1、BRITISH STANDARD BS EN 13996:2002 Surface active agents Foaming power and antifoaming power Turbine stirring method The European Standard EN 13996:2002 has the status of a British Standard ICS 71.100.40 BS EN 13996:2002 This British Standard, having been prepared under the direction of the Materials
2、 and Chemicals Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 6 December 2002 BSI 6 December 2002 ISBN 0 580 40937 6 National foreword This British Standard is the official English language version of EN 13996:2002. The UK pa
3、rticipation 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 to its secretary. Cross-references The British Standards which impl
4、ement international or European publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication do
5、es not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/Europe
6、an 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 comprises a front cover, an inside front cover, the EN title page, page
7、s 2 to 15 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 EUROPISCHENORM EN13996 October2002 ICS71.100.40 Englishversion SurfaceactiveagentsFoami
8、ngpowerandantifoamingpower Turbinestirringmethod AgentsdesurfacePouvoirmoussantetpouvoir antimoussantMthodedagitaionparturbine GrenzflchenaktiveStoffeSchumvermgenund EntschumerwirkungVerfahrenmittelsTurbinenrhrgert ThisEuropeanStandardwasapprovedbyCENon9September2002. CENmembersareboundtocomplywitht
9、heCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardex
10、istsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,
11、Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofex
12、ploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN13996:2002EEN13996:2002(E) 2 Contents page Foreword3 1 Scope 4 2 Normativereferences 4 3 Termsanddefinitions. .4 4 Principle5 5 Reagents.5 6 Apparatus .5 7 Sampling.6 8 Preparationoftestsolutions . .6 9 Procedure .7 10
13、 Calculationandexpressionofresults .7 11 Precision.8 12 Testreport 8 AnnexA (informative) Ringtestresult 15EN13996:2002(E) 3 Foreword Thisdocument(EN13996:2002)hasbeenpreparedbyTechnicalCommitteeCEN /TC 276“Surfaceactive agents“,thesecretariatofwhichisheldbyAFNOR. ThisEuropeanStandardshallbegiventhe
14、statusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyApril2003andconflictingnationalstandardsshallbewithdrawnatthelatestby April2003. AnnexAisinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareb
15、oundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain, Sweden,SwitzerlandandtheUnitedKingdom.EN13996:2002(E) 4 1Scope ThisEuropeanStandardspecifiesamethodformeasuringthefoaming
16、powerofasurfaceactiveagentandthe antifoamingpowerofadefoamerwithregardtoafoamingsolution. Themethodisapplicabletoallsurfaceactiveagentsandparticularlytolowfoamingproductsandantifoaming surfaceactiveagents. However,measurementofthefoamingpowerofsolutionsofreadilyhydrolyzableagentsdoesnotgivevalid res
17、ults,asthehydrolysisproductsgatherinthefilmsofliquidandaffectthepersistenceofthefoam. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.
18、For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). EN12829, SurfaceactiveagentsPreparationofwaterwithknownc
19、alciumhardness(ISO2174:1990modified) . ENISO3696, WaterforanalyticallaboratoryuseSpecificationandtestmethods(ISO3696:1987) . ISO607, SurfaceactiveagentsanddetergentsMethodsofsampledivision . ISO1042, LaboratoryglasswareOnemarkvolumetricflasks . ISO4788, LaboratoryglasswareGraduatedmeasuringcylinders
20、 . 3 Termsanddefinitions ForthepurposesofthisEuropeanStandard,thefollowingtermsanddefinitionsapply. 3.1 foam massofgascellsseparatedbythinfilmsofliquidandformedbythejuxtapositionofbubbles,givingagas dispersedinaliquid 3.2 foamingpower abilitytoproducefoam NOTE InthisEuropeanStandard,foamingpowerisch
21、aracterisedbythevolumeoffoamobtainedimmediatelyandthe evolutionofthisvolumeduringthe15minfollowingitsformation,underspecificexperimentalconditions. 3.3 foamingagent substancewhich,whenintroducedintoaliquid,confersonitanabilitytoformfoam 3.4 antifoamingagent defoamer substancewhichpreventstheformatio
22、nofafoamorconsiderablyreducesfoampersistence NOTE Antifoamingpowerisdefinedinrelationtodefinedsolutionsofreferencefoamingagentssuchassaponinor nonylphenolwith10ethyleneoxidemolecules(NP10EO).EN13996:2002(E) 5 InthisEuropeanStandard,antifoamingpowerischaracterisedbytheevolutionofthevolumeoffoamobtain
23、ed immediatelyandthestabilityofthisvolumeduringthe15minfollowingitsformation,asafunctionofthedefoamer contentofthereferencefoamingsolution,underspecificexperimentalconditions.Temperatureisasignificant parameter. 4Principle Afoamisproducedbystirringasurfaceactiveagentsolution,orareferencefoamingsolut
24、ioncontaininga defoamer,usingaturbinestirrer. Thevolumeoffoamobtainedimmediatelyismeasuredandtheevolutionofthisvolumeduringthe15minfollowing itsformationismonitoredtodeterminethefoamingpowerofthesurfaceactiveagent,orthedefoamingpowerof thedefoamerwithregardtothereferencefoamingsolution. NOTE Byvaryi
25、ngthestirringmethods,(forexamplebychangingthestirrer,rotatingspeed,thepresenceofcounterblades, baffle,thestirringduration)theprocedurecanbemodifiedtogiveresultsforawiderangeofapplications. 5Reagents 5.1 Water,grade3,inaccordancewithENISO3696. 5.2 Referencefoamingagent,eithernonylphenol10EO,withaclou
26、dtemperatureof(642)Corsaponin, analyticalgrade. 6Apparatus Ordinarylaboratoryapparatusandthefollowing. NOTE Perfectcleanlinessoftheapparatusisessentialforthesuccessofthetest.Glasswarecanbecleanedbyleavingit incontactwithamixtureofchromicacidsolutionandsulfuricacidsolution.Theapparatusshouldalwaysber
27、insedwithasma ll quantityofthesolutionundertest. 6.1 Laboratoryhighspeedstirrer 1) ,withcontinuouslyvariablespeedsrangingfrom50min 1 to3500min 1 , electronicallycontrolled. 6.2 Centripetalbladestirrer 2) ,with40mmdiameter. 6.3 Baffle,(10 10)mm. 6.4 Stainlesssteelbeaker ,2lcapacitywithaheightof190mma
28、nddiameterof120mm. 6.5 Thermometer,capableofmeasuringarangefrom10Cto40Ctothenearest0,5C. 6.6 Timer,stopwatchorclock,capableofmeasuringtothenearest2s. 6.7 Tachometer,suitableformeasuringthespeedofthecentripetalbladestirrer. 6.8 Graduatedmeasuringcylinders ,capacity2000ml,inaccordancewithISO4788. 6.9
29、Volumetricflask ,capacity1000ml,inaccordancewithISO1042. 1) TurbotestCompact1044fromRaynerisuppliedbyVMI(F.85601Montaigu,France)isanexampleofsuitableapparatus availablecommercially.Thisinformationisgivenfortheconvenienceofusersofthisstandardanddoesnotconstitutean endorsementbyCENofthisapparatus. 2)
30、CentripetalbladestirrerfromRaynerisuppliedbyVMI(F.85601Montaigu,France)isanexampleofsuitableapparatus availablecommercially.Thisinformationisgivenfortheconvenienceofusersofthisstandardanddoesnotconstitutean endorsementbyCENofthisapparatus.EN13996:2002(E) 6 6.10 Waterbath ,capableofmaintainingatemper
31、atureof(201)C. 6.11 Stand,comprisingabaseandverticalrod,withanattachmenttoholdthelaboratoryhighspeedstirrer(6.1) andthecentripetalbladestirrer(6.2)havinganadjustablelaboratoryjacktosupportthestainlesssteel beaker(6.4). 7Sampling PrepareandstorethelaboratorysampleinaccordancewithISO607. 8 Preparation
32、oftestsolutions 8.1 Testsolutionforthefoamingpowertest Preparefromthesurfaceactiveagentlaboratorysampleanaqueoussolutionofthematerialatitsworking strength,usingeitherwater(5.1)saturatedwithairbybubbling,orwaterofknownhardnessinaccordancewith EN12829,previouslyequilibratedatthetesttemperatureof(201)C
33、. NOTE Itisnecessarytomixverygentlytopreventtheformationoffoam.Thetesttemperaturecanbevariedprovidedthat theactualtemperatureisincludedinthetestreport. Keepthistestsolutioninthewaterbath(6.10)atthetesttemperaturewithoutstirringuntilthetestiscarriedout. Theageofthetestsolutionatthetimeofthemeasuremen
34、tshallbenotlessthan30minandnotgreaterthan2h. Theconditionsofthepreparationofthetestsolution(hardnessofwater,temperature)shallbeincludedinthetest report. 8.2 Testsolutionsfortheantifoamingpowertest 8.2.1 Referencefoamingsolution Preparea1g/lreferencefoamingsolutionofthereferencefoamingagent(5.2),usin
35、geitherwater(5.1)saturated withairbybubbling,orwaterofknownhardnessinaccordancewithEN12829,previouslyequilibratedatthetest temperatureof(201)C.Mixverygentlytopreventtheformationoffoam.Recordthereferencefoamingagent usedinthetestreport. Keepthereferencefoamingsolutioninthewaterbath(6.10)atthetesttemp
36、erature.Thereferencefoaming solutionshallnotbekeptmorethanoneday. 8.2.2 Testsolutionsofdefoamingagent Preparetestsolutionsofthedefoamingagentwitharangeofdefoamercontents,bypastingandthendissolution ordispersioninthereferencefoamingsolution(see8.2.1). NOTE Thismixtureshouldbestable(limpidsolutionorst
37、abledispersion).Ifthedefoamerisinsolubleorthedispersionis unstable,thedefoamershouldbedirectlyintroducedintothestainlesssteelbeaker(6.4),atthestartofthestirring. Themixturecanbemadeatalowertemperaturethanthechosentesttemperature.Inthatcasethe900gof solutionshallbebroughtuptothetesttemperatureinthest
38、ainlesssteelbeaker(6.4)usingthewaterbath(6.10). Theageofthetestsolutionatthetimeofmeasurementshallbenotlessthan30minandnotgreaterthan2h. Theconditionsofthepreparationofthetestsolution(referencefoamingagent,hardnessofwater,temperature, procedureusedtointroducethedefoamer)shallbeincludedintestreport.E
39、N13996:2002(E) 7 9Procedure 9.1 Adjustmentoftheapparatus Settheheightofthestand(6.11)usingthelaboratoryjack,thepositionofthebaffle(6.3)andthecentripetalblade stirrer(6.2)sothatitispossibletoadjustthestainlesssteelbeaker(6.4)rapidlyasshowninFigure1. Fillthestainlesssteelbeakerwith900gofwater,placeito
40、nthestandandadjusttheheightasshowninFigure1. Startthelaboratoryhighspeedstirrer(6.1)andadjustitsrotatingspeedto2000min 1 usingthetachometer(6.7). Stopthelaboratoryhighspeedstirrer(6.1),lowerthebeakeranddiscardthewater. 9.2 Determinationoffoamingandantifoamingpower 9.2.1 Foamformation Carefullypour90
41、0gofthetestsolutionforthefoamingpowertest(8.1)respectivelyofthetestsolutionforthe antifoamingpowertest(8.2.2)intothestainlesssteelbeaker(6.4),avoidingtheformationoffoam.Checkthe temperatureand,ifnecessary,adjustitto(201)C,byreturningitintothewaterbath(6.10)toequilibrate. Placethebeakeronthestand,adj
42、ustingthepositionasshowninFigure1. Simultaneouslyturnonthelaboratoryhighspeedstirrer(6.1)at2000min 1 andstartthetimer(6.6).Stopthe stirringafter5min10s. 9.2.2Foam measurement Pourthesolutionandthefoamrapidlyfromthebeakerintoagraduatedcylinder(6.8).byallowingthemtofallat the1600mlmarkandslidedowntheg
43、lasswallasshowninFigure2.Restartthetimer. Thenmeasureandrecordtheupperlevelofthefoam(air/foaminterface)andthelowerlevelofthefoam (foam/solutioninterface)aswellasthefoamvolumetothenearest1mlat0min,1min,2min,3min,5min,10min and15min(eachtothenearest5s)fromtheendofthestirringphase. Attheendofthetest,gentlyagitatethegraduatedcylinderwithacircularmovementandrecordtheresidualfoam
