EN ISO 15682-2001 en Water Quality - Determination of Chloride by Flow Analysis (CFA and FIA) and Photometric or Potentiometric Detection《水质 用流量分析(CFA和FIA)法和光度或电势检查法测定氯化物》.pdf

1、BRITISH STANDARD BS EN ISO 15682:2001 BS 6068-2.71:2000 Incorporating Amendment No.1 to BS ISO 15682:2000 (renumbers the BS ISO as BS EN ISO 15682:2001) Water quality Determination of chloride by flow analysis (CFA and FIA) and photometric or potentiometric detection The European Standard EN ISO 156

2、82:2001 has the status of a British Standard ICS 13.060.50 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN ISO 15682:2001 This British Standard, having been prepared under the direction of the Health and Environmental Sector Committee, was published under the authority of

3、 the Standards Committee and comes into effect on 15 October 2000 BSI 26 November 2001 ISBN 0 580 36300 7 National foreword This British Standard is the official English language version of EN ISO 15682:2001(as corrected). It is identical with ISO 15682:2000. The UK participation in its preparation

4、was entrusted by Technical Committee EH/3, Water quality, to Subcommittee EH/3/2, Physical, chemical and biochemical methods, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its secretary. Cross-references The British Standards

5、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 the BSI Standards Electronic Catalogue. A British Standard doe

6、s 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. aid enquirers to understand the text; present to the responsibl

7、e 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 inside front cover, t

8、he EN ISO title page, the EN ISO foreword page, the ISO title page, pages ii to v, a blank page, pages 1 to 21, the annex ZA page, and 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 publicatio

9、n Amd. No. Date Comments 13448 26 November 2001 Implementation of the European StandardEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM ENISO15682 August2001 ICS13.060.50 Englishversion WaterqualityDeterminationofchloridebyflowanalysis(CFA andFIA)andphotometricorpotentiometricdetection(ISO 15682:2000)

10、 QualitdeleauDosageduchlorureparanalyseenflux (CFAetFIA)etpardtectionphotomtriqueou potentiomtrique(ISO15682:2000) WasserbeschaffenheitBestimmungvonChloridmittels Flieanalyse(CFAundFIA)undphotometrischeroder potentiometrischerDetektion(ISO15682:2000) ThisEuropeanStandardwasapprovedbyCENon18June2001.

11、 CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyC

12、ENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustri

13、a,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brus

14、sels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENISO15682:2001ECORRECTED20011107 Foreword Thete xto ftheI nternational Standard from TechnicalCo mmittee ISO/TC147 , Waterquali ty oftheInternationalOrganizationforStandardization(ISO)hasbeenta

15、kenoverasan EuropeanS tandard by Technical CommitteeCEN/ TC23 0,Waterana lysis,th e Secretariatof whichisheldbyDIN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublication ofanidenticaltextorbyendorsement,atthelatestbyFebruary2002,andconflictingnational standardsshallbewithd

16、rawnatthelatestbyFebruary2002. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsof thefollowingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium, CzechRepublic,Denmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy, Luxembourg,Netherlands,Norway,Portu

17、gal,Spain,Sweden,SwitzerlandandtheUnited Kingdom. NOTE:NormativereferencestoInternationalStandardsarelistedinannexZA(normative). ENISO15682:2001Referencenumber ISO15682:2000(E) INTERNATIONAL STANDARD ISO 15682 Firstedition 2000-07-15 WaterqualityDeterminationofchloride byflowanalysis(CFAandFIA)and p

18、hotometricorpotentiometricdetection QualitdeleauDosageduchlorureparanalyseenflux(CFAetFIA)et pardtectionphotomtriqueoupotentiomtriqueii ENISO15682:2001 iii Contents Page Foreword.iv Introduction.v 1 Scope1 2 Normativereference1 3 Determinationofchloridebyflowanalysis(FIAandCFA)withphotometricdetecti

19、on1 4 Determinationofchloridebyflowanalysis(FIAandCFA)withpotentiometricdetection7 5 Expressionofresults10 6 Testreport.10 AnnexA(informative)Performancecharacteristics12 AnnexB(informative)Examplesofflowdiagrams14 AnnexC(informative)Determinationofchloridebyflowanalysis(FIAandCFA)andpotentiometric

20、detectionwithasinglecalibrationfunctionfortherange10mg/lto1000mg/l20 Bibliography21 ENISO15682:2001iv Foreword ISO(theInternationalOrganizationforStandardization)isaworldwidefederationofnationalstandardsbodies(ISO memberbodies).TheworkofpreparingInternationalStandardsisnormallycarriedoutthroughISOte

21、chnical committees.Eachmemberbodyinterestedinasubjectforwhichatechnicalcommitteehasbeenestablishedhas therighttoberepresentedonthatcommittee.Internationalorganizations,governmentalandnon-governmental,in liaisonwithISO,alsotakepartinthework.ISOcollaboratescloselywiththeInternationalElectrotechnical C

22、ommission(IEC)onallmattersofelectrotechnicalstandardization. InternationalStandardsaredraftedinaccordancewiththerulesgivenintheISO/IECDirectives,Part3. DraftInternationalStandardsadoptedbythetechnicalcommitteesarecirculatedtothememberbodiesforvoting. PublicationasanInternationalStandardrequiresappro

23、valbyatleast75%ofthememberbodiescastingavote. AttentionisdrawntothepossibilitythatsomeoftheelementsofthisInternationalStandardmaybethesubjectof patentrights.ISOshallnotbeheldresponsibleforidentifyinganyorallsuchpatentrights. InternationalStandardISO15682waspreparedbyTechnicalCommitteeISO/TC147,Water

24、quality, SubcommitteeSC2,Physical,chemicalandbiochemicalmethods. AnnexesA,BandCofthisInternationalStandardareforinformationonly. ENISO15682:2001 v Introduction Methodsusingflowanalysisautomatizewetchemicalproceduresandareparticularlysuitablefortheprocessingof manyanalytesinwaterinlargesampleseriesat

25、ahighanalysisfrequency(upto100samplesperhour). Differentiationisrequiredbetweenflowinjectionanalysis(FIA)1,2,andcontinuousflowanalysis(CFA)3.Both methodssharethefeatureofautomaticdosageofthesampleintoaflowsystem(manifold)wheretheanalytesin thesamplereactwiththereagentsolutionsontheirwaythroughtheman

26、ifold.Thesamplepreparationmaybe integratedinthemanifold.Theamountofreactionproductismeasuredinaflowdetector(e.g.photometer,orion- selectiveelectrode).Thedetectorproducesasignalfromwhichtheconcentrationoftheparameteriscalculated. Itshouldbeinvestigatedwhetherandtowhatextentparticularproblemswillrequi

27、rethespecificationofadditional marginalconditions. ENISO15682:2001ENISO15682:2001INTERNATIONALSTANDADR ISO28651:(0002)E1 WaterqualityDeterminationofchloridebyflowanalysis(CFA andFIA)andphotometricorpotentiometricdetection 1 Scope ThisInternationalStandardspecifiestwomethodsforthedeterminationofchlor

28、idebyflowanalysis.Thetwobasic methodsarecoveredinseparateclausesasfollows: a) Clause3:Determinationofchloridebyflowanalysisandphotometricdetection. b) Clause4:Determinationofchloridebyflowanalysisandpotentiometricdetection. Bothmethodsareapplicabletotheanalysisofwaterandwastewater(includingleachates

29、)containingchloridein theconcentrationrangefrom1mg/lto1000mg/l.Onacase-by-casebasistherangeoftheanalysiscanbe changed. Afterdilution,sampleswithachlorideconcentration1000mg/lcanalsobeanalysed. Themethodwithpotentiometricdetectionisalsoapplicabletoturbidand/orcolouredsamples. NOTE Fromtheecologicalpo

30、intofview,thepotentiometricmethodispreferablebecauseitavoidstheuseoftoxic reagents.Whenthephotometricmethodisapplied,volatileandsolidwastescontainingmercuryshouldbediscardedin accordancewithenvironmentalregulations. 2 Normativereference Thefollowingnormativedocumentcontainsprovisionswhich,throughref

31、erenceinthistext,constituteprovisionsof thisInternationalStandard.Fordatedreferences,subsequentamendmentsto,orrevisionsof,thispublicationdo notapply.However,partiestoagreementsbasedonthisInternationalStandardareencouragedtoinvestigatethe possibilityofapplyingthemostrecenteditionofthenormativedocumen

32、tindicatedbelow.Forundatedreferences, thelatesteditionofthenormativedocumentreferredtoapplies.MembersofISOandIECmaintainregistersof currentlyvalidInternationalStandards. ISO3696:1987,WaterforanalyticallaboratoryuseSpecificationandtestmethods. 3 Determinationofchloridebyflowanalysis(FIAandCFA)withpho

33、tometricdetection 3.1 Principle WhenusingFIA,thesampleisinjectedintoacontinuousflowingcarrierstream(water)throughaninjectionvalve. WhenusingCFA,thesampleispumpedintothecarrierstreamviaaperistalticpump.Dependingonthe concentrationofthesample,thesampleisdilutedwithwater.Areagentsolution(mercurythiocya

34、nateiron(III) nitratesolution),alsopumpedbytheperistalticpump,isthenmixedwiththesamplestream.Thethiocyanate, whichisliberatedbythechloride,reactswiththeiron(III)ionstoformared-colourediron(III)thiocyanatecomplex 4,5,6. ItisabsolutelyessentialthatthetestsdescribedinthisInternationalStandardbecarriedo

35、utbysuitablyqualified staff. ENISO15682:20012 3.2 Interferences Theanalysisissubjecttointerferencesasfollows: a)chemicalswhichliberatethiocyanate(i.e.themercurythiocyanate),forexamplebromideandiodideions; Bromidecausesinterferencewhenpresentinconcentrationsexceeding30mg/l.Themassconcentrationof brom

36、ideandiodidecanbedeterminedintermsofchlorideequivalents,andtheresultcanbeconsideredinthe calculationprocedure(3.7). b)chemicalswhichformacolouredproductwiththereagentusedintheanalysis(e.g.thiocyanateandsulfide ions); Whensulfideionsareexpected(insurface,wasteanddrainwaters),thesampleshouldbetreatedw

37、ith0,5ml ofhydrogenperoxide(3.3.7)per100mlofsampleandanalysedafteratleast5min. c)thenaturalcolourofthesample. Inthiscasedilutionofthesampleorin-linedialysisisrecommended. Filtrationofthesamplebeforeanalysisisadvisableforsampleswithparticlesizeslargerthan100 m(forexample surfaceandwastewaters),otherw

38、isetheparticlesinthesamplemayclogthetransporttubes. ThepHofthesampleshallbeadjustedtoavaluebetweenpH3andpH10. Theself-absorbanceofthesamplematrixcanbecompensatedforbymeasuring,inadditiontothesamplesignal (3.6.5),thesignalofthesampleinaparallelchannelwithouttheadmixtureofthereagents.Theparallelchanne

39、l canbeintegratedintotheflowsystem(3.4.1or3.4.2).Inthiscasethedifferencebetweenthetworesponses(with andwithoutadditionofreagents)isusedforthecalculationofresults(inaccordancewith3.7).Thedifference betweenthetwomeasuredsignalsisusedinequation(2)(3.7). 3.3 Reagents Allchemicalsrequiredshallbeofrecogni

40、zedanalyticalgrade. 3.3.1 Water,ofgrade1,inaccordancewithISO3696. 3.3.2 Mercury(II)thiocyanate,Hg(SCN) 2 . WARNINGVolatileandsolidwastescontainingmercuryshouldbediscardedinaccordancewith environmentalregulations. 3.3.3 Methanol,CH 3 OH. WARNINGMethanolistoxicandshouldbehandledwithcare. 3.3.4 Nitrica

41、cidI,HNO 3 , =1,4g/ml,massfraction=65%. 3.3.5 Iron(III)nitratenonahydrate,Fe(NO 3 ) 3 9H 2 O. 3.3.6 Sodiumchloride,NaCl,driedat105 C 5 C. 3.3.7 Hydrogenperoxide,H 2 O 2 , =1,11g/ml,massfraction=30%. 3.3.8 Detergentsolution,polyethyleneglycoldodecylether,HO-CH 2 CH 2 -O-C 12 H 25 . Freezingrange33 Ct

42、o41 C,solution,massfraction=30%. ENISO15682:2001 3 Thesolutionisstableforonemonth. 3.3.9 Reagentsolution(RinFiguresB.1toB.4). a)Dissolve31gofiron(III)nitratenonahydrate(3.3.5)inapproximately500mlofwater. b)Ina1000mlvolumetricflaskdissolve0,62gofmercurythiocyanate(3.3.2)in150mlofmethanol(3.3.3)while

43、constantlystirring.Add100mlofwater(3.3.1),3,4mlofnitricacidI(3.3.4),andtheabove-mentionedaqueous solutionofironnitrate.Makeuptovolumewithwater(3.3.1).Stirthesolutionfor2handfilter. Thesolutionisstableforthreemonthsinadarkplace. c)Beforeanalysis,degasthereagentsfor10min,e.g.bymembranefiltration(under

44、pressure). 3.3.10ChloridestocksolutionI, =10000mg/l. Dissolve16,50g 0,05gofsodiumchloride(3.3.6)inwater(3.3.1)andmakeuptoavolumeof1000mlwith water. Thesolutionisstableforoneyear. 3.3.11ChloridestocksolutionII, =100mg/l. Add5mlofstocksolutionI(3.3.10)ina500mlvolumetricflaskandmakeuptovolumewithwater.

45、 Thesolutionisstableforthreemonths. 3.3.12CarriersolutionforFIA(C1inFiguresB.1andB.2). Water(3.3.1)shallbeused. 3.3.13CarriersolutionsforCFA(C2andC3inFigureB.4). C2:Dilute8mlofnitricacidI(3.3.4)inapproximately900mlofwaterina1000mlvolumetricflask.Add1ml ofdetergentsolution(3.3.8)andmakeuptovolumewith

46、water. C3:Dilute4mlofnitricacidI(3.3.4)inapproximately900mlofwaterina1000mlvolumetricflask.Add1ml ofdetergentsolution(3.3.8)andmakeuptovolumewithwater. 3.3.14Calibrationsolutions. PreparethecalibrationsolutionsbydilutingstocksolutionIorII(3.3.10or3.3.11). Useaminimumofatleastfivecalibrationstandards

47、perworkingrange.Forexample,ifsixstandardsareused, proceedfortheworkingrangesItoIIIasfollows: a)RangeIII(1mg/lto10mg/l): Pipette1ml,3ml,5ml,6ml,8ml,and10mlrespectivelyofstocksolutionII(3.3.11)intoaseriesof100ml volumetricflasks.Makeuptovolumewithwater. Themassconcentrationsofchlorideintheresultingcal

48、ibrationsolutionare1mg/l,3mg/l,5mg/l,6mg/l, 8mg/l,and10mg/lrespectively.Thesecalibrationsolutionsarestableforoneweek. b)RangeII(10mg/lto100mg/l): Pipette10ml,30ml,50ml,60ml,80ml,and100mlrespectivelyofstocksolutionII(3.3.11)intoaseriesof 100mlvolumetricflasks.Makeuptovolumewithwater. ENISO15682:20014 Themassconcentrationsofchlorideinthesecalibrationsolutionsare10mg/l,30mg/l,50mg/l,60mg/l, 80mg/land100mg/lrespectively.Thesecalibrationsolutionsarestablef