1、BRITISH STANDARD BS EN ISO 2114:2000 BS 2782-4: Method 432B:2000 Incorporating Corrigendum No.1 Plastics (polyester resins) and paints and varnishes (binders) Determination of partial acid value and total acid value The European Standard EN ISO 2114:2000 has the status of a British Standard ICS 83.0
2、80.10 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN ISO 2114:2000 This British Standard, having been prepared under the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 1
3、5 November 2000 BSI 3 April 2002 ISBN 0 580 36545 X National foreword This British Standard is the official English language version of EN ISO 2114:2000. It is identical with ISO 2114:2000. It supersedes BS EN ISO 2114:1997 which is withdrawn. The UK participation in its preparation was entrusted to
4、 Technical Committee PRI/42, Fibre reinforced thermosetting plastics and prepegs, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references Attention is drawn to the fact that CEN and CENELEC Standards normall
5、y include an annex which lists normative references to international publications with their corresponding European publications. 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 en
6、titled “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 the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compl
7、iance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related
8、 international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to iv, pages 1 to 10, the Annex ZA page and a back cover. The BSI copyr
9、ight date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments 13829 Corrigendum No. 1 3 April 2002 Incorporating Annex ZAEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO2114 August2000 ICS83.080.10 SupersedesENISO2114
10、:1996 Englishversion Plastics(polyesterresins)andpaintsandvarnishes(binders) Determinationofpartialacidvalueandtotalacidvalue(ISO 2114:2000) Plastiques(rsinesdepolyesters)etpeinturesetvernis (liants)Dterminationdelindicedacidepartieletde lindicedacidetotal(ISO2114:2000) Kunststoffe(Polyester)undBesc
11、hichtungsstoffe (Bindemittel)BestimmungderpartiellenSurezahlund derGesamtsurezahl(ISO2114:2000) ThisEuropeanStandardwasapprovedbyCENon1August2000. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwith
12、outanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheCentralSecretariatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityof
13、aCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,Switzerlandan
14、dUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG CentralSecretariat:ruedeStassart,36B1050Brussels 2000CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO2114:2000ECORRECTED20020313 Foreword
15、Thisdocument(ISO2114:2000)hasbeenpreparedbyTechnicalCommitteeISO/TC61 “Plastics“incollaborationwithTechnicalCommitteeCEN/TC249“Plastics“,thesecretariatof whichisheldbyIBN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationof anidenticaltextorbyendorsement,atthelatestbyF
16、ebruary2001,andconflictingnational standardsshallbewithdrawnatthelatestbyFebruary2001. ThisdocumentsupersedesENISO2114:1996. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,Czech Republic,De
17、nmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg, Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandtheUnitedKingdom. Endorsementnotice ThetextoftheInternationalStandardISO2114:2000hasbeenapprovedbyCENasa EuropeanStandardwithoutanymodifications. NOTENormativereferencestoInte
18、rnationalStandardsarelistedinannexZA(normative). ENISO2114:2000 Referencenumber ISO2114:2000(E) INTERNATIONAL STANDARD ISO 2114 Thirdedition 2000-08-01 Plastics(polyesterresins)andpaintsand varnishes(binders)Determinationof partialacidvalueandtotalacidvalue Plastiques(rsinesdepolyesters)etpeinturese
19、tvernis(liants) Dterminationdelindicedacidepartieletdelindicedacidetotal ENISO2114:2000 ii ENISO2114:2000 iii Contents Page Foreword.iv 1 Scope1 2 Normativereferences1 3 Termsanddefinitions.1 4 Principle2 5 Reagents.2 6 Apparatus.3 7 Procedure.4 8 Calculationandexpressionofresults.6 9 Precision.7 10
20、 Testreport8 AnnexA(informative)Checkingtheconcentrationofthestandardpotassiumhydroxidesolution.9 ENISO2114:2000 iv Foreword ISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISO memberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedo
21、utthroughISOtechnical committees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhas therighttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnon-governmental,in liaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElec
22、trotechnical Commission(IEC)onallmattersofelectrotechnicalstandardization. InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IECDirectives,Part3. DraftInternationalStandardsadoptedbythetechnicalcommitteesarecirculatedtothememberbodiesforvoting. PublicationasanInternationalStandar
23、drequiresapprovalbyatleast75%ofthememberbodiescastingavote. AttentionisdrawntothepossibilitythatsomeoftheelementsofthisInternationalStandardmaybethesubjectof patentrights.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights. InternationalStandardISO2114waspreparedbyTechnicalCommitteeIS
24、O/TC61,Plastics,SubcommitteeSC12, Thermosettingmaterials. Thisthirdeditioncancelsandreplacesthesecondedition(ISO2114:1996)aswellasISO3682:1996,whichhave beentechnicallyrevised. ENISO2114:2000 1 Plastics(polyesterresins)andpaintsandvarnishes(binders) Determinationofpartialacidvalueandtotalacidvalue 1
25、 Scope ThisInternationalStandardspecifiesmethodsofdeterminingthepartialacidvalue(methodA)andthetotalacid value(methodB)ofpolyesterresinsandbindersforpaintsandvarnishes.Itisnotapplicabletophenolicresins. Itisintendedtoprovidequality-controldatafortheacceptanceorrejectionofsuchproductsinaccordancewith
26、the termsofaspecification,aswellastobeusedinresearchanddevelopmenttomonitorthecompletionofthe polycondensationreaction. 2 Normativereferences Thefollowingnormativedocumentscontainprovisionswhich,throughreferenceinthistext,constituteprovisionsof thisInternationalStandard.Fordatedreferences,subsequent
27、amendmentsto,orrevisionsof,anyofthese publicationsdonotapply.However,partiestoagreementsbasedonthisInternationalStandardareencouragedto investigatethepossibilityofapplyingthemostrecenteditionsofthenormativedocumentsindicatedbelow.For undatedreferences,thelatesteditionofthenormativedocumentreferredto
28、applies.MembersofISOandIEC maintainregistersofcurrentlyvalidInternationalStandards. ISO385-1:1984,LaboratoryglasswareBurettesPart1:Generalrequirements. ISO3251:1993,PaintsandvarnishesDeterminationofnon-volatilematterofpaints,varnishesandbindersfor paintsandvarnishes. ISO3696:1987,Waterforanalyticall
29、aboratoryuseSpecificationandtestmethods. ISO6353-2:1983,ReagentsforchemicalanalysisPart2:SpecificationsFirstseries. 3 Termsanddefinitions ForthepurposesofthisInternationalStandard,thefollowingtermsanddefinitionsapply. 3.1 acidvalue thenumberofmilligramsofpotassiumhydroxide(KOH)requiredtoneutralize1g
30、ofresinunderthetestconditions 3.2 partialacidvalue acidvaluecorrespondingtotheneutralizationofallthecarboxyl-terminatedgroupsandfreeacidsplushalfthefree anhydridesinaresin 3.3 totalacidvalue acidvaluecorrespondingtotheneutralizationofallthecarboxyl-terminatedgroupsandfreeacidsplusallthefree anhydrid
31、esinaresin ENISO2114:2000 2 4Principle 4.1 General Thefreeacids/anhydridescontainedinatestportionaretitratedwithpotassiumhydroxidesolution,either potentiometricallyorinthepresenceofacolourindicator. 4.2 MethodA Aweighedquantityofresinisdissolvedinasolventmixture.Thesolutionistitratedpotentiometrical
32、ly(seenote1) withastandardvolumetricsolutionofpotassiumhydroxideinethanol,givingthefollowingreaction: Theamount,inmilligrams,ofpotassiumhydroxideusedtoneutralize1gofresinisthencalculated. MethodAisrecommendedforbindersforpaintsandvarnishes(asgenerallyonlysmallamountsoffreeanhydrides arepresent)butis
33、alsosuitableforunsaturated-polyesterresins. 4.3 MethodB Aweighedquantityofresinisdissolvedinasolventmixtureincludingwater.Thefreeanhydridesareallowedto hydrolysefor20minbeforetitratingpotentiometrically(seenote1)withastandardvolumetricsolutionofpotassium hydroxideinethanol,givingthefollowingreaction
34、: Theamount,inmilligrams,ofpotassiumhydroxideusedtoneutralize1gofresinisthencalculated. MethodBisusefulforunsaturated-polyesterresinsinwhichtherearesignificantamountsoffreeanhydrides. NOTE1 Theuseofacolourindicatorforthetitrationisanoptionalalternativeinbothmethods. NOTE2 Whentitratingpuremaleicpoly
35、esterresins,itisbettertouseamethanolicsolutionofpotassiumhydroxide. 5 Reagents Duringtheanalysis,useonlyreagentsofrecognizedanalyticalgradeinaccordancewithISO6353-2andwaterof atleastgrade3asdefinedinISO3696. 5.1 SolventformethodA:solventmixturecontaining2partsoftoluene(5.7)and1partofethanol(5.5)by v
36、olume. Neutralizethesolventmixturewithpotassiumhydroxidesolution(5.3)priortouse,usingphenolphthaleinas indicatorifthedeterminationistobecarriedoutbypotentiometrictitration(see7.2.2)or,ifthedeterminationisto becarriedoutusinganindicator(see7.2.3),usingthesameindicatoraswillbeusedforthedetermination.
37、ENISO2114:2000 3 5.2 SolventformethodB:solventmixturecontaining400mlofpyridine(5.8),750mlofmethylethylketone (5.9)and50mlofwater. 5.3 Potassiumhydroxide,0,1mol/lstandardvolumetricsolutioninethanol(5.5)orinmethanol(5.6),freefrom carbonates. Checktheconcentrationofthissolutiononthedayofuse(seeannexA).
38、 Ifmorethan25mloftitrantwillberequiredwitha0,1mol/lsolution,usea0,5mol/lsolutiontoavoidtheadditional errorsinvolvedinrefillingtheburette(6.3). 5.4 Acetone,containinglessthan0,3%bymassofwater. 5.5 Ethanol,anhydrous,containinglessthan0,2%bymassofwater. 5.6 Methanol,anhydrous,containing99,8%bymass. 5.7
39、 Toluene,anhydrous,containinglessthan0,005%bymassofwater. 5.8 Pyridine,containinglessthan0,05%bymassofwater. WARNINGPyridineistoxicandflammable.Takeproperprecautionswhenhandlingthisreagent.Avoid contactwiththeskinoreyes.Useonlyinawellventilatedareainordertoavoidbreathinginthevapour. 5.9 Methylethylk
40、etone,containinglessthan0,01%bymassofwater. 5.10Indicators(foroptionalalternative): 5.10.1Bromothymolblue,0,1%solutioninethanol(5.5). 5.10.2Phenolphthalein,1%solutioninethanol(5.5). 6 Apparatus Ordinarylaboratoryapparatusandglassware,plusthefollowing: 6.1 Conicalflasks,ofcapacities100mland250ml,with
41、awideneck. 6.2 Conicalflask,ofcapacity250ml,withanarrowneckandfittedwithaground-glassstopper. 6.3 Burette,ofcapacity25ml(graduatedin0,05mldivisions),complyingwiththerequirementsofISO385-1. 6.4 Magneticstirrer. 6.5 Pipettes,ofcapacity25mland50ml. 6.6 Automaticpipettes,ofcapacity25ml,50mland60ml. 6.7
42、Analyticalbalance,accurateto1mg. 6.8 Potentiometric-titrationapparatus,comprisingasuitablepotentiometerfittedwithaglassreference electrodesystemandatitrationstand. ENISO2114:2000 4 7 Procedure 7.1 Testportion ByreferencetoTable1,selecttheappropriatemassoftestportiontobetaken. Table1Massoftestportion
43、 Expectedacidvalue Approximatemassoftest portion mgKOH/g g 0to5 W16 5to10 8 10to25 4 25to50 2 50to100 1 100 0,7 7.2 MethodA 7.2.1 Numberofdeterminations Maketwodeterminations. 7.2.2 Potentiometric-titrationprocedure Weigheachtestportionintoa250mlwide-neckconicalflask(see6.1)tothenearest0,001g(massm
44、1 ).Add 50mlofsolventmixture(5.1)usingapipette(6.5).Mixuntiltheresiniscompletelydissolved. Ifsolubilityisincompleteafter5min,prepareanothertestportion,butdissolveitin50mlofsolventmixture(5.1) and25mlofacetone(5.4). Placetheconicalflaskonthetitrationstand(see6.8)andadjustitspositionsothattheelectrode
45、iswellimmersed. Titratepotentiometricallywithpotassiumhydroxidesolution(5.3)usingaburette(6.3).Recordthevolume(V 1 ),in millilitres,ofKOHsolutionusedtoreachtheendpoint(thepointofinflectionofthetitrationcurve). Carryoutablankdeterminationinthesameway,using50mlofsolventmixtureand,ifneeded,25mlofaceton
46、e. Recordthevolume(V 2 ),inmillilitres,ofKOHsolutionused.Iftheneutralizationofthesolventmixturehasbeen carriedoutcorrectly,theresultoftheblankdeterminationwillbezero. 7.2.3 Colorimetric-titrationprocedure Asanalternative,acolourindicatorcanbeusedinsteadofthepotentiometric-titrationapparatus,asfollow
47、s: Addatleast3dropsofphenolphthaleinsolution(5.10.2)tothedissolvedtestportion.Titratewithpotassium hydroxidesolutionfromtheburetteuntilaredcolorationjustappearsandisstableforatleast10swhilethe solutionisstirred.Ifthecolourchangewithphenolphthaleinisnotverydefinite,useanotherindicator,forexample 5dro
48、psofbromothymolblue(5.10.1)(forwhichtheendpointiswhenthecolourremainsbluefor20sto30s). Recordthevolume(V 1 ),inmillilitres,ofKOHsolutionused. ENISO2114:2000 5 Carryoutablankdeterminationusing50mlofsolventmixtureand,ifneeded,25mlofacetone.Addthesame quantityofindicatorsolution.Titratetothesameendpointasobtainedwhentheresinwaspresent.Recordthe volume(V 2 ),inmillilitres,ofKOHsolutionused.Iftheneutralizationofthesolventmixturehasbeencarriedout corre
