1、BRITISH STANDARD BS EN 13435:2002 Surface active agents Determination of free amine content of alkyl dimethyl betaines The European Standard EN 13435:2001 has the status of a British Standard ICS 71.100.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN 13435:2002 This Br
2、itish Standard, having been prepared under the direction of the Materials and Chemicals Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 5 March 2002 BSI 5 March 2002 ISBN 0 580 39211 2 National foreword This British Standard i
3、s the official English language version of EN 13435:2001. The UK participation in its preparation was entrusted to Technical Committee CII/34, Methods of test for surface active agents, which has the responsibility to: A list of organizations represented on this committee can be obtained on request
4、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 entitled “International Standards Correspondence Index”, or by using the “Find” facility of the B
5、SI 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. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid en
6、quirers 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 them in the UK. Summary of pages This document compri
7、ses a front cover, an inside front cover, the EN title page, pages 2 to 10, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE
8、EUROPISCHENORM EN13435 December2001 ICS71.100.40 Englishversion SurfaceactiveagentsDeterminationoffreeaminecontentof alkyldimethylbetaines AgentsdesurfaceDterminationdelateneurenamines libresdanslesalkyldimthylbtanes GrenzflchenaktiveStoffeBestimmungdesfreien AmingehaltesvonAlkyldimethylbetainen Thi
9、sEuropeanStandardwasapprovedbyCENon11November2001. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybe
10、obtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official version
11、s. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFR
12、NORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN13435:2001EEN13435:2001(E) 2 Contents page Foreword3 1 Scope 4 2 Normativereferences 4 3 Termsanddefinitions. .4 4 Principle4 5 Reagents.4 6 A
13、pparatus .5 7 Samplingandsample. .5 8 Procedure .5 9 Expressionofresults . .5 10 Precision.6 11 Testreport 6 AnnexA (informative) Ringtestresults . .7 AnnexB (informative) Instrumentsettings. 8 AnnexC (informative) Exampleforatypicaltitrationcurveanditsderivative 9 Bibliography 10EN13435:2001(E) 3 F
14、oreword ThisEuropeanStandardhasbeenpreparedbyTechnicalCommitteeCEN/TC 276“Agentsdesurface“,the secretariatofwhichisheldbyAFNOR. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyJune2002,andconflictingnationalstandardsshall
15、bewithdrawnatthelatestby June2002. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Po
16、rtugal,Spain,Sweden, SwitzerlandandtheUnitedKingdom. AnnexesA,BandCareinformative.EN13435:2001(E) 4 1Scope ThisEuropeanStandardspecifiesamethodforthedeterminationof0,02mmolto1mmoloffreeamineinalkyl dimethylbetaines.Monochloroaceticacid,glycolicacidandstrongacidsdonotinterferethedetermination. 2 Norm
17、ativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuro
18、pean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). ENISO3696, WaterforanalyticallaboratoryuseSpecificationandtestmethods(ISO3696:1987) . ISO607, SurfaceactiveagentsanddetergentsMethodsofsampledivisio
19、n . 3 Termanddefinition ForthepurposesofthisEuropeanStandard,thefollowingtermanddefinitionapply. 3.1 freeamine contentofamineinalkyldimethylbetaineswhichcanbedeterminedbythismethod,expressedingramsper100g 4Principle Thesampleofalkyldimethylbetaineisdissolvedinaqueouspropan2ol.Allthecomponentsareconv
20、ertedinto theirbasicformbyadditionofsodiumhydroxidesolution.Carbondioxideisremovedbystrippingoutwithnitrogen. Thefreeamineisdeterminedbytitrationwithhydrochloricacidusingpotentiometricindicationoftheendpoint. NOTE Inaqueouspropan2olthedifferenceinbasicityissufficientforthefreeaminetobedeterminedsepa
21、ratelyfrom anymonochloroacetate,glycolateandbetaine. 5Reagents Duringtheanalysis,unlessotherwisespecified,useonlyreagentsofrecognizedanalyticalgradeandhavebeen checkedinadvanceastonotinterferewiththeanalyticalresults. 5.1 Water,complyingwithgrade3asdefinedinENISO3696. 5.2 Hydrochloricacidstandardvol
22、umetricsolution , c(HCl)=0,1mol/l. 5.3 Sodiumhydroxidesolution , c(NaOH)=0,1mol/l. 5.4 Indicatorsolution ,thymolblue,1g/linethanol. 5.5 Propan2ol/watermixture ,asvolumefractionapproximately1:1. 5.6 Trinbutylamine ,c(C 12 H 27 N)=0,02mol/linpropan2ol. 5.7 Aceticacid ,100%(glacialaceticacid). 5.8 Nitr
23、ogengas ,atleast99,9%.EN13435:2001(E) 5 6Apparatus Ordinarylaboratoryapparatusandthefollowing. 6.1 Potentiometrictitratingapparatus ,comprisingatitratorwithacombinedglass/calomelelectrode( c(LiCl)= 3mol/linethanol),apistonburetteof20mlcapacityandamagneticstirrer(seealsoAnnexB). 6.2 Analyticalbalance
24、 ,accurateto0,1mg. 7 Samplingandsample ThesampleshallbepreparedandstoredinaccordancewithISO607. Solidandpastysamplesshallgentlybemeltedonawaterbathatthelowestpossibletemperature (maximum60 C). 8Procedure 8.1Determination Weighapproximately10gofthesample,tothenearest1mg,intoa250mlglassbeaker.Thendiss
25、olvethe samplein150mlofpropan2ol/watermixture(5.5). Passinnitrogengas(5.8)for5minbymeansofadisposableglasspipette.Allowthetipofthepipettetodip approximately2cmintothesamplesolutionandadjusttheflowofnitrogensothat2to3bubblesemergeper second. Addexactly10mloftrinbutylaminesolution(5.6)andafterfivedrop
26、sofindicatorsolution(5.4). Addsodiumhydroxidesolution(5.3)dropwiseuntiltheindicatorchangesfromyellowtoblueandthenafurther millilitreofsodiumhydroxidesolution(5.3)inexcess. Immersetheelectrode,stirandtitratewiththehydrochloricacidstandardvolumetricsolution(5.2)tothesecond inflexionpoint(seeFigureC.1)
27、. 8.2 Blankdetermination Determinetheblankvalueaccordingtotheproceduregivenin8.1.Useonedropofaceticacid(5.7)insteadofthe sample. 9 Expressionofresults Calculatethecontentoffreeamine, w,expressedasgramsper100g,accordingtotheequation(1): 1000 100 4 3 2 1 m M c V V V V w (1) where: V 1 isthevolumeofhyd
28、rochloricacidstandardvolumetricsolution(5.2)tothesecondinflexionpoint duringtitrationofthesample,inmillilitres; V 2 isthevolumeofhydrochloricacidstandardvolumetricsolution(5.2)tothefirstinflexionpointduring titrationofthesample,inmillilitres; V 3 isthevolumeofhydrochloricacidstandardvolumetricsoluti
29、on(5.2)tothesecondinflexionpoint duringtitrationoftheblanktestsolution,inmillilitres;EN13435:2001(E) 6 V 4 isthevolumeofhydrochloricacidstandardvolumetricsolution(5.2)tothefirstinflexionpointduring titrationoftheblanktestsolution,inmillilitres; c istheamountofsubstanceconcentrationofthehydrochlorica
30、cidstandardvolumetricsolution(5.2),in molesperlitre; M isthemolarmassofthefreeamine,ingramspermole; m isthemassofthesample,ingrams. Theresultshallbegiventoonedecimalplace. 10Precision 10.1 Repeatabilitylimit Theabsolutedifferencebetweentwoindependentsingletestresults,obtainedusingthesamemethodoniden
31、tical testmaterialinthesamelaboratorybythesameoperatorusingthesameequipmentwithinashortintervaloftime, willnotexceedtherepeatabilitylimit, r, inmorethan5%ofcases. TypicalprecisiondataobtainedinaringtestaregiveninannexA. 10.2Reproducibilitylimit Theabsolutedifferencebetweentwoindependentsingletestres
32、ults,obtainedusingthesamemethodonidentical testmaterialindifferentlaboratoriesbydifferentoperatorsusingdifferentequipment,willnotexceedthe reproducibilitylimit, R,inmorethan5%ofcases. TypicalprecisiondataobtainedinaringtestaregiveninannexA. 11 Testreport Thetestreportshallincludethefollowinginformat
33、ion: a) allinformationnecessaryforthecompleteidentificationofthesample; b) areferencetothisEuropeanStandard; c) theresults; d) anyparticularpointsobservedinthecourseofthetest; e) detailsofanyoperationsnotspecifiedinthisEuropeanStandard,andanyoperationsregardedasoptional,as wellasanyincidentslikelyto
34、haveaffectedtheresults.EN13435:2001(E) 7 Annex A (informative) Ringtestresults TheringtestwascarriedoutbytheGermanCommonCommitteeAnalysisofSurfactants“ (GemeinschaftsausschussfrdieAnalytikvonTensiden“). Thesampleusedwasacommerciallyavailablealkyldimethylbetaine(molarmassofthecorrespondingN,N dimethy
35、lcocoamine:226g/mol). TheringtestresultswereevaluatedinaccordancewithISO57252(seeTableA.1). TableA.1Ringtestresults Designation Precisiondata Numberoflaboratoriesparticipating 8 Numberoflaboratoriesnoteliminated 8 Numberofindividualvaluesofalllaboratories 25 Meanvalue, wing/100g 0,24 Repeatabilityst
36、andarddeviation, sring/100g 0,03 Repeatabilitylimit, r,( r=2,8x sr)ing/100g 0,08 Variationcoefficientoftherepeatability,in% 12,1 Reproducibilitystandarddeviation, sRing/100g 0,07 Reproducibilitylimit, R,( R=2,8x s R)ing/100g 0,19 Variationcoefficientofthereproducibility,in% 29,3EN13435:2001(E) 8 Ann
37、ex B (informative) Instrumentsettings Datagivenasfollowsforinstrumentsettingsrefertothedynamicequivalencepointtitration.Theyaresettingsfor theMetrohmTitroprocessor670 1 )andareintendedtoactasaguideline,only: Burettevolume/Resolution: 20ml/2 l Measuredquantity: V Measuringpointdensity: 4 Dosingratefo
38、rincrements: 2ml/min Minimumincrementontitration: 4 l Driftthresholdformeasuredvalueacquisition: 100mV/min Equilibrationtimeformeasuredvalueacquisition: 19s 1 )MetrohmTitroprocessor670isthetradenameofaninstrumentsuppliedbyMetrohmLtd.(CH9101Herisau,Switzerland). Thisinformationisgivenfortheconvenienc
39、eofusersofthisEuropeanStandardanddoesnotconstituteanendorsementby CENoftheinstrumentnamed.EN13435:2001(E) 9 Annex C (informative) Exampleforatypicaltitrationcurveanditsderivative Legend 1 Inflexionpoint1 2 Inflexionpoint2 3 Volumeofhydrochloricacidstandardvolumetricsolutioninmillilitres 4 Voltageinm
40、illivolts FigureC.1Exampleofatypicaltitrationcurve(A)anditsfirstderivative(B)ofanalkyldimethylbetaineEN13435:2001(E) 10 Bibliography ISO57252, Accuracy(truenessandprecision)ofmeasurementmethodsandresults Part2:Basicmethodfor thedeterminationofrepeatabilityandreproducibilityofastandardmeasurementmeth
41、od. J.M.Plantinga,J.J.DonkerbroekandR.Mulder,JAOCS70,97(1993)blankBS EN 13435:2002 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national body responsible for preparing British Standards. It presents the UK view on standards in Europe and at the in
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