EN 12260-2003 en Water quality - Determination of nitrogen - Determination of bound nitrogen (TNb) following oxidation to nitrogen oxides《水质 氮的测定 随着氮氧化物的氧化测定结合氮(TNb) 代替ENV 12260-19.pdf

1、BRITISH STANDARD BS EN 12260:2003 BS 6068-2.83:2003 Water quality Determination of nitrogen Determination of bound nitrogen (TN b ), following oxidation to nitrogen oxides The European Standard EN 12260:2003 has the status of a British Standard ICS 13.060.50 BS EN 12260:2003 This British Standard, w

2、as published under the authority of the Standards Policy and Strategy Committee on 25 September 2003 BSI 25 September 2003 ISBN 0 580 42692 0 National foreword This British Standard is the official English language version of EN 12260:2003. It supersedes DD ENV 12260:1996 which is withdrawn. The UK

3、participation in its preparation 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-

4、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 Catalogue or of Br

5、itish 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 the text; pres

6、ent 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

7、inside front cover, the EN title page, pages 2 to 13 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN12260 September2003 ICS13

8、.060.50 SupersedesENV12260:1996 Englishversion WaterqualityDeterminationofnitrogenDeterminationof boundnitrogen(TN b ),followingoxidationtonitrogenoxides QualitdeleauDosagedelazoteDosagedelazoteli (TN b)aprsoxydationenoxydesdazote WasserbeschaffenheitBestimmungvonStickstoff BestimmungvongebundenemSt

9、i ckstoff(TN b)nach OxidationzuStickstoffoxiden ThisEuropeanStandardwasapprovedbyCENon1August2003. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographical

10、referencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManage

11、mentCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom. EUROPEANCOM

12、MITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN12260:2003EEN12260:2003(E) 2 Contents page Foreword. 3 Introduction 4

13、 1 Scope . 5 2 Normativereferences . 5 3 Principle. 5 4 Interferences 5 5 Reagents 6 6 Apparatus 6 7 Samplingandsamplepreparation . . 7 8 Procedure 7 9 Establishmentofthecalibrationcurve . 7 10 Systemcheck . . 8 11 Calculation. 8 12 Expressionofresults . 8 13 Testreport . 9 14 Precisiondata. . 9 Ann

14、exA (informative) Determinationofboundnitrogenusingothertechniques 10 AnnexB (informative) Recoveryratesofsinglecompoundsusingoxidationand chemiluminescencedetection(seetableB.1) . 11 AnnexC (informative) Precisiondata. 12 Bibliography . 13EN12260:2003(E) 3 Foreword Thisdocument(EN12260:2003)hasbeen

15、preparedbyTechnicalCommitteeCEN/TC230“Wateranalysis”, thesecretariatofwhichisheldbyDIN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofanidentical textorbyendorsement,atthelatestbyMarch2004,andconflictingnationalstandardsshallbewithdrawnat thelatestbyMarch2004. Thi

16、sdocumentsupersedesENV12260:1996 AnnexesAB,andCareinformativeannexes. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark, Finland,France,Germany,Greece,Hungary,Iceland,Ire

17、land,Italy,Luxembourg,Malta,Netherlands, Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN12260:2003(E) 4 Introduction WARNINGPersonsusingthisstandardshouldbefamiliarwithnormallaboratorypractice.This standarddoesnotpurporttoaddressallofthesafetyproblems,ifany,associatedwithitsu

18、se.Itis theresponsibilityoftheusertoestablishappropriatesafetyandhealthpracticesandtoensure compliancewithanynationalregulatoryconditions. ItisabsolutelyessentialthattestscarriedoutaccordingtothisEuropeanStandardarecarriedoutbysuitably qualifiedstaff. ThisEuropeanStandardspecifiesamethodforthedeterm

19、inationoftotalboundnitrogenafteroxidationof inorganicandorganicnitrogencompoundsbycombustiontonitrogenoxides.Quantificationiscarriedoutby chemiluminescence. Theprocedurereferredtointhenormativepartisthereferencemethod.Whilststayingwithinthescopeofthis standard,itispermissibletousesuchalternativesasg

20、iveninannexAonly,providedthattheirperformanceis equaltoorbetterthanthatgiveninclause13andtablesinannexBandC,whencalculatedusingprocedures giveninISO57252,andwhenthecomparisonofperformancedatabetweenthisEuropeanStandardandany alternativetechniqueiscarriedoutusingtheproceduresdescribedinISO2854. Allre

21、ferencestonitrogenconcentrationsareexpressedinunitsofmg/lN,i.e.milligramsofnitrogenperlitre solution.EN12260:2003(E) 5 1Scope ThisEuropeanStandardspecifiesamethodforthedeterminationofnitrogeninwaterintheformoffree ammonia,ammonium,nitrite,nitrateandorganiccompoundscapableofconversiontonitrogenoxides

22、under theoxidativeconditionsdescribed.Determinationiscarriedoutinstrumentally.Dissolvednitrogengasisnot determinedbythismethod. Thismethodisapplicabletotheanalysisofsurfacewater,wastewaterandtreatedsewageeffluent. Theconcentrationrangeofthemethodwilldependontheinjectionvolumeusedwhichisinstrumentspe

23、cific. Totalnitrogencanbedeterminedintherangefrom1mg/lupto200mg/l.Higherconcentrationscan,if necessary,bedeterminedbydilutionofthesample.Thelimitofdetectionwilldependontheinstrumentin use.Usingasuitableinjectionvolume,thelimitofdetectionistypicallyroundabout0,5mg/l. 2 Normativereferences ThisEuropea

24、nStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications. Thesenormativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelisted hereafter.Fordatedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplyto thisEuropeanStandardonlywhenincorp

25、oratedinitbyamendmentorrevision.Forundatedreferencesthe latesteditionofthepublicationreferredtoapplies(includingamendments). ENISO3696, WaterforanalyticallaboratoryuseSpecificationandtestmethods(ISO3696:1987) . ENISO56673, WaterqualitySamplingPart3:Guidanceonthepreservationandhandlingofsamples (ISO5

26、6673:1994) . ISO57252,Accuracy(truenessandprecision)ofmeasurementmethodsandresults Part 2:Basic methodsforthedeterminationofrepeatabilityandreproducibilityofastandardmeasurementmethod. ISO84661, WaterqualityCalibrationandevaluationofanalyticalmethodsandestimationofperformance characteristicsPart1:St

27、atisticalevaluationofthelinearcalibrationfunction . ISO84662,WaterqualityCalibrationandevaluationofanalyticalmethodsandestimationofperformance characteristicsPart2:Calibrationstrategyfornonlinearsecondordercalibrationfunction. 3Principle Oxidationofthesamplecontainingnitrogenbycatalyticcombustionina

28、noxygenatmosphereat700C,to nitrogenoxides.Quantificationofnitrogenconcentrationiscarriedoutbychemiluminescencedetection(after reactionwithozone). 4Interferences Dependingontheinstrumentinuse,interferencesmayarisefrommemoryeffects.Thesemayoccureither fromsamplesorstandardsolutionswithhighamountsofbou

29、ndnitrogen. NOTE Potentialproblemscanarisewithsamplescontainingsignificanttotalorganiccarbon(TOC)concentrations. TheanalysisofsamplescontaininglargeamountsofTOCwillleadtothereportingoflowerresultsfornitrogen.Suspected problemscanbeidentifiedbydeterminingnitrogenbeforeandaftersuitabledilution,orbyusi

30、ngstandardaddition techniques. Notallorganicnitrogencompoundsarequantitativelyconvertedtonitrogenoxidesbytheoxidationprocedure used(seerecoveryratesintableB.1).EN12260:2003(E) 6 Ifahomogenizedsamplecontainingsuspendedmaterialproducesresults(obtainedfromreplicate measurements)whichdeviatebymorethan10

31、%,thesampleneedstobefilteredthrougha0,45mfilter, freeofnitrogencontainingcompounds.Inthiscase,onlythedissolvedportionoftheboundnitrogenwillbe determinedandreported. 5Reagents 5.1General Usereagentsofrecognizedanalyticalgrade. 5.2Water DuringanalysisuseGrade3puritywaterasspecifiedinENISO3696.Theconte

32、ntsofbo undnitrogenin waterbeingusedforthepreparationofcalibrationsolutionsshallbenegligiblylowcomparedwiththelowest concentrationtobedetermined. 5.3Hydrochloricacid, (HCl)=1,12g/ml. 5.4Nitrogenstocksolutionforcalibration, (N)=1,000g/l. 5.4.1 Dissolve(4,717 0,001)gofammoniumsulfate,(NH 4 ) 2 SO 4 ,

33、previously dried at (1052)C to constantweight,ina1000mlvolumetricflask,andmakeuptovolumewithwater. 5.4.2 Dissolve(7,2190,001)gofpotassiumnitrate,KNO 3 ,previouslydriedat(1052)Ctoconstant weight,ina1000mlvolumetricflask,andmakeuptovolumewithwater. 5.4.3 Mixequalvolumesoftheabovesolutions(see5.4.1and5

34、.4.2)toproduceamixedstandardsolution. Storedinarefrigeratorat(42)C,thestandardsolutioncanbeusedforaboutonemonth. 5.5Nicotinicacid, C 6 H 5 NO 2 ,99,5%. 5.6Nitrogenstocksolutionsforsystemcheck, (N)=1,000g/l. 5.6.1 Prepareseparatelystocksolutionscorrespondingto5.4.1and5.4.2. 5.6.2 Dissolve(8,7930,001)

35、gofnicotinicacid(5.5),previouslydriedat(1052)Ctoconstantmass, transfertoa1000mlvolumetricflaskandmakeuptovolumewithwater(5.2). Storeinarefrigeratorat(42)C,thestandardsolutioncanbeusedforaboutonemonth. 5.7Oxygen, O 2 ,withavolumefractionof99,7%. 6Apparatus 6.1Apparatussuitableforthedeterminationoftot

36、alboundnitrogenbyoxidation Thisapparatuswillbeinstrumentdependantandcomprisesforexamplereactionvessel,automaticsample injectiondevice,samplehomogenizingequipment,suitabledetectorsorsensorsandcomputingsystem.A manualinjectionsystemmayalsobeused.Forrequirementsforasuitablesystemseeclause10.EN12260:200

37、3(E) 7 6.2Homogenizer 6.3Filtrationapparatus, withmembranefilters(porewidth0,45m). 6.4Syringes 7 Samplingandsamplepreparation Whensampling,ensurethatarepresentativesampleisobtained(thisisparticularlyimportantforsamples containinganyundissolvedmatter),andthatthesampleisnotcontaminated.Inaddition,seeE

38、NISO56673. Withdrawsamplesinsuitablecontainersconsistingofglassorsuitableplastics,appropriatelysealed. Analyzesamplesassoonaspossible. NOTE Delaymayresultinthereportingoflowvalues(especiallyinthecaseofbiologicallyactivesamples). Samplesmaybestabilizedbytheadditionofhydrochloricacid(5.3)toachieveapHv

39、alueoflessthan2,and storedinarefrigeratorat(4 2) C.Stabilisedsamplesmaybestoredforaperiodofupto8 days. Alternativelystoresmallersamplevolumes(e.g.50mlto100ml)at15Cto20Cupto14days. Ifnecessary,homogenizethesampleinordertoobtainarepresentativealiquotforthedetermination(see clause4).Ifthisisimpracticab

40、le,filterthrougha0,45mfilter(6.3). 8Procedure Followtheinstrumentmanufacturersinstructions. Priortothedeterminationofboundnitrogen,ensurethatinstrumentoperationaltestsandtheverificationof theresponsestoblankandstandardsolutionsarecarriedoutwithintheintervalsspecifiedbythe manufacturer. Adjusttheinst

41、rumentaccordingtothemanufacturersinstructionsforeachseriesofmeasurements. Ifaninstrumentisfittedwithanautomatedinjectionsystem,ensurethatthesampleisunlikelytocauseany interferencewiththeinjectionprocedureby,forexample,homogenizingthesample(seealsoclause4). Injectidenticalvolumesofblanksolutionsandsa

42、mplesintotheinstrumentaccordingtothemanufacturers instructionsandmeasuretheresponsesobtainedforaliquotsofeachsolutionatleastthreetimes. Rejectthefirstandusethemeanresponsefromatleasttwoinjectionstakingintoaccountanymemoryeffects likelytooccur(seeclause4).Usethecalibrationgraph(seeclause9)todetermine

43、theconcentrationoftotal boundnitrogeninthesample. 9 Establishmentofthecalibrationcurve Usethemixedstandardsolution(5.4.3)topreparecalibrationsolutionsinaccordancewiththerangeof concentrationsoftotalboundnitrogenexpectedinthesamplestobedetermined. Usethecalibrationsolutionsonthedayofpreparationonly.Calibratewithinonedecadeofconcentration.For theconcentrationrangeof10mg/lto100mg/l,proceed,forexample,asfollows: Into7separatevolumetric100mlflasks,pipette0,(blank)1,0ml;2,0ml;3,0ml;6,0ml;8,0m