EN 14207-2003 en Water quality - Determination of epichlorohydrin《水质 表氯醇的测定》.pdf

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1、BRITISH STANDARD BS EN 14207:2003 BS 6068-2.81:2002 Water quality Determination of epichlorohydrin The European Standard EN 14207:2003 has the status of a British Standard ICS 13.060.50 BS EN 14207:2003 This British Standard was published under the authority of the Standards Policy and Strategy Comm

2、ittee on 15 May 2003 BSI 15 May 2003 ISBN 0 580 41846 4 National foreword This British Standard is the official English language version of EN 14207:2002. The UK participation in its preparation was entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH/3/2, Physical chemical prese

3、nt 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 front cover, an i

4、nside front cover, the EN title page, pages 2 to 18, an inside back cover 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 EN14207

5、April2003 ICS13.060.50 Englishversion WaterqualityDeterminationofepichlorohydrin QualitdeleauDosagedelpichlorhydrine WasserbeschaffenheitBestimmungvonEpichlorhydrin ThisEuropeanStandardwasapprovedbyCENon17January2003. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheco

6、nditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).

7、Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Irel

8、and,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeans

9、reserved worldwideforCENnationalMembers. Ref.No.EN14207:2003EEN14207:2003(E) 2 Contents page Foreword3 Introduction .3 1 Scope 3 2 Normativereferences 3 3 Principle4 4 Interferences/Losses .4 5 Reagents.4 6 Apparatus .6 7 Sampling.7 8 Procedure .7 9 Calibration 8 10 Calculationoftheresults. .10 11 E

10、xpressionofresults 10 12 Testreport 10 13 Precisiondata. 11 AnnexA (informative) Exampleofsorbents. 12 AnnexB (informative) Examplesofrecommendedcapillarycolumns13 AnnexC (informative) Examplesofchromatogramsandspectra .14EN14207:2003(E) 3 Foreword ThisdocumentEN14207:2003hasbeenpreparedbyTechnicalC

11、ommitteeCEN/TC230“Wateranalysis”,the secretariatofwhichisheldbyDIN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyOctober2003,andconflictingnationalstandardsshallbewithdrawnatthelatest byOctober2003. AnnexesA,BandCarein

12、formative. WARNINGPersonsusingthisstandardshouldbefamiliarwithnormallaboratorypractice.Thisstandard doesnotproposetoaddressallofthesafetyproblems,ifany,associatedwithitsuse.Itisthe responsibilityoftheusertoestablishappropriatesafetyandhealthpracticesandtoensurecompliance withanynationalregulatorycon

13、ditions. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal, Slov

14、akia,Spain,Sweden,SwitzerlandandtheUnitedKingdom. Introduction Itishighlyrecommendedthatthetestdescribedinthisstandardbecarriedoutbysuitablyqualifiedstaff. Itshouldbeinvestigatedwhetherandtowhatextentparticularproblemswillrequirethespecificationofadditional marginalconditions. 1Scope ThisEuropeanSta

15、ndardspecifiesamethodforthedeterminationofepichlorohydrinindrinkingwaterandwater usedfordrinkingwaterprocessing.Accordingtothegivenprocedure,thelimitofdeterminationinroutineanalysis isabout0,5g/l 1) .Thelimitofdeterminationcanbeloweredtomonitor0,1g/l. 2 Normativereferences ThisEuropeanStandardincorp

16、oratesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyame

17、ndmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). EN256671, WaterqualitySamplingPart1:Guidanceonthedesignofsamplingprogrammes(ISO5667 1:1980). EN256672, WaterqualitySamplingPart2:Guidanceonsamplingtechniques(ISO56672:1991) . 1) Thisvaluewas

18、checkedinaninterlaboratorytrial.EN14207:2003(E) 4 ENISO56673, Waterquality Sampling Part3:Guidanceonthepreservationandhandlingofsamples (ISO56673:1994) . ISO56675, WaterqualitySamplingPart5:Guidanceonsamplingofdrinkingwaterandwaterusedforfood andbeverageprocessing . ISO84661,Waterquality Calibration

19、andevaluationofanalyticalmethodsandestimationofperformance characteristicsPart1:Statisticalevaluationofthelinearcalibrationfunction . 3Principle Solidphaseextractionofepichlorohydrinfromthedrinkingwatersamplefollowedbygaschromatographyusinga massspectrometer(MS)asdetector.Alternatively,anelectroncap

20、turedetector(ECD)canbeused. 4 Interferences/Losses 4.1Interferencesduringsampling Inordertoavoidinterferences,withdrawthesampleaccordingtoclause7,takingintoaccounttheinformation giveninEN256671,EN256672andENISO56673. Inordertoavoidlossesduetotheeasydecompositionofepichlorohydrin,avoidunnecessarystor

21、ageandanalyse thesampleassoonaspossibleaftersampling.Ifstorageisunavoidable,storebetween2Cand5Cuntilsample pretreatment. 4.2Interferencesduringenrichment Thecommerciallyavailableadsorbancematerialsareoftenofvaryingquality.Considerablebatchtobatch differencesinqualityandselectivityofthesematerialsare

22、possible.Performcalibrationandanalysiswithoneand thesamebatchofmaterial.Makesuretoavoidanylosseswhenremovingtheresidualwaterintheadsorbance material(8.1.2). 4.3Interferencesinthegaschromatographyandmassspectrometry Settheoperationalconditionsinaccordancewiththemanufacturersinstructions.Checktheseset

23、tingsatregular intervals. Generalinterferences,causedbytheinjectionsystemcanbeeliminatedwiththehelpofspeciallaboratory experienceandtheinstrumentsmanuals. Thestabilityoftheanalyticalsystemshouldbechecked(forexamplebyapplicationofameasuringstandard). 5Reagents Usereagentsofthereagentgrade“forresidual

24、analysis”orequivalentasfarasavailable.Impuritiesinthe reagentsandinthewatercontributingtotheblankshallbenegligiblylow.Checktheblankregularly,especially priortotheuseofanewbatch. 5.1Water Usedoubledistilledwaterorwaterofcomparablepurity.EN14207:2003(E) 5 5.2Operatinggasesforthegaschromatography/masss

25、pectrometry/ECD , accordingtothe manufacturersinstructions.Theoperatinggasesshallbeofhighpurity. 5.3Nitrogen, highpurity,minimum99,996%(v/v),forremovalofwaterinthesorbentpackingaftersample extraction. 5.4Solvents 5.4.1Diisopropylether, C 6 H 14 O. 5.4.2Methanol, CH 3 OH,asconditioningagent. 5.5Reduc

26、ingagents, e.g.sodiumthiosulfate(Na 2 S 2 O 3 ). 5.6Epichlorohydrinstocksolution Weigh50mgofepichlorohydrin(C 3 H 5 ClO)intoa100mlvolumetricflaskcontainingdiisopropylether(5.4.1)upto theneckandfilltomarkwithdiisopropylether(5.4.1).Storethesolutioninarefrigeratorbetween2Cand5C. Theshelflifeofthesolut

27、ionislimited(about6months).Checktheconcentrationpriortoanalysisinordertomake surethatnosignificantdifferencesarise. 5.7Internalstandardstocksolution Theinternalstandardshallnotbepresentinthesampleitself. 5.7.1 13 C 3 epichlorohydrinstocksolutionforGCMS Thissolutionmaybepurchasedascertifiedsolution(e

28、.g.ataconcentrationof100g/mlinnonane)orpreparedfrompure standardmaterialaccordingto5.6.Neveraddmorethan100lofadilutedinternalstandardstocksolutionindiisopropyleth er (5.4.1)to100mlofthewatersample,agreatervolumemayresultinpoorrecovery. NOTE Thepeakareaoftheinternalstandardshouldbeequivalenttothatof1

29、g/loftheanalyte.Forexample,ifthecon centrationofthestocksolutionis100g/mlof 13 C3epichlorohydrin innonane,100l,dissolvedin1mldiisopropylether(5.4.1) isrequiredtoproducea10g/mlspikingsolutionfromwhichavolumeof10lcanbeinjecteddirectlyinto100mlofwater (5.1). 5.7.2Ethyl2chloropropionate(C 5 H 9 ClO 2 )s

30、tocksolutionforGCECD(see5.6) 5.8Epichlorohydrinspikingsolutions Usingstockstandardsolution(5.6),preparespikingsolutionsbyappropriatedilutionina100mlvolumetricflask containingdiisopropylether(5.4.1).Preparethespikingsolutionsatconcentrationssuchthattheaqueous calibrationsolutions(5.9)willcoverthework

31、ingrangeoftheanalyticalsystem.Storespikingsolutionsina refrigeratorbetween2Cand5C.Letthesolutionsadjusttoroomtemperaturebeforepreparingcalibration solutions.Thestoragetimeshallnotexceedonemonth. 5.9Epichlorohydrincalibrationsolutionsforthemultipointcalibration Prepareaqueouscalibrationsolutionsfromt

32、hespikingsolutions(5.8)byinjectionofanappropriatevolume(e.g. 10l)ofthespikingsolutiondirectlyinto100mlofwater(5.1).However,donotusemorethan100lofaspiking solutiontoproducethecalibrationsolutions.Mixtheaqueouscalibrationsolutionsthoroughlybyinvertingtheflask severaltimes.Preparefivedifferentconcentra

33、tionlevels.Preparecalibrationsolutionsfreshdaily. Table1givesanexampleforadilutionscheme.EN14207:2003(E) 6 Table1Dilutionscheme Millilitreof5.6addedto100ml 5.4.1 Analyteconcentrationinthe spikingsolutioninmilligramper millilitre Concentration(inmicrogramperlitre)inthe calibrationsolution (10lofthesp

34、ikingsolutionaddedto100ml water) 0,2 0,001 0,1 0,6 0,003 0,3 1,0 0,005 0,5 1,4 0,007 0,7 1,8 0,009 0,9 IfthedesiredmeasuringrangediffersfromthatofTable1,differentsolutionratiosshouldbetaken. 5.10Solidphasematerial Solidphasematerialonstyrenedivinylbenzenecopolymerbasisisnormallyused,merciallyavailab

35、le cartridgesoradequatelyglasscolumnsfilledwithaminimumpackingof200mgofthesorbent(seeannexA).A recoveryof 6Apparatus 6.1Generalrequirements Equipmentorpartsofitwhichmaycomeintocontactwiththewatersampleortheextractshouldbefreefrom interferingcompounds. 6.2Samplebottles, preferablybrownglass,500ml,wit

36、hglassstoppersorPTFElined(PTFE=polytetrafluoro ethene)screwcaps. 6.3Solidphaseextractioncartridges, see5.10. 6.4Vacuumorpressureassembly ,fortheextractionstep. 6.5Volumetricflaskswithinertstopper. 6.6Vials, suitableforautomaticormanualinjection,preferablybrownglass,withPTFElinedsepta. 6.7Capillaryga

37、schromatograph, equippedwithamassspectrometerasdetectororanECD.Preferablyuse anautosamplerforsampleinjection.Foroperationalaspectsoftheinstrumentsthemanufacturersinstructions shouldbefollowed. 6.8Capillaryinjector, forsplitsplitless,coldoncolumnorprogrammedtemperaturevaporizing(PTV)injection. 6.9Cap

38、illarycolumnsforgaschromatography, examplesseeannexB. 6.10 Injectionsyringes,nominalcapacity5lor10l.EN14207:2003(E) 7 7Sampling CollectsamplesaccordingtoEN256671,EN256672,ENISO56673,andISO56675. Useforsamplingcarefullycleaned,preferablybrownglassbottles,500ml.Fillthebottlescompletelywiththe watertob

39、eexamined.Treatandanalysethesamplesassoonaspossibleaftersampling. Ifstorageis unavoidable,storethesampleinarefrigeratorbetween2Cand5Cpriortoanalysis. Sampleswhichareknownorsuspectedtocontainfreechlorineoranotheroxidizingdisinfectantshallbepreserved withareducingreagent.Addapproximately100mg/lsodiumt

40、hiosulfate(5.5)oranotherreducingreagenttothe samplebottlepriortocollectingthesample.Afterfilling,sealthebottleandshakemanuallyuntilreagentis dissolved. 8Procedure 8.1Solidphaseextraction 8.1.1 Conditioningofthesolidphasematerial Thefollowingprocedureisdescribedforcommerciallyavailable3mland6mlcartri

41、dges(sorbentmass200mg). Rinsethecartridgewith5mlofdiisopropylether(5.4.1).Letthecartridgedrainafterrinsing.Subsequently,rinse thecartridgewith5mlofmethanol(5.4.2),lettingthecartridgedrainafterrinsing.Thesorbentbedshouldnotbe allowedtorundrybetweenthisstepandthenextconditioningstep.Ifthebedfallsdry,r

42、epeatrinsingwith methanol.Pass5mlofwater(5.1)throughthecartridge,andmakesurethatthesorbentpackinginthecartridge doesnotrundry.Retainthewaterinthecartridge(waterleveljustabovethepacking)tokeepthesorbent activated. 8.1.2 Sampleextraction Starttheextractionimmediatelyafterconditioning.Makesurethatnoairbubblesaretrappedinthesorbentbed whenchangingfromconditioningtoextraction.Maintainthesorbentmaterialinthecartridgeimmersedinwaterat alltimes. Filla100mlvolumetricflasktothemarkwithsample.Addaninternalstandard(5.7)andmixthoroughly.Letthis samplerunthroughthecolumn,conditionedasgivenin8.1.1,