BS EN 1877-1-2000 Products and systems for the protection and repair of concrete structures - Test methods - Reactive functions related to epoxy resins - Determination of epoxy equ.pdf

1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS EN 1877-1:2000 The Eur

2、opean Standard EN 1877-1:2000 has the status of a British Standard ICS 91.080.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Products and systems for the protection and repair of concrete structures Test methods Reactive functions related to epoxy resins Part 1: Determinat

3、ion of epoxy equivalentThis British Standard, having been prepared under the direction of the Sector Committee for Building and Civil Engineering, was published under the authority of the Standards Committee and comes into effect on 15 October 2000 BSI 10-2000 ISBN 0 580 36599 9 BS EN 1877-1:2000 Am

4、endments issued since publication Amd. No. Date Comments National foreword This British Standard is the official English language version of EN 1877-1:2000. The UK participation in its preparation was entrusted by Technical Committee B/517, Concrete, to Subcommittee B/517/8, Protection and repair of

5、 concrete, which has the responsibility to: aid enquirers to understand the text; present to the responsible European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate the

6、m in the UK. A list of organizations represented on this subcommittee can be obtained on request to its secretary. Cross-references 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

7、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 the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Com

8、pliance 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 EN title page, pages 2 to 8, an inside back cover and a back cover. The BSI copyright notice displayed in this document indica

9、tes when the document was last issued.EUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN18771 July2000 ICS91.080.40 Englishversion Productsandsystemsfortheprotectionandrepairofconcrete structuresTestmethodsReactivefunctionsrelatedtoepoxy resinsPart1:Determinationofepoxyequivalent Produitsetsystmespou

10、rlaprotectionetlarparationdes structuresenbtonMthodesdessaiFonctions ractivesdesrsinespoxydesPartie1:Dterminationde lquivalentpoxyde ProdukteundSystemefrdenSchutzunddie InstandsetzungvonBetontragwerkenPrfverfahren Reaktive,funktionelleGruppenvonEpoxidharzenTeil1: BestimmungdesEpoxidquivalents ThisEu

11、ropeanStandardwasapprovedbyCENon7July2000. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtained

12、onapplicationtotheCentralSecretariatortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheCentralSecretariathasthesamestatusast heofficial versions. C

13、ENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORM

14、UNG CentralSecretariat:ruedeStassart,36B1050Brussels 2000CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN18771:2000EPage2 EN18771:2000 Contents Page Foreword. 3 1 Scope 4 2 Normativereferences 4 3 Termsanddefinitions . 4 4 Principle 4 5 Sampling. 4

15、6 Apparatus . 5 7 Reagents. 5 8 Preparationoftheperchloricacid(0,1mol/l)inaceticacid 5 9 Standardization 6 10 Calculationoftheconcentration. . 6 11 PreparationoftheTetraethylammoniumbromidereagentsolution 6 12 Procedure. 6 13 Calculation . 7 14 Precision. 7 15 Testreport 7 Bibliography . 8Page3 EN18

16、771:2000 Foreword ThisEuropeanStandardhasbeenpreparedbyTechnicalCommitteeCEN/TC104“Concrete(performance, production,placingandcompliancecriteria)“,thesecretariatofwhichisheldbyDIN . ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atth

17、elatestbyDecember2002,andconflictingnationalstandardsshallbewithdrawnatthelatest byDecember2002. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany

18、,Greece,Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden, SwitzerlandandtheUnitedKingdom. ThisEuropeanStandarddescribesseveraltypeoftestmethods.Specificationsfortheproductsandsystemsforthe protectionandrepairofconcretestructureswillbesubjectofseparatestandards. ThisEuropeanS

19、tandardisbasedontheISO3001:1997standard.Page4 EN18771:2000 1 Scope ThisEuropeanStandardspecifiesamethodforthedeterminationoftheepoxyequivalentandisapplicabletoall epoxycompounds,forproductsandsystemsfortheprotectionandrepairofconcretestructure.ThisEuropean standarddoesnotapplytothemeasurementofepoxi

20、deequivalentofnitrogencontainingresins. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetextandthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrev

21、isionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). EN21512 PaintsandvarnishesSamplingofproductsinliquidorpasteform (ISO1512:1991) 3 Termsanddefinitions Fo

22、rthepurposesofthisstandardthefollowingtermsanddefinitionsapply: 3.1 epoxideequivalent Themassofresin,ingrams,whichcontainsonemoleofepoxidegroup. 3.2 expoxidenumber equivalent epoxide 100 group epoxy of mass Molar Contentofepoxygroupsin(%)in100gepoxyresin 3.3 epoxideindex equivalent epoxide 1000 Mole

23、sofepoxideperkilogramepoxyresin. 4 Principle Reactionoftheepoxidegroupswithnascenthydrogenbromideproducedbytheactionof0,1mol/lstandard volumetricperchloricacidsolutionontetraethylammoniumbromide.Determinationoftheendpointeitherusing crystalvioletasindicatororbyapotentiometricmethod. 5 Sampling Arepr

24、esentativeandhomogeneoussampleofthematerialtobetestedshallbetakenaccordingtoEN21512. Eliminatemineralfillerandpigmentswithasuitableorganicsolventbeforethedeterminationoftheepoxide equivalent.Itshouldbechecked,thatanysolventhasevaporated.Page5 EN18771:2000 6 Apparatus Balance,accuratetowithin0,1mg. C

25、alibratedburette,capacity50ml. Pipette,capacity10ml Conicalflask,100mlor200ml,withgroundglassneckandgroundglassstopper. Instrumentandelectrodesforpotentiometrictitration. Inaddition,whenpreparedthe0,1mol/lperchloricacidinaceticacid. Magneticstirrerwithpolytetrafluoroethylenecoatedbar. Calibratedther

26、mometertopermittemperaturemeasurementswithinanaccuracyof0,1K. Volumetricflask,1000ml. Graduatedcylinders,50mland500ml. 7 Reagents Fortheanalysis,onlyreagentsofanalyticalgradeshallbeused. Perchloricacid,0,1mol/linaceticacid(Standardvolumetricsolution). Tetraethylammoniumbromide. Tetrabuthylammoniumio

27、dide. Aceticacid99%to100%. Chloroform,methylenchloride,acetone. Crystalviolet,0,1%insolutioninaceticacid. Potassiumhydrogenphthalate. Inaddition,whenpreparedthe0,1mol/lperchloricacidinaceticacid. Aceticacid99%to100%. Aceticanhydride,purity96%. Phenolphthalein,0,1%solution. Perchloricacid,70%. Sodium

28、hydroxidesolution0,1mol/l. Distilledwater. 8 Preparationoftheperchloricacid(0,1mol/l)inaceticacid WARNINGTheuseofsafetygogglesandasafetyscreenisrecommended. Determinationofthetruepercentageoftheapproximately70%(m/m)perchloricacid.Weighapproximately0,3g oftheperchloricacid(E 1 )ina200mlconicalflask,a

29、dd50mldistilledwaterandmixthoroughly.Titrateitagainst 0,1mol/lsodiumhydroxidesolution(V 1 )usingthephenolphthaleinindicatorsolution.Thecontentofperchloricacid isgivenbytheequation: P= E 1000 V F 1 1N a O H where P =contentoftheperchloricacid; E 1 =isthemassin(g),oftheapproximate70%perchloricacid; V

30、1 =isthevolume,in(ml),ofthe0,1mol/lsodiumhydroxidesolution; F naOH =isthefactorofthe0,1mol/lsodiumhydroxidesolution. Weighthecalculatedmassofthe70%aqueoussolutionoftheperchloricacidtoanaccuracyof0,1mgintoa 1000mlvolumetricflask.Add300mloftheaceticacidfollowedby50mloftheaceticanhydrideundercooling. T

31、hetemperatureofthesolutionshallbekeptat20C.Diluteto1000mlwiththeaceticacidandmixthoroughly. Thesolutionshouldnotshowanydiscolorationtoyellowforaperiodof12h.Thencarryoutthestandardization.Page6 EN18771:2000 9 Standardization a)Standardizethissolutionbytitratingitina200mlconicalflaskto300mgto500mgpota

32、ssiumhydrogen phthalatedissolvedin15mlaceticacid,usingthecrystalvioletindicatorsolution.Ifnecessary,drythepotassium hydrogenphthalatefor24hoursat120Cbeforeuse.Carryouttheendpointdeterminationusing4to6dropsof thecrystalvioletindicatorsolution,titratinguntilastablegreencolourisobtained.Recordthetemper

33、ature t s ofthe standardvolumetricsolution.Carryoutadoubledetermination. NOTE: Ifthepotentiometricmethodisusedforthedeterminationofepoxideequivalent,itisrecommendedtousethesame methodforthestandardizationoftheperchloricacid. b)Alternative:Usethemanufacturersconcentrationofthesolution. 10 Calculation

34、oftheconcentration Theconcentrationcoftheperchloricacidsolutioninmolesperlitreisgivenbytheequation: c= E V 0,2042 2 2 where E 2 :isthemass,in(g),ofpotassiumhydrogenphthalateused; V 2 :isthevolume,in(ml),oftheperchloricacidsolutionusedinthetitration. 11 PreparationoftheTetraethylammoniumbromidereagen

35、tsolution Dissolve100goftetraethylammoniumbromidein400mloftheaceticacid.Addafewdropsofthecrystalviolet indicatorsolution;ifitchangescolour,bringitbacktotheoriginalcolourwiththestandardvolumetricperchloric acidsolution. NOTE Forsomeepoxidecompoundsoflowreactivity,theuseoftetrabutylammoniumiodideisadv

36、ised,eitherasthesolid orasa10%solutioninchloroform;inthiscase,lightshouldbeexcludedasmuchaspossible.Solutionsoftetrabutyl ammoniumiodideinchloroformareunstableandshouldbefreshlypreparedforeachtitration. 12 Procedure Weighintotheflask,tothenearest0,1mg,atestportioncontainingfrom0,6mmolto0,9mmolofepox

37、ygroups (thiscorrespondstoamassofbetween0,6xEEmgand0,9xEEmg,whereEEistheestimatedepoxy equivalent). Add10mlofsolvent,thendissolvethetestportionusingthemagneticstirrerand,ifnecessary,byheating slightly. Cooltoroomtemperature,add20mlofaceticacidandthen,withthepipette,10mloftetraethylammonium bromideso

38、lution. Ifusingtheindicatormethod,add4to6dropsofcrystalvioletsolutionandtitratethesolutiononthemagnetic stirrerwiththeperchloricacidsolution. Carryoutthetitrationuntilastablegreencolourisobtained. Ifusingthepotentiometricmethod,placetheelectrodesinthetestsolutionandtitratethesolutiononthe magneticst

39、irrerwiththeperchloricacidsolution. Notethetemperaturetoftheperchloricacidsolutioninordertobeabletoallowforexpansionofthesolution withincreasingtemperature. Carryoutablanktestanthesametimeasthedetermination,followingthesameprocedureandusingthesame reagentsbutomittingthetestportion.Page7 EN18771:2000

40、 13 Calculation Theepoxideequivalent EE isgivenbytheequation: where m isthemass,in(g),ofthetestportion; V 0 isthevolume,in(ml),oftheperchloricacidsolutionusedintheblanktest; V 1 isthevolume,in(ml),oftheperchloricacidsolutionusedinthedetermination; tisthetemperature,in(C),oftheperchloricacidsolutiona

41、tthetimeofthedeterminationandblanktest; t s isthetemperature,in(C),oftheperchloricacidsolutionatthetimeofstandardization; cistheconcentrationoftheperchloricacidsolution(usually0,1mol/l)atthetimeofstandardization. NOTE Theuseofthecorrectionfactorisrecommendedbecauseofthesignificantcoefficientofexpans

42、ionoftheperchloric acidsolution(1,07x10 3 K 1 ),whichcorrespondstoavolumevariationof0,1%perKelvin.Useofthisfactorcanbeavoided byworkinginatemperaturecontrolledroom. 14 Precision Repeatabilitylimit :0,5% Reproducibilitylimit :1%. 15 Testreport Thetestreportshallincludethefollowinginformation: a) aref

43、erencetothisEuropeanStandard; b) alldetailsnecessarytoidentifytheproducttested; c) theepoxideequivalentandthewayinwhichitisexpressed; d) thereagentusedifitisnottetraethylammoniumbromide; e) anyotherfactorlikelytohaveaffectedtheresult; f) anydeviations,byagreementorotherwise,fromtheproceduredescribed; g) thedateoftest. EE= 1000 m ( V V )1 t t 1000 1o s cPage8 EN18771:2000 Bibliography ISO3001:1997 PlasticsEpoxycompoundsDeterminationofepoxyequivalent .blankBS EN 1877-1:2000 BSI