1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | DRAFT FOR DEVELOPMENT DD ENV 13800:2000 IC
2、S 77.120.60 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Lead and lead alloys Analysis by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma emission spectrometry (ICP-ES), without separation of the lead matrixThis Draft for Development, having been p
3、repared under the direction of the Engineering Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 September 2000 BSI 09-2000 ISBN 0 580 36181 0 DD ENV 13800:2000 Amendments issued since publication Amd. No. Date Comments National foreword This
4、Draft for Development is the English language version of ENV 13800:2000. This publication is not to be regarded as a British Standard. It is being issued in the Draft for Development series of publications and is of a provisional nature because, although the analytical procedures in the method are g
5、enerally recognized, the evaluation of the method via Round-Robin analyses, together with the resultant statistical validation, as required by CEN has not yet been carried out. It should be applied on this provisional basis, so that information and experience of its practical application may be obta
6、ined. Comments arising from the use of this Draft for Development are requested. The results of the evaluation of this Draft for Development and the comments arising from its application by CEN members will be reported to the European organization responsible for its conversion into a European Stand
7、ard. A review of this publication will be initiated 2 years after its publication by the European organization so that a decision can be taken on its status at the end of its three-year life. The commencement of the review period will be notified by an announcement in Update Standards. According to
8、the replies received by the end of the review period, the responsible BSI Committee will decide whether to support the conversion into a European Standard, to extend the life of the prestandard or to withdraw it. Comments should be sent in writing to the Secretary of BSI Technical Committee NFE/22,
9、Lead and lead alloys, at 389 Chiswick High Road, London W4 4AL, giving the document reference and clause number and proposing, where possible, an appropriate revision of the text. A list of organizations represented on this committee can be obtained on request from the secretary. Cross-references Th
10、e 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 Correspondance Index, or by using the Find facility of the British Standards Electronic Catalogue. Su
11、mmary of pages This document comprises a front cover, an inside front cover, the ENV title page, pages 2 to 18, an inside back cover and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued.EUROPEANPRESTANDARD PRNORMEEUROPENNE EUROPISCHEVORNOR
12、M ENV13800 July2000 ICS77.120.60 Englishversion LeadandleadalloysAnalysisbyflameatomicabsorption spectrometry(FAAS)orinductivelycoupledplasmaemission spectrometry(ICPES),withoutseparationoftheleadmatrix PlombetalliagesdeplombAnalyseparspectromtrie dabsorptionatomiquedanslaflamme(FAAS)ou spectromtrie
13、dmissionplasmainductifcoupl(ICP ES),sanssparationdelamatriceplomb BleiundBleilegierungenAnalysedurchFlammen Atomabsorptionsspektrometrie(FAAS)oder EmissionsspektrometriemitinduktivgekoppeltemPlasma (ICPOES),ohneAbtrennungderBleimatrix ThisEuropeanPrestandard(ENV)wasapprovedbyCENon25June2000asaprospe
14、ctivestandardforprovisionalapplication. TheperiodofvalidityofthisENVislimitedinitiallytothreeyears.AftertwoyearsthemembersofCENwillberequestedto submittheir comments,particularlyonthequestionwhethertheENVcanbeconvertedintoaEuropeanStandard. CENmembersarerequiredtoannouncetheexistenceofthisENVinthesa
15、mewayasforanENandtomaketheENVavailablepromp tly atnationallevelinanappropriateform.Itispermissibletokeepconflictingnationalstandardsinforce(inparalleltothe ENV)untilthefinal decisionaboutthepossibleconversionoftheENVintoanENisreached. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRep
16、ublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG CentralSecretariat:ruedeStassart,36B1050Brussels 2000CEN All
17、rightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.ENV13800:2000EPage2 ENV13800:2000 Contents Foreword3 1 Scope 4 2 Normativereferences 4 3 Principle5 3.1 Dissolution5 3.2 Instrumentaltechniques . 5 4 Apparatus .6 4.1 General6 4.2 Volumetricglassware 6 4.3 Plas
18、ticware 6 4.4 Instruments.6 5 Reagents.7 5.1 General7 5.2 Nitricacid(HNO 3 ) 7 5.3 Tartaricacidsolution(C 4 H 6 O 6 )300g/l.7 5.4 Hydrochloricacid(HCl) . 7 5.5 Fluoboricacid(HBF 4 )7 5.6 Leadformatrixmatching 7 5.7 Standardsolutions 8 6 Samplingandsamplepreparation . 10 7 Procedure .10 7.1 Preparati
19、onofthetestsolution 10 7.2 Preparationoftheblanktestsolution .11 7.3 Dilutionofthetestsolutionsandoftheblanktestsolution . 11 8 DeterminationofelementsbyFAAS. .11 8.1 Preparationofcalibrationsolutions 11 8.2 Calibration,measurementsandresults . .13 9 DeterminationofelementsbyICPES . 15 9.1 Preparati
20、onofcalibrationsolutions 15 9.2 Calibration,measurementsandresults . .16 10 Testreport 18Page3 ENV13800:2000 Foreword ThisEuropeanPrestandardhasbeenpreparedbyTechnicalCommitteeCEN/TC306“Leadandleadalloys“,the secretariatofwhichisheldbyAFNOR. AccordingtotheCEN/CENELECInternalRegulations,thenationalst
21、andardsorganizationsofthefollowing countriesareboundtoannouncethisEuropeanPrestandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden, SwitzerlandandtheUnitedKingdom. CAUTIONFORSAFETYANDTRAINING Themethods
22、inthisstandardarerecommendedforthecertificationofreferencematerialsandasumpiremethods incasesofadispute.Theimportanceofeitherapplication,andtheparamountissueofsafety,requiresthatthey shouldonlybecarriedoutbyfullytrainedanalystswhoareexperiencedinallrelevanttechniquesandthe precautionsnecessaryinthei
23、nherentlyhazardousenvironsofalaboratory,especiallythoserequiredwhenusing particularlyhazardousapparatusandreagentsusedinsomeofthesemethods. Whereaparticularhazardexists,thisisgivenasa DANGERadjacenttothepointinthetextwheretheapparatus orreagentisreferenced.Page4 ENV13800:2000 1Scope ThisEuropeanPres
24、tandardspecifiesmethodsofanalysisusingflameatomicabsorptionspectrometry(FAAS)and inductivelycoupledplasmaemissionspectrometry(ICPES)forthedeterminationofelementcontentsinleadand leadalloysfortherangesgiveninTable1. Table1Rangesofapplicationforthedeterminationofelementcontents Rangesofapplication(%m/
25、m) Element FAAS ICPES Ag 0,0005 1 0,0001 1 Al 0,005 0,04 0,0005 0,05 As 0,005 0,25 0,002 0,3 Ba 0,0025 0,025 0,0002 0,005 Bi 0,0025 0,2 0,002 0,2 Ca 0,001 0,2 0,0005 0,2 Cd 0,001 0,2 0,0001 0,2 Cu 0,0005 0,06 0,0001 0,06 Na 0,001 0,02 0,001 0,02 Ni 0,0005 0,005 0,0005 0,005 S 0,002 0,01 Sb 0,0025 10
26、 0,002 10 Se 0,005 0,04 0,005 0,04 Sn 0,005 2 0,002 2 Te 0,0025 0,05 0,002 0,05 TI 0,0025 0,05 0,0025 0,05 Zn 0,0005 0,01 0,0002 0,01 Thesemethodsareintendedasthedefinitivemethodsincaseofdisputeforthedeterminationofelementsatlow contentinlead.TheyarealsorecommendedfortheanalysisofCertifiedReferenceM
27、aterials(CRM)and ReferenceMaterials(RM)whichareusedinanalysisaccordingtoENV12908. 2 Normativereferences ThisEuropeanPrestandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetextandthepublicationsarelistedhereafter.Fo
28、r datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Prestandardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). EN12402, LeadandleadalloysMethodsofsamplingforanalysis.
29、 ENV12908, LeadandleadalloysAnalysisbyOpticalEmissionSpectrometry(OES)withsparkexcitation. ISO648:1977, LaboratoryglasswareOnemarkpipettes.Page5 ENV13800:2000 ISO1042:1983, LaboratoryglasswareOnemarkvolumetricflasks. ISO3696, WaterforanalyticallaboratoryuseSpecificationandtestmethods. 3Principle 3.1
30、Dissolution Dissolutionofatestportionin,either: nitricacid;or mixtureofnitricacid/tartaricacid;or mixtureofnitricacid/fluoboricacid. Dilutionofthetestsolutiontoadefinedvolume,anddeterminationoftheanalyteconcentrationusingoneofthe twotechniquesdescribedin3.2. 3.2Instrumentaltechniques 3.2.1 Flameatom
31、icabsorptionspectrometry(FAAS) Theanalyteconcentrationinthetestsolutionisobtainedby: nebulizationofthetestsolutionintotheflameofanatomicabsorptionspectrometer; measurementoftheabsorptionoftheresonancelineenergyofthespectrumfromtheelementattherelevant wavelength(absorbency); comparisonwiththatofmatri
32、xmatchedcalibrationsolutionsofthesameelement. 3.2.2 Inductivelycoupledplasmaemissionspectrometry(ICPES) Theanalyteconcentrationinthetestsolutionisobtainedby: nebulizationofthetestsolutionintotheplasmaofaninductivelycoupledplasmaopticalemission spectrometer; measurementoftheintensityoftheemissionsign
33、alfromthespectrumoftheelementstobedeterminedatthe relevantwavelength; comparisonwiththatofmatrixmatchedcalibrationsolutionsofthesameelement.Page6 ENV13800:2000 4Apparatus 4.1General Useordinaryapparatusasavailableinachemicallaboratory. Allglasswareandplasticwaretobeusedshallbecleanedwithdilutednitri
34、cacid(5.2.2)andthoroughlyrinsedwith water. 4.2Volumetricglassware 4.2.1 Onemarkvolumetricflasksofcapacities100ml,250ml,500ml,and1000mlinaccordancewith ISO1042:1983classA. 4.2.2 Onemarkpipettesofcapacities2ml,5ml,10ml,15ml,20ml,25ml,50mland100mlinaccordance withISO648:1977classA. 4.3Plasticware Thefo
35、llowingarerequired: Polytetrafluoroethylene(PTFE)beakersof250mlcapacity; SuitablePTFEcovers; Onemarkvolumetricflasksof100mlcapacity. 4.4Instruments 4.4.1 Flameatomicabsorptionspectrometer Flameatomicabsorptionspectrometer(FAAS)equippedwithlaminarflowburnerssuitableforacetyleneair, hydrogenairoracety
36、lenenitrousoxideflames,andwithradiationsourcessuchashollowcathodelamps(HCL)or electrodelessdischargelamps(EDL)asappropriatetotheelementtobedetermined. Theinstrumentshallbeusedinaccordancewiththemanufacturersinstructionsandtheperformancechecked(see theISOdocumentsinpreparation,numbers00023056and00023
37、057). DANGER Toavoidanyrisktopersonnelduetoemissionofacidandleadfumes,theoffgasshallbe exhaustedexternally. 4.4.2 Inductivelycoupledplasmaemissionspectrometer Inductivelycoupledplasmaemissionspectrometer(ICPES),eitherasimultaneousinstrumentwiththerelevant wavelengthsinstalledorasequentialinstrumentw
38、hereamonochromatorsystemallowstheselectionof wavelengths(seetheISOdocumentinpreparation,number00021288). Theinstrumentshallbeusedinaccordancewiththemanufacturersinstructionsandtheperformanceschecked (seetheISOdocumentinpreparation,number00023058). DANGER Toavoidanyrisktopersonnelduetoemissionofacida
39、ndleadfumes,theoffgasshallbe exhaustedexternally.Page7 ENV13800:2000 5Reagents 5.1General Forallstagesofanalysis,unlessotherwisestated,useonlyreagentsofrecognisedanalyticalgrade,preferably withanactualanalysis,andonlywaterofatleastgrade2,asspecifiedinISO3696. Prepareallsolutionsusingthesamecontainer
40、ofeachreagent. 5.2Nitricacid(HNO 3 ) 5.2.1 Concentratednitricacid Nitricacidwhich 20 =1,41g/ml. 5.2.2 Nitricacid1:1(v/v) Addtoonevolumeofwater,thesamevolumeofnitricacid(5.2.1)inasuitablecontainerandmixthoroughly.This dilutedacidisalsousedtocleanthelaboratoryware. 5.2.3 Nitricacid1:2(v/v) Add200mlnit
41、ricacid(5.2.1)to400mlwaterintoa1000mlbeakerandmixthoroughly. 5.3Tartaricacidsolution(C 4 H 6 O 6 )300g/l Weigh150goftartaricacid(C 4 H 6 O 6 )intoa500mlvolumetricflask,addabout350mlofwaterandshakeuntil dissolutioniscomplete.Makeuptothemarkwithwaterandmixthoroughly. 5.4Hydrochloricacid(HCl) Hydrochlo
42、ricacidwhich 20 =1,18g/ml. 5.5Fluoboricacid(HBF 4 ) Fluoboricacidwhich 20 =1,22g/ml. DANGER Thisreagenthassevererisksbothbyingestionandparticularlybyskincontact.Beforeusing thisreagentcarefullyreadthesafetydatasheettoensurethatallthenecessaryprecautionsaretaken, includingthepersonalprotectiveequipme
43、ntrequired. 5.6Leadformatrixmatching 5.6.1 Purelead Forthedeterminationofmostoftheelementcontentsdetailedinclauses8and9,purelead(99,99%m/m)maybe usedprovidingthatnorelevantelementsarepresentinanamountthatcouldbesignificanttothedetermination required.Ifanyrelevantelementsarepresent,leadofhigherpurity
44、(99,999%ormore)shallbeused. 5.6.2 Leadsolution(100g/l) Weigh100goflead(5.6.1)intoa600mlbeaker,add300mlofwater,andthen,inseveralstepstocontrola possiblyvigorousreaction,add100mlofnitricacid(5.2.1);coverwithawatchglassandheatgentlyuntil dissolutioniscomplete.Boilgentlyuntilnitrousfumesareexpelledandthen,allowtocool. Transferintoa1000mlvolumetricflask(4.2.1),makeuptothemarkwithwaterandmixthoroughly.Page8 ENV13800:2000 5.7 Standardsolutions 5.7.1
