EN 13955-2002 en Surface active agents Determination of Krafft point and solubility of ionic surface active agents《表面活性剂 离子型表面活性剂的克拉夫特点和溶解性的测定》.pdf

1、BRITISH STANDARD BS EN 13955:2002 Surface active agents Determination of Krafft point and solubility of ionic surface active agents The European Standard EN 13955:2002 has the status of a British Standard ICS 71.100.40 BS EN 13955:2002 This British Standard, having been prepared under the direction

2、of the Materials and Chemicals Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 20 December 2002 BSI 20 December 2002 ISBN 0 580 41014 5 National foreword This British Standard is the official English language version of EN 139

3、55:2002. 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 to its secretary. Cross-references The British St

4、andards which implement 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. T

5、his publication does 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 in

6、ternational/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 comprises a front cover, an inside front cover, the E

7、N 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 CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN13955 December2002 ICS71.100.40 Englishversion Surfac

8、eactiveagentsDeterminationofKrafftpointand solubilityofionicsurfaceactiveagents AgentsdesurfaceDterminationdupointdeKrafftetde lasolubilitdesagentsdesurfaceioniques GrenzflchenaktiveStoffeBestimmungvonKrafftPunkt undLslichkeitvonionischengrenzflchenaktivenStoffen ThisEuropeanStandardwasapprovedbyCEN

9、on23October2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManageme

10、ntCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandar

11、dsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:rue

12、deStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN13955:2002EEN13955:2002(E) 2 Contents page Foreword3 1 Scope 4 2 Normativereferences 4 3 Termsanddefinitions. .4 4 Principle5 5 Apparatus .5 6 Procedure .6 7 Expressionof

13、results . .7 8 Precision.8 9 Testreport . .8 AnnexA (informative) GraphicalrepresentationoftheKrafftpoint 9EN13955:2002(E) 3 Foreword Thisdocument(EN13955:2002)hasbeenpreparedbyTechnicalCommitteeCEN/TC 276,“Surfaceactive agents“,thesecretariatofwhichisheldbyAFNOR. ThisEuropeanStandardshallbegiventhe

14、statusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyJune2003,andconflictingnationalstandardsshallbewithdrawnatthelatestby June2003. AnnexAisinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesarebo

15、undtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain, Sweden,SwitzerlandandtheUnitedKingdom.EN13955:2002(E) 4 1Scope ThisEuropeanStandardspecifiesamethodforthedeterminationofth

16、esolubilityofionicsurfaceactiveagentsin waterasafunctionofconcentrationandtemperatureandforthedeterminationoftheKrafftpointbygraphical evaluationofthemeasurementresults. Inthetemperaturerangefrom0 Cto90 C,thesolubilityisdeterminedwithoutanylimitationsiftheviscosityof thesolutiondoesnotexceedabout700

17、mPas. Attemperaturesbelow0 C,determinationisonlypossibleifthesolventdoesnotfreeze. Themethodisapplicablebothtopuresurfaceactiveagentsandtotechnicalproductsopticallyclearandnot undulycolouredsolutions. Thesolubilitybothofsolidandliquidsurfaceactiveagentsandofaqueoussolutionsofsurfaceactiveagentsis de

18、terminedbythemethodspecified. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetextandthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofan

19、yofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). ENISO3696, WaterforanalyticallaboratoryuseSpecificationandtestmethods(ISO3696:1987). ISO383, LaboratoryglasswareI

20、nterchangeableconicalgroundjoints . 3 Termsanddefinitions ForthepurposesofthisEuropeanStandard,thefollowingtermsanddefinitionsapply: 3.1 solubility concentrationatthattemperatureatwhichthecloudinessdisappearsagainonheatingacloudysurfaceactive agentsolution NOTE Solutionsofionicsurfaceactiveagentsbec

21、omecloudywhencooledassoonasthesaturationconcentration associatedwithaparticulartemperatureisexceeded.Foragivensurfaceactiveagentconcentration,thetemperatureatwhich cloudinessappearsdecreasesasthesolubilityofthesurfaceactiveagentincreases.Thiscloudinessdisappearsagainifthe solutionisheated. 3.2 Kraff

22、tpoint i)temperatureatwhichthesolubilityofanionicsurfaceactiveagentinwaterchangessuddenlyor ii)temperatureatwhichthesaturationconcentrationofthesurfaceactiveagentreachesitscriticalmicelle concentration(SeeannexA)EN13955:2002(E) 5 4Principle Anaqueoussolutionofthechosenconcentrationofthesampleiscoole

23、dwhilestirringcontinuouslyuntilitis completelycloudy.Thesolutionisthenheatedslowlyatarateof0,5 C/minuntilitisclearagainandthe temperatureatwhichthisoccursisrecorded.TodeterminetheKrafftpoint,themeasurementsobtainedatvarious concentrationsareplottedingraphform.Thisyieldsasolubilitycurvehavingthetwobr

24、anchesaandb,theKrafft point T k beingindicatedbythepointatwhichtheyintercept. 5Apparatus 5.1 TestapparatusaccordingtoFigure1,consistingof: a) thetestvesselwithgroundsocket45/40inaccordancewithISO383; b) theheatingjacketwhichshallbeconnectedtoacirculatingthermostat; c) thestopperwithgroundjoint45/40i

25、naccordancewithISO383,forpreventingthatairisbeingstirredintothe surfaceactiveagentsolution; d) thestraightthermometerwithascaledivisionof0,1 C,alengthofatleast100mmandameasurementrange matchedtothetemperaturetobemeasured. NOTE1 Thethermometercanbeattachedwithadhesivetapetotheguideforthestirrerspindl

26、e(5.1e)ortoastandby meansofaclamp. NOTE2 Thethermometerandthebasketstirrer(5.1f)donotcompletelysealthetestapparatussoastoenableanyair bubblesintroducedintothetestsolutiontoescape.Thestopper(5.1c),however,adequatelyseparatestheliquidaboveitfr om theliquidinthemeasurementchambersothattheliquidabovethe

27、stopperremainsstationaryevenduringvigorousstirringand noaircanpenetrateintothemeasuringchamber; e) thestirrerspindleofstainlesssteel; f) thebasketstirrerofstainlesssteel. 5.2 Analyticalbalance .,accurateto0,1mg. 5.3 Onemarkpipettes withnominalcapacitiesof20mland100ml. 5.4 Conicalflask ,wideneck,with

28、anominalcapacityof250ml.EN13955:2002(E) 6 Dimensionsinmillimetres Key 1 Testvessel 2 Heatingjacket 3 Stopper 4 Thermometer 5 Stirrershaft 6 Basketstirrer 7 Tothermostat 8 Fromthermostat Figure1Testapparatus 6Procedure Solutionswhicharecloudyduetodispersedcontaminantsshallbefiltered,butstepsshallbeta

29、kentoensurethat thetemperatureisabovethesolubilitylimitandnochangeoccursinthesurfaceactiveagentconcentrations. Weighthesample,tothenearest0,01g,intotheconicalflask(5.4),usetheonemarkpipettes(5.3)toadd120ml ofwatergrade3, W A ,inaccordancewithENISO3696andstirintheclosedflask,heatingifnecessary,untilt

30、he sampleiscompletelydissolved.Thentransferthesolutiontothetestvessel(5.1a)andfitthestopper(5.1c), thermometer(5.1d)andbasketstirrer(5.1f)andstirrerspindle(5.1e).EnsurethatthetemperatureofthetestEN13955:2002(E) 7 vesselisaboutthesameasthatofthetestsolution.Thequantityofsolutionshallbesuchthatthestop

31、peris coveredbyalayerofsolutionabove1cmdeep.Removeanyairbubblesinthesolutionintroducedwhenthe surfaceactiveagentisdissolvedorwhiletransferringitbyslowlystirringandheatingthesolution.Thenlowerthe temperatureusingthethermostatuntilthesolutioniscompletelycloudy.Whenthispointisreached,heatthe solutionat

32、arateof0,5 C/minwhilestirringuntilitiscompletelyclearagain. Whenheatingthecloudysurfaceactiveagentsolution,alwaysensurethatequilibriumisestablished,particularlyif therateatwhichthesurfaceactiveagentdissolvesislow. NOTE1 Tocheckthatthesolutionissaturatedattheclearpoint,itcanbekeptforafewminuteswhiles

33、tillcloudyata temperaturejustbelowtheclearpointmeasured.Ifthesolutionbecomesclearatthistemperature,equilibriumhadnotyetbee n established. Iftheequilibriumhasnotbeenestablished,repeatthedeterminationoftheclearpointatalowerheatingrate. Notethetemperatureatwhichthetestsolutionisclearagain. Toplotthesol

34、ubilitycurve,determinethemeasuredpointsforatleastsixdifferentsurfaceactiveagent concentrations,ensuringthatthecurvebranchesaandbinthephasediagramshowninFigureA.1eachcontain threemeasurements.Ifbothcurvesaandbarenotstraightlines,whichisgenerallythecase,determinethe numberofmeasurementsnecessaryforthe

35、solubilitycurvebycarryingoutpreliminaryexperiments.Carryouttwo determinationswhichareindependentofeachotherforeverymeasuredvalue. NOTE2 Aplotofthesolubilitycurvecanbeobtainedmuchmorequicklyifthedeterminationsarecarriedoutsimultaneously inseveraltestvesselswhichcontaindifferentsurfaceactiveagentconce

36、ntrations.Itisadvisabletochoosetheconcentratio ns sothatthemeasuredvaluesareabout5 Cto10 Capart. 7 Expressionofresults RecordtheconcentrationschosenandthemeasuredvaluesobtainedasshowninTable1. Table1 Serial numberof test Sample Massof solvent Sampleconcentration Measured temperature Typeand identifi

37、cation Initialsample mass Massof substance in100gof solvent Massof substance in100gof solution g g g/100g g/100g C ThevalueoftheKrafftpointindegreesCelsiusisgivenbytheinterceptofthetwobranchesaandbofthephase diagramshowninFigureA.1obtainedbyplottingthemeasuredvalueswiththetemperature, T,indegreesCel

38、sius ashorizontalaxisandtheconcentrationing/100gofsolventorasmassfractioninpercentasverticalaxis.EN13955:2002(E) 8 8Precision Theresultsofduplicateandmultipledeterminationsshallnotdifferfromoneanotherbymorethan0,5 C.Ifthisis notthecase,thedeterminationsshallberepeated. 9 Testreport Thetestreportshal

39、lincludethefollowinginformation: a) areferencetothisEuropeanStandard; b) thevaluesandinformationcontainedinTable1; c) theKrafftpoint,indegreesCelsius; d) anydeviationsfromthisEuropeanStandard; e) thedateoftesting.EN13955:2002(E) 9 Annex A (informative) GraphicalrepresentationoftheKrafftpoint Express

40、edintheformofagraph(FigureA.1),theKrafftpointisthetemperature T k atthetriplepointinthephase diagramofthesurfaceactiveagent/watersysteminwhichtheconcentrationandtemperaturearethevariables.In thesimplestcase,thisphasediagramisdividedintothreeregionsasfollows. regionI: thisisaregionoflowconcentrationi

41、nwhichallthesurfaceactiveagentisdissolvedinmonomolecularform; regionII: thisisaregionofhighconcentrationwhichisabovetheKrafftpointandinwhichthesolutioncontainsnotonly truedissolvedmoleculesbutalsomicelles; region III: thisisaregionoffairlyhighconcentrationwhichisbelowtheKrafftpointandinwhichthesurfa

42、ceactiveagent assumeseithertheformofcrystalsorofagel. Theabsolutevaluesatwhichtheconcentrationisdescribedas“low“,“high“and“fairlyhigh“alwaysdependina givensystemonthenatureofthesurfaceactiveagentandnofigurescanthereforebespecifiedhere; ThebranchesaandbofthecurveinFigureA.1arethesolubilitycurveofthes

43、urfaceactiveagentaboveand belowtheKrafftpoint,whereasthebranchcshowsthemicelleformationconcentrationasafunctionof temperature. Key 1 Concentration 2 Temperature FigureA.1Typicalphasediagramofasurfaceactiveagent/watersystem TheKrafftpointofhomologoussurfaceactiveagentsincreaseswiththelengthofthehydrocarbonchain.BS EN 13955:2002 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the independent national body responsible fo