1、BRITISH STANDARD BS EN 12836:2002 Surface active agents Determination of the water number of alkoxylated products The European Standard EN 12836:2002 has the status of a British Standard ICS 71.100.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN 12836:2002 This British
2、 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 11 April 2002 BSI 11 April 2002 ISBN 0 580 39491 3 National foreword This British Standard is t
3、he official English language version of EN 12836:2002. It supersedes DD ENV 12836:2001 which is withdrawn. 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 represen
4、ted on this committee 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 entitled “International Standards Correspondence
5、 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. Compliance with a British Standard does not of itse
6、lf confer immunity from legal obligations. 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 them
7、 in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 9 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 CommentsEUROPE
8、ANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN12836 March2002 ICS71.100.40 SupersedesENV12836:1999 Englishversion SurfaceactiveagentsDeterminationofthewaternumberof alkoxylatedproducts AgentsdesurfaceDterminationdunombredeaudans lesproduitsalkoxyls GrenzflchenaktiveStoffeBestimmungderWasserzahl vonalko
9、xyliertenProdukten ThisEuropeanStandardwasapprovedbyCENon3January2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnat
10、ional standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusas
11、the official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALIS
12、ATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN12836:2002EEN12836:2002(E) 2 Contents page Foreword3 Introduction .4 1 Scope 5 2 Normativereferences 5 3 Termanddefi
13、nition. .5 4 Principle5 5 Reagents.5 6 Apparatus .6 7 Preparationoftestsample 6 8 Procedure .6 9 Expressionofresults . .7 10 Precision.7 11 Testreport 7 AnnexA(informative) Interlaboratorytestresults .8 Bibliography 9EN12836:2002(E) 3 Foreword ThisdocumentEN12836:2002hasbeenpreparedbyTechnicalCommit
14、teeCEN/TC276“Surfaceactiveagents“, thesecretariatofwhichisheldbyAFNOR. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbySeptember2002,andconflictingnationalstandardsshallbewithdrawnatthe latestbySeptember2002. Thisdocument
15、supersedesENV 12836:1999. SignificanttechnicaldifferencesbetweenthisstandardandENV12836:1999arethedeletionofannexesBandC andthemodificationofannexArelatingofprecisiondata. AnnexAisinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesarebo
16、undtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain, Sweden,SwitzerlandandtheUnitedKingdom.EN12836:2002(E) 4 Introduction H.L.Greenwald,G.L.BrownandM.N.Fineman1andW.C.Griffin2
17、proposedthesocalledwaternumberasan easytomeasurecriterionforthehydrophiliclipophilicbalance(HLB)valueofsurfaceactiveagentsandoils.The methoddescribedwasbasedonadioxane/benzenemixture.Inthefollowingtestmethodnoxiousbenzenehas beenreplacedbytoluene.Thewaternumberisnotalteredbythischange. Itisalsopossi
18、bletoreplacedioxanewithtriethyleneglycoldimethylether.This,however,resultsinachangeinthe absolutenumericalvalueofthewaternumber,especiallyforhighmolecularmassnonionics(forexampleethylene oxide/propyleneoxide(EO/PO)blockpolymers).EN12836:2002(E) 5 1Scope ThisEuropeanStandardspecifiesthedeterminationo
19、fthewaternumberofethoxylatedproductsuptoabout70% ethyleneoxide.EO/POblockpolymerswithwaternumbershigherthanabout23becomehardtointerpret. NOTE Thevaluesobtainedbythismethodarenotcompletelyidenticalwiththewaternumberobtainedindioxane,in particularwaternumbershigherthan23. 2 Normativereferences ThisEur
20、opeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenin
21、corporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). ENISO3696, WaterforanalyticallaboratoryuseSpecificationandtestmethods(ISO3696:1987). ENISO4320, NonionicsurfaceactiveagentsDeterminationofcloudpointindexVolumetricmethod (
22、ISO4320:1977). 3 Termanddefinition ForthepurposesofthisEuropeanStandard,thefollowingtermanddefinitionapply. 3.1 waternumber numberofmillilitresofwaterrequiredtobringaboutapersistentturbidityinasolutionwithaspecifiedvolumeofa solventmixtureataconstanttemperature NOTE Resultsofwaternumbersareverysensi
23、tivetotemperaturedeviations. 4Principle Toasolventmixtureconsistingofdioxane/toluene(ortriethyleneglycoldimethylether/toluene)inwhichthesample isdissolvedtogiveaclearsolution,waterisaddedatatemperatureof(251)Cuntilapersistentturbidity appears. 5Reagents Allreagentsshallbeofarecognizedanalyticalgrade
24、andthewaterusedshallconformtograde3,inaccordance withENISO3696. 5.1 Solventmixture ,withamassfractionof97,0%dioxaneand3,0%toluene. NOTE Ifdioxaneisnotwantedorcannotbeused,itmaybereplacedbytriethyleneglycoldimethylether(purity 98%).EN12836:2002(E) 6 6Apparatus Ordinarylaboratoryapparatusandthefollowi
25、ng: 6.1 100mlconicalflask withglassstopper. 6.2 2x50mlsemimicroburettes orthermostatable(doublewalled)titrationequipment. 6.3 Doublewalledbeaker (seeFigure1). 6.4 Thermostatwithcirculatingpump ,adjustableto0,1C. 6.5 Analyticalbalance ,accurateto0,01g. 6.6 Magneticstirrer. Dimensionsinmillimetres Key
26、 1 Directionofwatercirculation Figure1DoublewalledbeakerinaccordancewithENISO4320 7 Preparationoftestsample Forthedeterminationofthewaternumber,100%activesubstanceshallbeused.Ifthesamplecontainssolvent,it shallbecompletelyremoved(bydistillationforexamplerotatingevaporation). 8Procedure 8.1 Dissoluti
27、onofthesample Weigh(1,000,01)gofsubstance(sample)intoadryflask(6.1)withgroundglassjointordirectlyintothe doublewalledbeaker(6.3).Intothisflaskorbeakerpour30,0 mlofsolventmixture(5.1)froma50ml semimicroburette(6.2)whosestoragebottlestandsinathermostatedbathat(251)C.Whenusingaconical flaskwithagroundg
28、lassjointcloseitwithaglassstopperanddissolvethesample,ifnecessarybyheatingslightly andbriefly.Thetemperaturetostabilizeat(251)C.EN12836:2002(E) 7 8.2 Determinationofwaternumber Pourtheclearsolutionintothedoublewalledbeaker(6.3),maintainedat(251)C,stirwithmagneticstirrer (6.6),coveredwithapolyethylen
29、ecoveranddropinwateratarateof1ml/minto2ml/minfromasecond semimicroburette(6.2),whosestoragebottlealsostandsinathermostatedbathat(251)C,untilturbidity persistsfor2min. 9 Expressionofresults Reporttheresultasthemeanoftwotitrationscalculatedtothenearest0,1ml. 10Precision 10.1Repeatability Theabsolutedi
30、fferencebetweentwoindependentsingletestresults,obtainedusingthesamemethodonidentical testmaterialinthesamelaboratorybythesameoperatorusingthesameequipmentwithinashortintervaloftime, willnotexceedtherepeatabilitylimit, r,inmorethan5%ofcases. TypicalprecisiondataobtainedinaringtestaregiveninannexA. 10
31、.2Reproducibility Theabsolutedifferencebetweentwoindependentsingletestresults,obtainedusingthesamemethodonidentical testmaterialindifferentlaboratoriesbydifferentoperatorsusingdifferentequipment,willnotexceedthe reproducibilitylimit, R,inmorethan5%ofcases. Typicalprecisiondataobtainedinaringtestareg
32、iveninannexA. 11 Testreport Thetestreportshallincludethefollowinginformation: a) allinformationnecessaryforthecompleteidentificationofthesample; b) areferencetothisEuropeanStandard; c) themethodandthesolvantused(dioxaneortriethyleneglycoldimethylether); d) thetestresults; e) thetestdate; f) detailso
33、fanyoperationsnotspecifiedinthisEuropeanStandardandanyoperationsregardedasoptional,as wellasanyincidentswhichmayhaveinfluencedtheresults.EN12836:2002(E) 8 Annex A (informative) Interlaboratorytestresults Theseprecisiondatawereobtainedbyaringtestcarriedoutonfivesamples.Theevaluationwasperformedin acc
34、ordancewithISO57252: TableA.1Samples Sample Description A Ethoxylatednonylphenol2EO B Ethoxylatednonylphenol4EO C Ethoxylatednonylphenol6EO D Ethoxylatednonylphenol8EO E Ethoxylatednonylphenol10EO TableA.2Precisiondata Designation SampleA SampleB SampleC SampleD SampleE Numberofparticipatinglaborato
35、ries 4 4 4 4 4 Numberoflaboratoriesnoteliminated 4 4 4 4 4 Numberofindividualmeasurementofalllaboratories 9 8 10 8 9 Meanvalue(ml) 17,08 19,77 21,81 23,40 24,35 Repeatabilitystandarddeviation s r (ml) 0,06 0,06 0,06 0,06 0,06 Repeatabilitylimit, r,( r=2,8x s r )(ml) 0,17 0,17 0,17 0,17 0,17 Repeatab
36、ilitycoefficientofvariation(%) 1,00 0,86 0,78 0,73 0,70 Reproducibilitystandarddeviation s R (ml) 0,44 0,46 0,44 0,75 0,55 Reproducibilitylimit, R,( R=2,8x s R )(ml) 1,23 1,28 1,23 2,10 1,54 Reproducibilitycoefficientofvariation(%) 7,20 6,47 5,64 8,97 6,32EN12836:2002(E) 9 Bibliography 1 H.L.Greenwa
37、ld;G.L.BrownetM.NFineman:Analyt.Chemistry28(1956),1693. 2 W.CGriffin:Journ.Soc.Cosm.Chem.1(1949),311. 3ISO 57252, Accuracy(truenessandprecision)ofmeasurementmethodsandresultsPart2:Basic methodforthedeterminationofrepeatabilityandreproducibilityofastandardmeasurementmethod.BS EN 12836:2002 BSI 389 Ch
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