1、BRITISH STANDARD BS EN 13716:2002 Surface active agents Determination of total base nitrogen Potentiometric titration The European Standard EN 13716:2001 has the status of a British Standard ICS 71.100.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN 13716:2002 This Bri
2、tish Standard, having been prepared under the direction of the Sector Policy and Strategy Committee for Materials and Chemicals, was published under the authority of the Standards Policy and Strategy Committee on 05 March 2002 BSI 05 March 2002 ISBN 0 580 39200 7 National foreword This British Stand
3、ard is the official English language version of EN 13716:2002. 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 req
4、uest 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
5、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 itself confer immunity from legal obligations. a
6、id 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 in the UK. Summary of pages This document c
7、omprises 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 CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN1
8、3716 December2001 ICS71.100.40 Englishversion SurfaceactiveagentsDeterminationoftotalbasenitrogen Potentiometrictitration AgentsdesurfaceDterminationdelateneurenazote totalbasiqueTitragepotentiomtrique GrenzflchenaktiveStoffeBestimmungdesGehaltsan GesamtBasenStickstoffPotentiometrischeTitration This
9、EuropeanStandardwasapprovedbyCENon11November2001. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeo
10、btainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions
11、. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRN
12、ORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN13716:2001EEN13716:2001(E) 2 Contents page Foreword3 1 Scope 4 2 Normativereference . .4 3 Principle4 4 Reagents.4 5 Apparatus .4 6 Samplingand
13、preparationofthesample 4 7 Procedure .5 8 Expressionofresults . .5 9 Precision.6 10 Testreport 6 AnnexA (informative) Instrumentsettings. 7 AnnexB (informative) Typicaltitrationcurve. 8 AnnexC (informative) Resultsofinterlaboratorytest.9EN13716:2001(E) 3 Foreword ThisEuropeanStandardhasbeenpreparedb
14、yTechnicalCommitteeCEN/TC276,“Surfaceactiveagents“,the secretariatofwhichisheldbyAFNOR. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyJune2002,andconflictingnationalstandardsshallbewithdrawnatthelatestby June2002. Accor
15、dingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden, SwitzerlandandtheUn
16、itedKingdom. TheannexesA,BandCareinformative.EN13716:2001(E) 4 1Scope ThisEuropeanStandardspecifiesamethodforthedeterminationoftotalbasenitrogencontentinsurfaceactive agentsbypotentiometrictitration. 2 Normativereference ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpu
17、blications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatestedition
18、ofthe publicationreferredtoapplies(includingamendments). ISO607, SurfaceactiveagentsanddetergentsMethodsofsampledivision . 3Principle Thetotalbasenitrogen,ingramsper100g,isdeterminedbypotentiometrictitrationwithtrifluoromethanesulfonic acidinglacialaceticacid. NOTE Thecontentoftotalbasenitrogenisthe
19、sumofthenitrogeninprimary,secondaryandtertiaryamines. 4Reagents Duringtheanalysis,unlessotherwisespecified,useonlyreagentsofrecognizedanalyticalgradeandhavebeen checkedinadvanceastonotinterferewiththeanalyticalresults. 4.1 Glacialaceticacid ,purity100%. 4.2 Trifluoromethanesulfonicacidstandardvolume
20、tricsolution, c(HSO 3 CF 3 )=0,1mol/l,inglacialacetic acid. NOTE Perchloricacid, c(HClO 4 )=0,1mol/l,inglacialaceticacidcanalsobeused. 4.3 Tris(hydroxymethyl)aminomethane(titrimetricstandard),driedat(1052)C,purity99,9%(minimum). 5Apparatus Ordinarylaboratoryapparatusandthefollowing. 5.1 Potentiometr
21、ictitratingapparatus,comprisingatitratorwithacombinedpHglasselectrode,a20ml plungerburetteandstirrer. NOTE AnexampleofinstrumentsettingsisgiveninannexA. 5.2 Beaker,capacity150ml. 5.3 Analyticalbalance ,accurateto0,1mg. 6 Samplingandpreparationofthesample Thelaboratorysampleofsurfaceactiveagentshallb
22、epreparedandstoredinaccordancewithISO607.EN13716:2001(E) 5 7Procedure 7.1 Factorofthetrifluoromethanesulfonicacidstandardvolumetricsolution Weighapproximately120mg( m 1 )oftris(hydroxymethyl)aminomethane(4.3)tothenearest0,1mgintothebeaker (5.2)anddissolvein80mlofglacialaceticacid(4.1). Immersetheele
23、ctrode,stirandtitratewithtrifluoromethanesulfonicacidstandardvolumetricsolution(4.2). Recordtheconsumptionattheequivalent(inflection)point(volume V 1 );(seeannexB). Calculatethefactor, f,ofthetrifluoromethanesulfonicacidstandardvolumetricsolution(4.2)bytheequation(1): c V M m f 1 1 1000 (1) where m
24、1 isthemassoftris(hydroxymethyl)aminomethane(4.3),ingrams; M isthemolarmassoftris(hydroxymethyl)aminomethane(4.3), M=121,14g/mol; V 1 isthevolumeoftrifluoromethanesulfonicacidstandardvolumetricsolution(4.2)used,inmillilitres; c istheconcentrationoftrifluoromethanesulfonicacidstandardvolumetricsoluti
25、on(4.2),inmolesper litre. 7.2 Titrationofthetotalbasenitrogen Weighfromthesampletobetestedintothebeaker(5.2)aquantity( m 2 )whichcontainsabout0,5mmolto1mmol oftotalbasenitrogentothenearest0,1mg. Dissolvethesamplein80mlofglacialaceticacid(4.1)byslightheatingifneeded. Immersetheelectrode,stirandtitrat
26、ewithtrifluoromethanesulfonicacidstandardvolumetricsolution(4.2). Recordtheconsumptionattheequivalent(inflection)point(volume V 2 );(seeannexB). 8 Expressionofresults Calculatethetotalbasenitrogencontent, w,ingramsper100g,bytheequation(2): 1000 100 2 2 m M f c V w (2) where V 2 isthevolumeoftrifluor
27、omethanesulfonicacidstandardvolumetricsolution(4.2)used,inmillilitres; c istheconcentrationoftrifluoromethanesulfonicacidstandardvolumetricsolution(4.2),inmolesper litre; f isthefactoroftrifluoromethanesulfonicacidstandardvolumetricsolution(4.2)determinedin7.1; M isthemolarmassofnitrogen, M=14g/mol;
28、EN13716:2001(E) 6 m 2 isthemassofthesample,ingrams. Theresultsshallbegiventotwodecimalplaces. 9Precision 9.1 Repeatabilitylimit Theabsolutedifferencebetweentwoindependentsingletestresults,obtainedusingthesamemethodonidentical testmaterialinthesamelaboratorybythesameoperatorusingthesameequipmentwithi
29、nashortintervaloftime, willnotexceedtherepeatabilitylimit r inmorethan5%ofcases. TypicalprecisiondataobtainedinaringtestaregiveninannexC. 9.2Reproducibility limit Theabsolutedifferencebetweentwosingletestresults,obtainedusingthesamemethodonidenticaltestmaterial indifferentlaboratoriesbydifferentoper
30、atorsusingdifferentequipment,willnotexceedthereproducibilitylimit Rin morethan5%ofcases. TypicalprecisiondataobtainedinaringtestaregiveninannexC. 10 Testreport Thetestreportshallincludethefollowinginformation: a) allinformationnecessaryforthecompleteidentificationofthesample; b) themethodused(arefer
31、encetothisEuropeanStandard); c) thetestresults; d) detailsofanyoperationsnotspecifiedinthisEuropeanStandardorintheEuropeanStandardstowhich referenceismade,andanyoperationsregardedasoptional,aswellasanyincidentslikelytohaveaffected theresults.EN13716:2001(E) 7 Annex A (informative) Instrumentsettings
32、 DatagivenaresettingsfortheMetrohmTitroprocessor682 1) andareintendedtoactasaguideline,only. Pause1 20s Electricalinput 1 Titrationrate 1,50ml/min Anticipation 40 Stopvolume 15,00ml Temperature 25C Equivalentpointcriterion 1 1) MetrohmTitroprocessor682isthetradenameofoninstrumentsuppliedbyMetrohmLtd
33、.(CH9101Herisau,Switzerland). ThisinformationisgivenfortheconvenienceofusersofthisEuropeanStandardanddoesnotconstituteanendorsementby CENoftheinstrumentnamed.EN13716:2001(E) 8 Annex B (informative) Typicaltitrationcurve Key 1 Equivalentpoint 2 Consumptionofthestandardvolumetricsolution,inmillilitres
34、 3 Voltage,inmillivolts FigureB.1TypicaltitrationcurveEN13716:2001(E) 9 Annex C (informative) Resultsofinterlaboratorytest Theinterlaboratorytestwascarriedoutin1997bytheAISE/CESIOWG“SurfactantAnalysis“. Thetestsampleswerecommercialproducts(cocofattyamine 2C 2 H 4 O,laurylpropylenediamineand cocofatt
35、yaciddiethanolamide). TableC.1Resultsofinterlaboratorytest Designation Cocofatty amine 2C 2 H 4 O Lauryl propylene diamine Cocofattyacid diethanolamide Numberoflaboratoriesparticipating 14 14 13 Numberoflaboratoriesnoteliminated 14 14 12 Numberofindividualtestresultsofalllaboratoriesoneachsample 42
36、40 36 Meanvalue, w (g/100g) 5,01 11,16 0,27 Repeatabilitystandarddeviation, s r ,ing/100g 0,017 0,026 0,006 Repeatabilitylimiti r ,(r = s r x2,8)in(g/100g) 0,05 0,07 0,02 Reproducibilitystandarddeviation, s R ,ing/100g 0,022 0,073 0,010 Reproducibilitylimit, R, R= ( s R x2,8),ing/100g 0,06 0,20 0,03
37、 Repeatabilitycoefficientofvariation,in% 0,3 0,2 2,3 Reproducibilitycoefficientofvariation, in% 0,4 0,7 3,5BS EN 13716:2002 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
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