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
