1、 | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS ISO 11359-2:1999 ICS 8
2、3.080.01 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Plastics Thermomechanical analysis (TMA) Part 2: Determination of coefficient of linear thermal expansion and glass transition temperatureThis British Standard, having been prepared under the direction of the Sector Comm
3、ittee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 November 1999 BSI 11-1999 ISBN 0 580 35346 X BS ISO 11359-2:1999 Amendments issued since publication Amd. No. Date Comments National foreword This British Standard reproduces v
4、erbatim ISO 11359-2:1999 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics, which has the responsibility to: aid enquirers to understand the text; present to the responsible international/European c
5、ommittee any enquiries on the interpretation, or proposals for 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-r
6、eferences The British Standards which implement international 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 C
7、atalogue. A British Standard does not purport to include all 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
8、comprises a front cover, an inside front cover, the ISO title page, pages ii and iii, a blank page, pages 1 to 10, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued.A Referencenumbe r ISO113592:1999 (E) INTERNATIONA
9、L STANDARD ISO 113592 Firstedition 19991001 PlasticsThermomechanicalanalysis (TMA) Part2: Determinationofcoefficientoflinearthermal expansionandglasstransitiontemperature PlastiquesAnalysethermomcanique(TMA) Partie2:Dterminationducoefficientdedilatationthermiqueliniqueetde latempraturedetransitionvi
10、treuseISO113592:1999(E) ii Contents 1Scop e1 2Normativereference s1 3Termsanddefinition s.1 4Principl e3 5Apparatu s.3 6Testspecimen s3 7Procedur e.3 8Expressionofresult s4 9Testrepor t7 AnnexA (informative) Precisionandreproducibilitydataforthedeterminationofthemeancoefficientof linearthermalexpans
11、ionusingTM A9 Bibliography10 ISO113592:1999(E) iii Foreword ISO (the InternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISO memberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOtechnical committees.Eachmemberbodyinterestedinasub
12、jectforwhichatechnicalcommitteehasbeenestablishedhas therighttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnongovernmental,in liaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnical Commission(IEC)onallmattersofelectrotechnicalstanda
13、rdization. InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IECDirectives,Part3. DraftInternationalStandardsadoptedbythetechnicalcommitteesarecirculatedtoth ememberbodiesforvoting. PublicationasanInternationalStandardrequiresapprovalbyatleast75%ofthememberbodiescastingavote. Int
14、ernationalStandardISO113592waspreparedbyTechnicalCommitteeISO/TC61,Plastics,Subcommittee SC5, Physicalchemicalproperties. ISO11359consistsofthefollowingparts,underthegeneraltitle PlasticsThermomechanicalanalysis: Part1:Generalprinciples Part2:Determinationofcoefficientoflinearthermalexpansionandglas
15、stransitiontemperature Part3:Determinationofpenetrationtemperature AnnexAofthispartofISO11359isgivenforinformationonly.INTERNATIONALSTANDARD ISO113592:1999(E) 1 PlasticsThermomechanicalanalysis(TMA) Part2: Determinationofcoefficientoflinearthermalexpansionandglass transitiontemperature 1Scope Thispa
16、rtofISO 11359specifiesatestmethod,usingthermodilatometry,forthedeterminationofthecoefficientof linearthermalexpansionofplasticsinasolidstatebythermomechanicalanalysis(TMA).ThispartofISO 11359 alsospecifiesthedeterminationoftheglasstransitiontemperatureusingTMA. NOTE Thecoefficientoflinearther malexp
17、ansioncanbe measuredusingvarioustypesofthermodilatometryapparatus. ThispartofISO11359concernsonlyTMAapparatus. 2Normativereferences The following normative documents contain provisions which,throughreferenceinthistext,constituteprovisionsofthis part of ISO 11359.F or datedr eferences,s ubsequentamen
18、dmentsto,orrevisionsof,anyofthes e publications do not apply.However,partiestoagreements based on this part of ISO 11359 are encouragedtoinvestigatethepossibilityof applyingthemostrecenteditionsofthenormativedocumentsindicatedbelow.Forundatedreferences,thelatest editionofthenormativedocumentreferred
19、toapplies.MembersofISOandIECmaintainregistersofcurrentlyvalid InternationalStandards. ISO291, PlasticsStandardatmospheresforconditioningandtesting. ISO113591, PlasticsThermomechanicalanalysis(TMA)Part1:Generalprinciples. 3Termsanddefinitions ForthepurposesofthispartofISO11359,thetermsanddefinitionsg
20、iveninISO113591apply,plusthefollowing: 3.1 thermalexpansion increaseindimensionsofaspecimenasafunctionoftemperature,measuredbythermodilatometry 3.2 coefficientoflinearthermalexpansion reversibleincreaseinlengthofamaterialperunitlengthperdegreechangeintemperature NOTE Twodifferentcoefficientsoftherma
21、lexpansioncanbedetermined:thedifferentialcoefficientoflinearthermal expansionandthemeancoefficientoflinearthermalexpansion.ISO113592:1999(E) 2 3.2.1 differentialcoefficientoflinearthermalexpansion a coefficientofexpansionforanyofthethreedimensionsa ttemperatureTandatconstantpressure pgiven,in recipr
22、ocalkelvins,bythefollowingequation: a= (d) (d) 1 (d d) (d d) 1 00 L TL Lt TtL p p p p / / (1) where L 0 isthereferencelengthatroomtemperature T 0 ,intheaxisofmeasurement; L isthelengthattemperature T,intheaxisofmeasurement; dL isthechangeinlengthoverthetimeintervald tatconstantpressure p; dT isthech
23、angeintemperatureoverthetimeintervald tatconstantpressure p. 3.2.2 meancoefficientoflinearthermalexpansion a coefficientofexpansionforanyofthethreedimensionsatconstantpressure,given,inreciprocalkelvins,bythe followingequation: a= D D L TL 1 0 (2) where D L isthechangeinlengthofthetestspecimenbetween
24、twotemperatures T 1 and T 2 ; L 0 isthereferencelengthofthetestspecimenatroomtemperatureintheaxisofmeasurement; D T isthechangeintemperature,equalto T 2 - T 1 . Thedeterminationismadeoveratemperatur eintervalD Tbetween T 1 and T 2 .Therepresentativetemperatureis givenby T TT (representative) 2 12 =
25、 NOTE Byreplacingtheterm“length”by“volume”inequations(1)and(2),thecoefficientofvolumetricthermalexpansion canbeobtained. 3.3 glasstransition reversiblechangeinanamorphouspolymerorintheamorphousregionso fapartiallycrystallinepolymerfrom(or to)aviscousorrubberystateto(orfrom)ahardandrelativelybrittle
26、one 3.4 glasstransitiontemperature T g approximatemidpointofthetemperaturerangeoverwhichtheglasstransitiontakesplace Theglasstransitiontemperatureobtainedbythermodilatometryisdefinedasthepointofintersectionofthe tangentstothelengthversustemperaturecurvebeforeandaftertheglasstransition(seeFigure3). I
27、SO113592:1999(E) 3 4Principle ThechangeinadimensionofatestspecimenismeasuredasafunctionoftemperatureusingaTMAapparatusto generateaTMAcurvefromwhichthecoefficientoflinearthermalexpansioncanbecalculated. 5Apparatus ThecomponentsoftheTMAapparatususedforthisparto fISO 11359shallbeasspecifiedinISO 113591
28、and shallalsobecapableof: a) operatinginacompressionmodeoratensionmodeorboth; b) maintainingthespecimenunderacontrolledatmosphereinaccordancewithISO291. NOTE1 Measurementsonspecimensoffilmorfibrearemadeinthetensionmode. NOTE2 Itispreferabletouseanatmosphereofdryairoraninertgassuchasnitrogen. 6Testsp
29、ecimens 6.1Preparation PreparetestspecimensinaccordancewithISO113591,clause7. Thestandardtestspecimenisarectangularspecimen5mmto10mminlengt h and about 5m m in width. However, specimensofotherdimensionsmaybeusedbyagreementbetweentheinterestedparties.Theendsofthetest specimenshallbeparallel.Record,if
30、applicable,theorientationofthespecimenwithrespecttothedirectionof production,i.e.machinedirection,transversedirectionorother. Refertotherelevantmaterialstandardsforthenumberoftestspecimens,butprepar eandtestatleastthree specimensfromeachsample. 6.2Conditioning Refertotherelevantmaterialstandardsfort
31、heconditioningofspecimensbeforemeasurement. NOTE 1 Inordertoeli minateanyther malmemoryeffectsinthespeci men,itispreferablethateachspeci menbeheated from the minimum measurement temperature (at least 50C below Tg )tothemaximumtemperatur e (at least 50 C above Tg), thenheldatthislattertemperaturefor5
32、min.Subsequently,coolthespeciment o the minimum temperature at the same rate as thatwhichwillbeusedfortheactualdetermination. NOTE 2 Heatingthetestspecimentotemperature s of 50 C above Tg mayresultinchangesin molecularorientationand/or blendmorphology,therebychangingthecoefficientoflinearthermalexpa
33、nsionincertaindirections. 7Procedure 7.1Calibrationofapparatus CalibratetheapparatusinaccordancewithISO 113591.Aftercleaningthesurfacesofthespecimen,probeand sampleholder,placethespecimenonthesampleholderwiththeprobeascloseaspossible. 7.2Determination Settheunloadedprobeontheuppersurfaceofthespecime
34、n.Applyaloadofpreferably4, 0kPa 0,1kPa. Providedtheeffectonthemeasuredvalueissmall,otherloadsmaybeused.ISO113592:1999(E) 4 Whenspecimensmadeoffilm,fibreorsoftmaterialaretested,carryou t the determination in the tension mode with bothendsofthespecimengripped. Maintainaconstantgasflow,preferablyofdrya
35、ir,aroundthespecimenwithinaflowraterangeof5 0 ml/minto 100ml/min.However,otheratmospheresmaybeusedbyagreementbetweentheinterestedparties. Increasethetemperatureofthespecimenataconstantrateofnotmorethan5C/min. RecordtheTMAcurveforthetestspecimen,i.e.thechangeinlengthwithincreasingtemperature. NOTE1 I
36、tispreferablewithsomesamplesthatspecimenstakenindifferentdirectionsfromthesamplebeinvestigated. Measure,underthesameconditions,thechangeinlengthofareferencespecimenhavingaknownmean coefficientoflinearthermalexpansionandaboutthesamelengthasthetestspecimen. NOTE 2 This is not necessary when the appara
37、tusused measuresthedifferenceinlengthbetweenthetestspeci menanda referencespecimendirectly. 8Expressionofresults 8.1Methodofcalculation 8.1.1 Coefficientoflinearthermalexpansion a Thecoefficientoflinear thermal expansion a ,inreciprocalkelvins(K -1 ),attemperature TisobtainedfromtheTMA curveusingthe
38、followingequation(seeFigure1): a= d d 1L TL 0 where L 0 isthelengthofthespecimen,inmicrometres,atroomtemperature; L isthelengthofthespecimen,inmicrometres,attemperature T; T isinkelvins. Calculatethevalueof a tothenearest10 -7 K -1 foreachspecimen.Calculatethemea noftheseindividualvalues androundthe
39、meantothenearest10 -6 K -1 . Inthecaseofatestspecimenexhibitingaglasstransition,calculatethecoefficientbeforeandaftertheglass transition. ISO113592:1999(E) 5 Figure1Determinationofcoefficientoflinearthermalexpansion a 8.1.2 Meancoefficientoflinearthermalexpansion a 8.1.2.1 MethodA:Determinationwitho
40、utreferencespecimen Themeancoefficientoflinearthermalexpansion a,inreciprocalkelvins(K -1 ),betweentw otemperatures T 1 and T 2 isobtainedfromtheTMAcurveusingthefollowingequation(seeFigure2): a= D D L TL 1 0 where L 0 isthelengthofthespecimen,inmicrometres,atroomtemperature; D L isthedifferenceinlen
41、gth,inmicrometres; D T (= T 2 - T 1 )isthetemperaturedifference,inkelvins. Selecttwotemperaturesandcalculatethedifferenceintemperature D T. Determinethecorrespondingchangeinlength D LfromtheTMAcurve . Calculatethevalueof a tothenearest10 -7 K -1 for eachspecimen.Calculatethemeanoftheseindividualvalu
42、es androundthemeantothenearest10 -6 K -1 . Inthecaseofatestspecimenexhibitingaglasstransition,calculatethecoefficientbeforeandaftertheglass transition.ISO113592:1999(E) 6 Figure2Determinationofmeancoefficientoflinearthermalexpansion a 8.1.2.2 MethodB:Determinationwithreferencespecimen Themeancoeffic
43、ientoflinearthermalexpansion a,inreciprocalkelvins(K -1 ),betweentwotemperatures T 1 and T 2 isobtainedusingthefollowingequation: aa= - - + DD ( LL LTT Spm Ref Ref ) 021 where a isthemeancoefficientoflinearthermalexpansion,inreciprocalkelvins(K -1 ); L 0 isthelengthofthespecimen,inmicrometres,atroom
44、temperature; T 1 is the lower end of the temperaturerange,indegreesCelsius,usedtomeasurethecoefficientoflinear thermalexpansion; T 2 is the higher end ofthetemperaturerange,indegreesCelsius,usedtomeasurethecoefficientoflinear thermalexpansion; D L Spm isthedifferenceintestspecimenlength,i n micrometr
