasbeen establishedas0,30percentagepoints.Twosingletestresults(orde
33、terminations)thatdifferbymorethan 0,30percentagepointsshallbeconsideredsuspectanddictatethatsomeappropriateinvestigativeactionbe taken. 8.9 Reproducibilityforvinylcontent:ThereproducibilityRforthevinylcontentofpolybutadienehasbeen establishedas0,64percentagepoints.Twosingletestresults(ordeterminatio
34、ns),obtainedinseparate laboratories,thatdifferbymorethan0,64percentagepointsshallbeconsideredsuspectanddictatethatsome appropriateinvestigativeactionbetaken.ISO12965:2000(E) 6 Table1Precisiondataforciscontent Meanlevel Withinlab Betweenlabs Sample % s r rr% s R RR% A 93,48 0,33 0,91 0,97 0,46 1,28 1
35、,37 B 97,52 0,22 0,61 0,63 0,84 2,33 2,39 C 39,94 0,49 1,36 3,41 0,66 1,83 4,58 Pooledoraveragevalues 76,98 0,36 1,00 1,30 0,67 1,86 2,42 where s r isthewithin-labstandarddeviation; s R isthebetween-labsstandarddeviation; r istherepeatabilityinmeasurementunits; r% istherepeatabilityinpercent; a R is
36、thereproducibilityinmeasurementsunits; R% isthereproducibilityinpercent. a a Thesevaluesrepresentpercentrelative,i.e.percentofapercent. Table2Precisiondatafortranscontent Meanlevel Withinlab Betweenlabs Sample % s r rr% s R RR% A 3,5 0,13 0,36 10,3 0,22 0,61 17,4 B 1,86 0,16 0,44 23,7 0,35 0,97 52,1
37、 C 50,2 0,4 1,11 2,21 0,42 1,16 2,31 Pooledoraveragevalues 18,52 0,26 0,72 3,89 0,34 0,94 5,08 where s r isthewithin-labstandarddeviation; s R isthebetween-labsstandarddeviation; r istherepeatabilityinmeasurementunits; r% istherepeatabilityinpercent; a R isthereproducibilityinmeasurementsunits; R% i
38、sthereproducibilityinpercent. a a Thesevaluesrepresentpercentrelative,i.e.percentofapercent.ISO12965:2000(E)7 Table3Precisiondataforvinylcontent Meanlevel Withinlab Betweenlabs Sample % s r rr% s R RR% A 3,05 0,10 0,28 9,18 0,31 0,86 28,2 B 0,35 0,11 0,30 85,7 0,19 0,53 151,4 C 9,62 0,13 0,36 3,74 0
39、,17 0,47 4,89 Pooledoraveragevalues 4,34 0,11 0,30 6,91 0,23 0,64 14,75 where s r isthewithin-labstandarddeviation; s R isthebetween-labsstandarddeviation; r istherepeatabilityinmeasurementunits; r% istherepeatabilityinpercent; a R isthereproducibilityinmeasurementsunits; R% isthereproducibilityinpe
40、rcent. a a Thesevaluesrepresentpercentrelative,i.e.percentofapercent. 9 Testreport Thetestreportshallincludethefollowinginformation: a) areferencetothisInternationalStandard; b) fullidentificationoftherubberanalysed; c) whetheranygelwaspresent(see7.2); d) theresultsoftheanalysis; e) detailsofanydevi
41、ationsfromthemethodspecified; f) thedateofthetest.BS ISO 12965:2000 BSI 389 Chiswick High Road London W4 4AL | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | |
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