1、BRITISH STANDARD BS EN 13405:2002 Surface active agents Determination of dialkyl-tetralins content in linear alkylbenzene by high performance liquid chromatography (HPLC) The European Standard EN 13405:2002 has the status of a British Standard ICS 71.100.40 BS EN 13405:2002 This British Standard, ha
2、ving 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 20 December 2002 BSI 20 December 2002 ISBN 0 580 41022 6 National foreword This British Standard is the offi
3、cial English language version of EN 13405:2002. 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 sec
4、retary. Cross-references The British Standards 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 Cata
5、logue or of British Standards Online. This 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
6、the text; present to the responsible international/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 fr
7、ont cover, an inside front cover, the EN title page, pages 2 to 17 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 EN13405 Decembe
8、r2002 ICS71.100.40 Englishversion SurfaceactiveagentsDeterminationofdialkyltetralinscontent inlinearalkylbenzenebyhighperformanceliquid chromatography(HPLC) AgentsdesurfaceDterminationdelateneuren dialkylttralinesdanslesalkylbenzneslinairespar chromatographieliquidehauteperformance(CLHP) Grenzflchen
9、aktiveStoffeBestimmungdesGehaltesvon DialkyltetralininlinearemAlkylbenzolmittels HochleistungsFlssigchromatographie(HPLC) ThisEuropeanStandardwasapprovedbyCENon23October2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthes
10、tatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslatio
11、n undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portu
12、gal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN13405:2002EE
13、N13405:2002(E) 2 Contents page Foreword3 1 Scope 4 2 Normativereference . .4 3 Principle4 4 Reagents.4 5 Apparatus .4 6 Procedure .5 6.1 Preliminarytest 5 6.2 Calibration 5 6.3 Determination.6 7 Calculation8 8 Precision.8 8.1 General8 8.2 Repeatibilitylimit . 8 8.3 Reproducibilitylimit . .8 9 Testre
14、port . .9 AnnexA(informative)Methodofdeterminationofthecarbonnumberdistributionofthe LABsample (UOPMethod67388). .11 A.1 General11 A.2 Principle11 A.3 Reagents.11 A.4 Apparatus .11 A.5 Procedure .12 A.5.1 Chromatographicconditions 12 A.5.2 Determination.13 A.5.3 Timeforanalysis. .14 A.6 Calculations
15、15 A.7 Precision.15 A.7.1 Repeatability.15 A.7.2 Reproducibility.16 Bibliography 17EN13405:2002(E) 3 Foreword Thisdocument(EN13405:2002)hasbeenpreparedbyTechnicalCommitteeCEN /TC 276,“Surfaceactive agents“thesecretariatofwhichisheldbyAFNOR. ThisEuropeanStandardshallbegiventhestatusofanationalstandar
16、d,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyJune2003,andconflictingnationalstandardsshallbewithdrawnatthelatestby June2003. AnnexAisinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEurope
17、anStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain, Sweden,SwitzerlandandtheUnitedKingdom.EN13405:2002(E) 4 1Scope ThisEuropeanStandardspecifiesamethodforthedeterminationofdialkyltetralins( DAT),bei
18、ng 1,4dialkyl2,3dihydronaphthaleneinlinearalkylbenzene( LAB)intherangeofthemassfractionof0,5%to10%. 2 Normativereference ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetextandthepublicationsarelist
19、edhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). ENISO3696:1995, Waterforanalyticallaboratory
20、useSpecificationandtestmethods(ISO3696:1987). 3Principle Thesampleisanalysedbyisocratichighperformanceliquidchromatography(HPLC)usingamicroparticulate silicastationaryphase,2,2,4methylpentanemobilephaseandultravioletabsorbancedetectionat254 nm. Quantificationismadebyusinga“modified“externalstandardt
21、echnique.Purestandarddialkyltetralins(DAT)are notavailable,thereforethemolarresponseofDATisassumedtobethesameasthecommerciallyavailable tetrahydronaphthalene(THN)usedasexternalstandard. 4Reagents Duringtheanalysis,unlessotherwisespecified,useonlyreagentsofrecognizedanalyticalgradeandhavebeen checked
22、inadvanceastonotinterferewiththeanalyticalresults. 4.1 Water,complyingwithgrade3asdefinedinENISO3696: 1995. 4.2 2,2,4trimethylpentane (isooctane),C 8 H 18 ,HPLCgrade,withawatercontentlessthan100mg/kg. NOTE Careshouldbetakenwhenusingisooctane,whichishighlyflammable. 4.3 Tetrahydronaphthalene(THN),C 1
23、0 H 12 ,minimumpurity96%(determinationbygaschromatographyarea standardtechnique). NOTE Careshouldbetakenwhenusingtetrahydronaphthalenewhichcanbeirritatingtoeyesandskin. 4.4 Hexane,C 6 H 14 . 4.5 Toluene,C 7 H 8 . 5Apparatus Ordinarylaboratoryapparatusandglasswaretogetherwiththefollowing. 5.1 Highper
24、formanceliquidchromatograph ,suitableforanalysisaccordingtotheoperatinginstructions giveninTable1.EN13405:2002(E) 5 5.2 Chromatographiccolumn,normalphase,250 mmlength,4 mminternaldiametercontaining microparticulatesilica. 5.3 Suitablemeans ,fordeterminingpeakarea,e.g.integratororcomputer. 5.4 Dispos
25、ablefilter ,0,5 m mporediameter. 6Procedure 6.1 Preliminarytest Thecolumnlength(1columnor2columnsinseries)andtheflowrateshallbearrangedinordertooptimisethe efficiencyandresolution(seeTable2forcolumndetails).OnewaytotestthisistorunanHPLCchromatogram usingastandardsolutioncontainingapproximately100mgo
26、ftoluene(4.5)and10mgoftetrahydronaphthalene (4.3)( THN)in100mlofhexane(4.4).AnexampleofachromatogramisgiveninFigure1. Donotwashthecolumnswithanypolarsolventotherwisetheoriginalseparationfactorisnottoberestoredany more. Fromthischromatogramdeterminethenetretentiontime( t)andthecapacityfactor( k)ofbot
27、h THNandtoluene andcalculatetherelativeseparationfactor( a ). NOTE TypicalvaluesfortwoLichrosorbSi60columnsand1ml/minflowrateareshowninTable1. Table1Netretentiontimeandcapacityfactorfortolueneand THNfortwoLichrosorbSi 60columnsandaflowrateof1ml/min Reagent Netretentiontime(min) Capacityfactor o t t
28、t - = o t to t k - = Toluene 4,8 0,94 THN 6,3 1,24 NOTE t o isthedurationofelutionatthedeadvolume.Atypicalvalueof t o fornhexaneis 5,1min. Thecalculatedseparationfactor, 1 2 k k = a ,is: 32 1 , = = Tolune THN k k a Areproducibleandcorrect DATanalysisin LABsamplesrequiresthattheHPLCconditionsaresetup
29、sothat a is greaterthanorequalto1,20. 6.2Calibration Prepareasolutionof0,1 g/lof THNin2,2,4trimethylpentane(4.2)byweighing100 mgofthe tetrahydronaphthalene(4.3)tothenearest0,1mgandmakinguptovolumeinan1lvolumetricflaskorbydilution ofamoreconcentratedsolution.EN13405:2002(E) 6 NOTE AreferencesampleofL
30、ABcontaining1,2% DATisavailablefromECOSOL 1) forcheckingthecalibrationofthe method. AnalysethesolutionbyHPLCaccordingtotheconditionsgiveninTable2.Thepeakareaforthe THNpeakis usedforthecalculationinclause7. Ifthemeanmolarmassisunknown,determinethecarbonnumberdistributionofthe LABsampletobeanalysedby
31、agaschromatographypeakareanormalisationtechnique,forexample,asdescribedinAnnexA. Calculatetheaveragemolarmass, M DAT ,ofthe DATinthesampleasfollows: () () = = 15 8 100 i i DAT LAB DAT M i W M (1) where W LAB(i) isthemassfractionof LABatcarbonnumberiofthealkylchain,inpercent; M DAT(i) isthemolarmasso
32、f DAT atcarbonnumberiofthealkylchain,ingramspermole. 6.3Determination Prepareasolutionof10g/lofthesamplein2,2,4trimethylpentane(4.2)byweighing250mgofthesampletothe nearest0,1mgandmakinguptovolumeina25mlvolumetricflask. Filterapproximately5mloftheabovesolutionthroughthedisposablefilter(5.4). Analyset
33、hefilteredsolutionbyHPLCaccordingtotheconditionsgiveninTable2. NOTE AnexampleofachromatogramisgiveninFigure2. Usetangentskimtechniquefordeterminingtheareaofthe DATpeak. 1) ECOSOLisasectorgroupofCEFIC/CESIO(AvenueE.VANNIEUWENHUYSE4,bte2B1 160Brussels,Belgium).EN13405:2002(E) 7 Table2Operatinginstruct
34、ions Column Material Stainlesssteel Lengthxinternaldiameter 250mmx4mm Packing Microparticulatesilica,5 m m Mobilphase Solvent 2,2,4trimethylpentane Flowrate 0,5ml/min1column(seeclause6) 1,0ml/min2columns(seeclause6) Programme Isocraticfor30min Detectorsystem Type Ultravioletabsorbance Wavelength 254
35、nm Temperature Roomtemperature Injectionvolume 20lEN13405:2002(E) 8 7Calculation Determinethecontentof DAT, W DAT ,expressedasmassfractioninpercent,inthesampleasfollows: () () R c THN A A W s c THN s DAT 100 r r = (2) where As isthepeakareafor DAT obtainedbyanalysingthefilteredsolutionbyHPLCin6.3; r
36、 THN(c) isthemassconcentrationof THNinthecalibrationsolutionaspreparedin6.2,ingramsperlitre; R isthemolarmassratio DAT DAT THN M M M 132 = = ; A THN(c) isthepeakareafor THNobtainedbyanalysingthesolutionusingHPLCasspecifiedin6.2,same arbitraryunitsas A s ; r s isthemassconcentrationofthesampleintheso
37、lutionaspreparedin6.3,ingramsperlitre. Theresultshallbegiventoonedecimalplace. 8Precision 8.1General Theprecisiondatawereobtainedbystatisticalevaluationoftheresultsofaninterlaboratorytestcarriedoutby ECOSOL 1) in1992.Fivelaboratoriestookpartinthisinterlaboratorytestwherethreesamplesintherangeof mass
38、fractionsfrom0,5%to3,0%wereanalysed. 8.2 Repeatibilitylimit Theabsolutedifferencebetweentwoindependentsingletestresults,obtainedusingthesamemet hodonidentical testmaterialinthesamelaboratorybythesameoperatorusingthesameequipmentwithinashortintervaloftime, willnotexceedtherepeatabilitylimit, r,inmore
39、than5%ofcases. Inaringtest,thefollowingrepeatabilitylimits, r,wereobtained: lessthanorequalto0,1%atmassfractionsupto2%;and lessthanorequalto0,2%atmassfractionsgreaterthan2%. 8.3Reproducibility limit Theabsolutedifferencebetweentwosingletestresults,obtainedusingthesamemethodonidenticaltestmaterialin
40、differentlaboratoriesbydifferentoperatorsusingdifferentequipment,willnotexceedthereproducibilitylimit, R,in morethan5%ofcases.EN13405:2002(E) 9 Inaringtest,thefollowingreproducibilitylimits,R,wereobtained: lessthanorequalto0,4%atmassfractionsupto0,5%; lessthanorequalto0,6%atmassfractionsgreaterthan0
41、,5%to1,5%;and lessthanorequalto0,8%atmassfractionsgreaterthan1,5%. 9 Testreport Thetestreportshallincludethefollowinginformation: a) allinformationnecessaryforthecompleteidentificationofthesample; b) areferencetothisEuropeanStandard; c) theresultsobtainedandtheunitsinwhichtheyareexpressed; d) anyope
42、rationaldetailsinthisEuropeanStandardtowhichreferenceismade,aswellasanyoperational detailsregardedasoptional,plusdetailsofanyincidentslikelytohaveaffectedtheresults. Key 1 Areaunits 2 Timeinminutes 3 Toluene 4 THN Figure1ExamplechromatogramResolutioncheckEN13405:2002(E) 10 Key 1 Areaunits 2 Timeinmi
43、nutes 3 LAB 4 DAT Figure2ExamplechromatogramECOSOL 1) referencesample( w DAT =1,2%)EN13405:2002(E) 11 Annex A (informative) Methodofdeterminationofthecarbonnumberdistributionofthe LAB sample(UOP 2) Method67388) A.1General ThismethodisfordeterminingtheisomerdistributioninC 15 throughC 20 monosubstitutedlinearalkylbenzenes (LAB)6phenyltridecaneand7phenyltridecaneisomersarenotresolvedfromeachotherandaredeterminedasa composite.Thelowerlimitofdetectionforasinglecomponentis0,1%. Compone
