1、BRITISH STANDARD BS EN ISO 10548:2003 Carbon fibre Determination of size content ICS 59.100.20 Incorporating October2008corrigendumNational foreword This British Standard is the UK implementation of EN ISO 10548:2003. It is identical with ISO 10548:2002 incorporating corrigendum October 2008. It sup
2、ersedes BS EN ISO 10548:1996 which is withdrawn. The UK participation in its preparation was entrusted to Technical Committee PRI/42, Fibre reinforced thermosetting plastic and prepegs. A list of organizations represented on this committee can be obtained on request to its secretary. This publicatio
3、n does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard cannot confer immunity from legal obligations. BS EN ISO 10548:2003 This British Standard was published under the authority of the Standards
4、 Policy and Strategy Committee on 9 July 2003 BSI 2009 ISBN 978 0 580 67849 3 Amendments/corrigenda issued since publication Date Comments 31 October 2009 Implementation of ISO corrigendum October 2008. Text deleted in clauses 2 and 5EUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO10548 July2003
5、 ICS59.100.20 SupersedesENISO10548:1996 Englishversion CarbonfibreDeterminationofsizecontent(ISO10548:2002) FibresdecarboneDterminationdutauxdensimage (ISO10548:2002) KohlenstofffasernBestimmungdes Prparationsmassenanteils(ISO10548:2002) ThisEuropeanStandardwasapprovedbyCENon5June2003. CENmembersare
6、boundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEuropean Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcerningsuchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEu
7、ropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytranslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusastheofficial versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRep
8、ublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUnited Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG ManagementCentre:ruedeStass
9、art,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO10548:2003EForeword ThetextofISO10548:2002hasbeenpreparedbyTechnicalCommitteeISO/TC61“Plastics”of theInternationalOrganizationforStandardization(ISO)andhasbeentakenoverasENIS
10、O 10548:2003byTechnicalCommitteeCEN/TC249“Plastics“,thesecretariatofwhichisheldby IBN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationof anidenticaltextorbyendorsement,atthelatestbyJanuary2004,andconflictingnational standardsshallbewithdrawnatthelatestbyJanuary2004.
11、ThisdocumentsupersedesENISO10548:1996. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Czech Republic,Denmark,Finland,France,Germany,Greece,Hungary,Iceland,Ireland,Italy, Luxembourg,Malta,Ne
12、therlands,Norway,Portugal,Slovakia,Spain,Sweden,Switzerlandand theUnitedKingdom. Endorsementnotice ThetextofISO10548:2002hasbeenapprovedbyCENasENISO10548:2003withoutany modifications. NOTENormativereferencestoInternationalStandardsarelistedinannexZA(normative). BS EN ISO 10548:2003 EN ISO 10548:2003
13、INTERNATIONAL STANDARD ISO 10548 Secondedition 20020715 Referencenumber ISO 10548:2002(E) Carbonfibre Determinationofsize content Fibresdecarbone Dterminationdutauxdensimage BS EN ISO 10548:2003 EN ISO 10548:2003ii FDPdicslaimre ThisFDPfamelitnocytdeddebmeniayfep.secaInroccatiwecnadAhycilopgnisnecil
14、sebod,thfsimeliarpebytnieivrodewbdetusllahtoneb tidesselnudettehyfepsecahwichraemeileradeddebctdesnetsnidnaolatnodelmocehtupreepfrromigntideehti.gnInodaolnwdinghtislife, rapticcasetpetrehietnehserilibisnoptyfotonfnirisebodAgnignilopgnisnecilcy.TIehSOtneCrceSlarteraitacatpeconsillibaytiinihtsaera. eb
15、odAsitarmedarakfodASebotsysmeInroctarop.de teDailfostfosehtwareprtcudostdesuocrtaetehFDPsiffebnacelitnidnuoGehlareneInfotalerivetotfeh;elitehPDFrctaeirapnomateers weertpofdezimiorrptnii.gnvErecyaeebsahertnaktneorusnetetahtfehielistiusbafelobesuryISOmerebmseidob.Inthekilnuleyevtne ttahaborpmeltalerig
16、ntotifsi,dnuosaelpfnieromtehtneCSlartercerataitathserddaesigvneolebw. BS EN ISO 10548:2003 EN ISO 10548:2003iii Contents Page 1 Scope . 1 2 Normativereference . 1 3 Termsanddefinitions 1 4 Principle 1 5 Testspecimens. 2 6 Conditioning 2 7 Testmethods 2 7.1 Method A:Solventextraction. 2 7.2 Method B:
17、Digestionwithsulfuricacidandhydrogenperoxide . 4 7.3 Method C:Decompositionbypyrolysis 7 8 Precision. 8 9 Testreport 8 BS EN ISO 10548:2003 EN ISO 10548:2003iv Foreword ISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISO member bodies). The work of
18、preparing International Standards is normally carried out through ISO technical committees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhas therighttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnongovernmental,in liaison with ISO, also tak
19、e part in the work. ISO collaborates closely with the International Electrotechnical Commission(IEC)onallmattersofelectrotechnicalstandardization. InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IECDirectives,Part 3. DraftInternationalStandardsadoptedbythetechnicalcommitteesare
20、circulatedtothememberbodiesforvoting. PublicationasanInternationalStandardrequiresapprovalbyatleast75 %ofthememberbodiescastingavote. AttentionisdrawntothepossibilitythatsomeoftheelementsofthisInternationalStandardmaybethesubjectof patentrights.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchp
21、atentrights. InternationalStandardISO 10548waspreparedbyTechnicalCommitteeISO/TC 61,Plastics,SubcommitteeSC 13, Compositesandreinforcementfibres. Thissecondeditioncancelsandreplacesthefirstedition(ISO 10548:1994),whichhasbeentechnicallyrevised. BS EN ISO 10548:2003 EN ISO 10548:20031 Carbonfibre Det
22、erminationofsizecontent 1 Scope ThisInternationalStandardspecifiestestmethodsforthedeterminationofthesizecontentofcarbonfibreyarn.Itis applicabletocontinuousfilamentyarnsandstaplefibreyarns. 2 Normativereference 3 Termsanddefinitions ForthepurposesofthisInternationalStandard,thefollowingtermsanddefi
23、nitionsapply. 3.1 size anymaterialappliedtofibrestofacilitatethehandlinganduseofthefibres 3.2 sizecontent massofthesizeexpressedasapercentageofthesizedcarbonfibreyarn 4 Principle Testspecimensareweighedbeforeandafterremovalofthesizebyoneofthefollowingthreemethods: method A: size removal by Soxhlet e
24、xtraction, to be used when the size is completely soluble in a suitable solvent; method B:sizeremovalbychemicaldigestionusingamixtureofsulfuricacidandhydrogenperoxide,used whenthesizeispartiallyhardenedandnotcompletelysolubleinsolvents; method C:sizedecompositionbypyrolysisathightemperatureinanatmos
25、phereofnitrogen,usedwhenthe sizeiscompletelyremovedbypyrolysis. Methods AandBrequirethelastweighingtobemadetoconstantmassbyrepetitionofthefinaldryingandweighing procedure.Inthosecaseswhereknownmaterialsarebeingtestedregularly,itispermittedtodefine,byexperiment, aminimumtimefordryingwhichwillensureth
26、atconstantmasshasbeenreached.Particularcaremayberequired ifthecarbonfibreorsizingiswaterabsorbent. BS EN ISO 10548:2003 EN ISO 10548:20032 5 Testspecimens Twotestspecimensormoreshallbetakenfromeachlotoryarnsample.Thesizecontentistakenastheaverageof thetwoormoredeterminations. Whenhandlingtestspecime
27、ns,glovesshallbewornortweezersusedtoavoiddamagetothespecimens. NOTE Thespecificationorthepersonrequiringthetestmaystipulatethatadditionaldeterminationsbecarriedoutatdifferent placeswithintheelementaryunit. 6 Conditioning Elementaryunitsandyarnsamplesshallbeallowedtoattainlaboratorytemperaturebeforet
28、esting.Beforeweighing theyarn,itshallbedriedifrequired. 7 Testmethods 7.1 Method A:Solventextraction 7.1.1 Apparatusandmaterials 7.1.1.1 Balance,accurateto ,readableto . 7.1.1.2 Hotairoven ,capableofbeingcontrolledto . 7.1.1.3 Desiccator, containing a suitable desiccant, for example silica gel, anhy
29、drous calcium chloride or phosphorouspentoxide. 7.1.1.4 Soxhletextractor , capacity,witha flask. 7.1.1.5 Soxhletextractionthimbles ,measuring . NOTE ThesizesoftheSoxhletextractor,theflaskandtheSoxhletextractionthimblesaregivenasanindicationonlyandmay bevariedtosuitindividualrequirements. IMPORTANT T
30、he extraction and all handling of organic solvents should be carried out in a fume cupboard. 7.1.1.6 Rubbergloves ortweezers. 7.1.1.7 Cuttingblade . 7.1.1.8 Heatingmantle ,fittedwithapowerregulatorcapableofcontrollingtheboilingrateofthesolvent. 7.1.1.9 Distilled water , or an organic solvent such as
31、 butan2one (methyl ethyl ketone), tetrahydrofuran, dichloromethane(methylenechloride),acetoneordichloroethane. NOTE Thechoiceofsolventdependsuponthetypeofsizeappliedtothecarbonfibreundertest.Thischoiceisbestmadeby consultationbetweenthecustomerandthesupplier. 0,5 mg 0,1 mg 5 C 200 ml 500 ml 41 mm 12
32、3 mm BS EN ISO 10548:2003 EN ISO 10548:2003 3 7.1.2 Procedure 1 7.1.2.1 Dryanextractionthimble(7.1.1.5)at intheoven(7.1.1.2)for andallowtocooltoroom temperatureinadesiccator(7.1.1.3). 7.1.2.2 Weighthethimbletothenearest ( ). 7.1.2.3 Placeatestspecimeninthethimbleandweightothenearest ( ). 7.1.2.4 Pla
33、cethethimbleanditscontentsinthesiphonchamberoftheSoxhletapparatus(7.1.1.4),andplacea sufficientvolumeofsolventintheflasktoensureoperationofthesiphonduringtherefluxcycles. 7.1.2.5 Extractfor ,adjustingtheheatingmantle(7.1.1.8)sothatatleastfourrefluxcyclesoccurduringthe extraction period (a shorter ex
34、traction periodmay, however,be used if itcan bedemonstratedtogive complete extraction). 7.1.2.6 Turnofftheheatingmantle.Wait fortheapparatustocool.Removethethimbleandcontents.Allow tostandatambienttemperaturefor toallowexcesssolventtoevaporate. 7.1.2.7 Drythethimbleandcontentsfor intheoven(7.1.1.2)a
35、t (or,ifthesolventusedhasa boilingpointhigherthan ,atatemperature abovetheboilingpointofthesolvent)andallowtocoolina desiccator.Weightothenearest . 7.1.2.8 Repeatthedryingandweighingprocedureuntilthedifferenceinmassbetweentwosuccessiveweighings ( ) is less than . If a minimum drying time known to gi
36、ve constant mass has been established (see clause 4),thisrequirementdoesnotapply. 7.1.3 Procedure 2 7.1.3.1 IfthespecimenisfreeofloosefibreandcanbecoiledintoaformwhichcanbeinsertedintotheSoxhlet extractionchamberwithoutthedangeroflossoffibreduringextraction,anextractionthimbleneednotbeused. 7.1.3.2
37、Weighthetestspecimentothenearest ( ). 7.1.3.3 CarryouttheextractionasdescribedinProcedure 1,butwithouttheextractionthimble. 7.1.3.4 Drythespecimenfor at orahighertemperature(see7.1.2.7)andallowtocoolina desiccator.Weightothenearest . 7.1.3.5 Repeatthedryingandweighingprocedureuntilthedifferenceinmas
38、sbetweentwosuccessiveweighings ( ) is less than . If a minimum drying time known to give constant mass has been established (see clause 4),thisrequirementdoesnotapply. 7.1.4 Expressionofresults 7.1.4.1 Procedure 1 CalculatethesizecontentSC,expressedasapercentagebymass,fromtheequation: 105 C 5 C1 h 0
39、,1 mg m 1 0,1 mg m 2 2h 2h 10 min 10 min 1h 1 10 C 5 C 100 C1 0 C 0,1 mg m 3 0,2 mg 0,1 mg m 4 1h 1 10 C 5 C 0,1 mg m 5 0,2 mg SC = m 2 m 3 m 2 m 1 100 BS EN ISO 10548:2003 EN ISO 10548:20034 where istheinitialmass,ingrams,oftheextractionthimble; istheinitialmass,ingrams,ofthethimbleplustestspecimen
40、; isthefinalmass,ingrams,ofthethimbleplustestspecimenafterextraction. 7.1.4.2 Procedure 2 CalculatethesizecontentSC,expressedasapercentagebymass,fromtheequation: where istheinitialmass,ingrams,ofthespecimen; isthefinalmass,ingrams,ofthespecimenafterextraction. 7.2 Method B:Digestionwithsulfuricacida
41、ndhydrogenperoxide 7.2.1 Apparatusandreagents 7.2.1.1 Balance,accurateto ,readableto . 7.2.1.2 Hotairoven ,capableofbeingcontrolledto . 7.2.1.3 Desiccator, containing a suitable desiccant, for example silica gel, anhydrous calcium chloride or phosphoruspentoxide. 7.2.1.4 Fumecupboard . 7.2.1.5 Rubbe
42、rgloves ,faceshield andlaboratorycoat . 7.2.1.6 Sinteredglassfilters ,porosityP 40,porediameter to ,capacity to . 7.2.1.7 Cuttingblade . 7.2.1.8 Dryblockheater (seeFigure 1),fittedwithanexhausthoodconnectedtoascrubbingsystemandsuction pump,andalsofittedwithafixedsupportrackdesignedtoholddigestiontub
43、esandgraduateddroppingfunnelsfor theadditionofreagents.Theheatingblockshallbeplacedonasecurelaboratoryjackorsimilaritemofequipment. 7.2.1.9 Concentratedsulfuricacid ,atleast (bymass)( ). 7.2.1.10 Hydrogen peroxide solution , containing at least (by mass) H 2 O 2 . The volumes given in the procedurearefor (bymass). 7.2.1.11 Sodiumhydroxidesolution ,containingapproximately (bymass)NaOH,foruseinneutralizingacid fumesextractedbytheexhausthood. m 1 m 2 m 3 SC = m 4 m 5 m 4 100
