1、DRAFT FOR DEVELOPMENT DD ENV 14029:2001 Lead and lead alloys Analysis by flame atomic absorption spectrometry (FAAS) or inductively coupled plasma emission spectrometry (ICP-ES), after separation of the lead matrix ICS 77.150.60 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWD
2、D ENV 14029:2001 This Draft for Development, having been prepared under the direction of the Engineering Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 September 2001 BSI 07-2001 ISBN 0 580 37219 7 National foreword This Draft for Developme
3、nt is the English language version of ENV 14029:2001. 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 generally recognised
4、, 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 obtained. Comments ari
5、sing from the use if this Draft for Development are requested so that UK experience can be reported to the European organization responsible for its conversion into a European Standard. A review of this publication will be initiated 2 years after its publication by the European organization so that
6、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 the replies received by the end of the review period, the responsible BSI Committee will decide whether to support the
7、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, Lead and lead alloys, at 389 Chiswick High Road, London W4 4AL, giving the document reference and clause number and pro
8、posing, where possible, an appropriate revision of the text. A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in t
9、he BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. Summary of pages This document comprises a front cover, an inside front cover, the ENV title page, pages 2 to 14, an inside
10、 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 CommentsEUROPEANPRESTANDARD PRNORMEEUROPENNE EUROPISCHEVORNORM ENV14029 July2001 ICS77.040.30;77.120.60 Englishversion Leadan
11、dleadalloysAnalysisbyflameatomicabsorption spectrometry(FAAS)orinductivelycoupledplasmaemission spectrometry(ICPES),afterseparationoftheleadmatrix PlombetalliagesdeplombAnalyseparspectromtrie dabsorptionatomiquedanslaflamme(FAAS)ou spectromtriedmissionatomiqueplasmainductif coupl(ICPES),aprssparatio
12、ndelamatriceplomb BleiundBleilegierungenAnalysedurchFlammen Atomabsorptionsspektrometrie(FAAS)oderEmissions SpektrometriemitinduktivgekoppeltemPlasma(ICPES), nachAbtrennungderBleimatrix ThisEuropeanPrestandard(ENV)wasapprovedbyCENon9June2001asaprospectivestandardforprovisionalapplication. Theperiodo
13、fvalidityofthisENVislimitedinitiallytothreeyears.AftertwoyearsthemembersofCENwillberequestedto submittheir comments,particularlyonthequestionwhethertheENVcanbeconvertedintoaEuropeanStandard. CENmembersarerequiredtoannouncetheexistenceofthisENVinthesamewayasforanENandtomaketheENVavailablepromp tly at
14、nationallevelinanappropriateform.Itispermissibletokeepconflictingnationalstandardsinforce(inparalleltothe ENV)untilthefinal decisionaboutthepossibleconversionoftheENVintoanENisreached. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Icela
15、nd,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved w
16、orldwideforCENnationalMembers. Ref.No.ENV14029:2001EVNE41:9202100(E) 2 Contents page Foreword3 1 Scope.4 2 Normativereferences 5 3 Principle 5 3.1 Preparationofthetestsolution 5 3.2 Instrumentaltechniques. .5 4 Apparatus .6 4.1 General6 4.2 Volumetricglassware 6 4.3 Filtrationsystem . .6 4.4 Instrum
17、ents.6 5 Reagents .6 5.1 General6 5.2 Nitricacid(HNO 3 ) 7 5.3 Hydrochloricacid(HCl) . 7 5.4 Purelead . 7 5.5 Standardsolutions .7 6 Samplingandsamplepreparation . 9 7 Procedure .9 7.1 Preparationofthetestsolution 9 7.2 Preparationofthesynthetictestsolution .9 7.3 Preparationoftheblanktestsolution .
18、9 7.4 Preparationofcalibrationsolutions 10 8 DeterminationofelementsbyFAAS. .10 8.1 General10 8.2 Calibrationandmeasurementofthetestsolution .11 8.3 Expressionofresults. 12 9 DeterminationofelementsbyICPES. .13 9.1 General13 9.2 Calibrationandmeasurementofthetestsolution .14 9.3 Expressionofresults.
19、 14 10 Testreport 14 ENV14029:2001 VNE41:9202100(E) 3 Foreword ThisEuropeanPrestandardhasbeenpreparedbyTechnicalCommitteeCEN/TC306,“Leadandleadalloys“,the secretariatofwhichisheldbyAFNOR. CAUTIONFORSAFETYANDTRAINING Themethodsinthisstandardarerecommendedforthecertificationofreferencematerialsandasum
20、piremethods incasesofadispute.Theimportanceofeitherapplication,andtheparamountissueofsafety,requiresthatthey shouldonlybecarriedoutbyfullytrainedanalystswhoareexperiencedinallrelevanttechniquesandthe precautionsnecessaryintheinherentlyhazardousenvironsofalaboratory,especiallythoserequiredwhenusing p
21、articularlyhazardousapparatusandreagentsusedinsomeofthesemethods. Whereaparticularhazardexists,thisisgivenasa DANGERadjacenttothepointinthetextwheretheapparatus orreagentisreferenced. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefollowing countriesareboundtoanno
22、uncethisEuropeanPrestandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden, SwitzerlandandtheUnitedKingdom. ENV14029:2001 VNE41:9202100(E) 4 1Scope ThisEuropeanPrestandardspecifiesmethodsusingflameatomica
23、bsorptionspectrometry(FAAS)andinductively coupledplasmaemissionspectrometry(ICPES)forthedeterminationofelementsatlowcontentinleadforthe rangesgiveninTable1. HighercontentsthanthoselistedinTable1shouldbedeterminedaccordingtoENV13800. Table1Rangesofapplicationforthedeterminationofelements Rangesofappl
24、ications(%m/m) Element FAAS ICPES Ag 0,00001 0,001 0,00001 0,001 Al 0,0001 0,005 0,00005 0,005 As 0,0002 0,005 0,00005 0,005 Bi 0,00005 0,0025 0,00005 0,0025 Ca 0,00005 0,001 0,00001 0,001 Cd 0,00005 0,001 0,00001 0,001 Co 0,00005 0,001 0,00005 0,001 Cr 0,00005 0,001 0,00005 0,001 Cu 0,00001 0,001 0
25、,00001 0,001 Fe 0,00005 0,001 0,00005 0,001 Mg 0,00005 0,001 0,00005 0,001 Mn 0,00005 0,001 0,00005 0,001 Na 0,00005 0,001 0,00001 0,001 Ni 0,00005 0,001 0,00001 0,001 Sb 0,0002 0,0025 0,0002 0,0025 Se 0,0002 0,005 0,0002 0,005 Sn 0,0005 0,005 0,0002 0,005 Te 0,00002 0,0025 0,00002 0,0025 TI 0,00002
26、 0,0025 0,00002 0,0025 Zn 0,00001 0,001 0,00001 0,001 Thesemethodsareintendedasthedefinitivemethodsincaseofdisputeforthedeterminationofelementsatlow contentinlead.TheyarealsorecommendedfortheanalysisofCertifiedReferenceMaterials(CRM)and ReferenceMaterials(RM)whichareusedinanalysisaccordingtoENV12908
27、. ENV14029:2001 VNE41:9202100(E) 5 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetextandthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevision
28、sofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditionofthe publicationreferredtoapplies(includingamendments). EN12402, LeadandleadalloysMethodsofsamplingforanalysis. ENV12908, LeadandleadalloysAnalysisbyOpticalEmission
29、Spectrometry(OES)withsparkexcitation. ENV13800,LeadandleadalloysAnalysisbyflameatomicabsorptionspectrometry(FAAS)orinductively coupledplasmaemissionspectrometry(ICPES),withoutseparationoftheleadmatrix. ISO648:1977, LaboratoryglasswareOnemarkpipettes. ISO1042:1998, LaboratoryglasswareOnemarkvolumetri
30、cflasks. ISO3696, WaterforanalyticallaboratoryuseSpecificationandtestmethods. 3Principle 3.1 Preparationofthetestsolution Dissolutionofatestportioninnitricacid. Separationofleadbycrystallisationasleadnitrate. Reductionofthetestsolutiontoadefinedvolume,anddeterminationoftheanalyteconcentrationusingon
31、eofthe twotechniquesdescribedin3.2. 3.2 Instrumentaltechniques 3.2.1 Flameatomicabsorptionspectrometry(FAAS) Theanalyteconcentrationinthetestsolutionisobtainedby: nebulizationofthetestsolutionintotheflameofanatomicabsorptionspectrometer; measurementoftheabsorptionoftheresonancelineenergyofthespectru
32、mfromtheelementattherelevant wavelength(absorbance); comparisonwiththatofmatrixmatchedcalibrationsolutionsofthesameelement. 3.2.2 Inductivelycoupledplasmaemissionspectrometry(ICPES) Theanalyteconcentrationinthetestsolutionisobtainedby: nebulizationofthetestsolutionintotheplasmaofaninductivelycoupled
33、plasmaopticalemission spectrometer; measurementoftheintensityoftheemissionsignalfromthespectrumoftheelementtobedeterminedatthe relevantwavelength; comparisonwiththatofmatrixmatchedcalibrationsolutionsofthesameelement. ENV14029:2001 VNE41:9202100(E) 6 4Apparatus 4.1General Useordinaryapparatusasavail
34、ableinachemicallaboratory. Allglasswaretobeusedshallbecleanedwithdilutednitricacid(5.2.2)andthoroughlyrinsedwithwater. 4.2 Volumetricglassware 4.2.1 Onemarkvolumetricflasksofcapacities20ml,200ml,500ml,and1000mlinaccordancewithISO 1042:1998classA. 4.2.2 Onemarkpipettesofcapacities2ml,5ml,10ml,and50ml
35、inaccordancewithISO648:1977classA. 4.3Filtration system VacuumfiltrationsystemwithafiltermembraneofPTFE,orothermaterialinerttonitricacid,ofabout5m porosity(filteringdiameter20mmto50mm). 4.4Instruments 4.4.1 Flameatomicabsorptionspectrometer Flameatomicabsorptionspectrometer(FAAS)equippedwithlaminarf
36、lowburnerssuitableforacetyleneair, hydrogenairoracetylenenitrousoxideflames,andwithradiationsourcessuchashollowcathodelamps(HCL)or electrodelessdischargelamps(EDL)asappropriatetotheelementtobedetermined. Theinstrumentshallbeusedinaccordancewiththemanufacturersinstructionsandtheperformancechecked(see
37、 alsotheISOdocumentsinpreparation,numbers00023056and00023057). DANGER Toavoidanyrisktopersonnelduetoemissionofacidandleadfumes,theoffgasshallbe exhaustedexternally. 4.4.2 Inductivelycoupledplasmaemissionspectrometer Inductivelycoupledplasmaemissionspectrometer(ICPES),eitherasimultaneousinstrumentwit
38、htherelevant wavelengthsinstalledorasequentialinstrumentwhereamonochromatorsystemallowstheselectionof wavelengths(seealsotheISOdocumentinpreparationnumber00021288). Theinstrumentshallbeusedinaccordancewiththemanufacturersinstructionsandtheperformanceschecked (seealsotheISOdocumentinpreparation,numbe
39、r00023058). DANGER Toavoidanyrisktopersonnelduetoemissionofacidandleadfumes,theoffgasshallbe exhaustedexternally. 5Reagents 5.1General Forallstagesofanalysis,unlessotherwisestated,useonlyreagentssuitablefortraceanalysisofrecognised analyticalgrade,preferablywithanactualanalysis,andonlywaterofatleast
40、grade2,asspecifiedinISO3696. Prepareallsolutionsusingthesamecontainerofeachreagent. ENV14029:2001 VNE41:9202100(E) 7 5.2 Nitricacid(HNO 3 ) 5.2.1 Concentratednitricacid Nitricacidofhighpurity,which 20 =1,41g/ml. 5.2.2 Nitricacid1:1(v/v) Addtoonevolumeofwater,inasuitablecontainer,thesamevolumeofnitri
41、cacid(5.2.1)andmixthoroughly.This dilutedacidisalsousedtocleanthelaboratoryware. 5.2.3 Nitricacid1:2(v/v) Add200mlnitricacid(5.2.1)to400mlwaterina1000mlbeakerandmixthoroughly. 5.3 Hydrochloricacid(HCl) Hydrochloricacidofhighpurity,which 20 =1,18g/ml. 5.4 Purelead Forthedeterminationoftherecoveryrate
42、oftheanalyte(see7.2),verypurelead(99,9999%m/m)shouldbe used.However,leadoflowerpuritymaybeusedprovidedthattheanalyteisnotpresentinanamountthatcould besignificanttothedeterminationrequired. 5.5 Standardsolutions 5.5.1 Standardsolutions(1g/l) 5.5.1.1General Eitherusecommerciallyavailablecertifiedstand
43、ardsolutionsorpreparestandardsolutionsasdescribedin5.5.1.2 to5.5.1.10. 5.5.1.2 Solutionsforsilver,bismuth,cadmium,cobalt,chromium,iron,manganese,magnesium,copper, nickel,thalliumandzinc Weigh(1,00,001)goftherelevantmetal(99,99%m/mminimumpurity)andtransferintoa250mlbeaker.Add 75mlofnitricacid(5.2.3),
44、coverwithawatchglassandheatgentlyuntildissolutioniscomplete.Allowtocool,then transferintoa1000mlvolumetricflask(4.2.1),thenmakeuptothemarkwithwaterandmixthoroughly. Storethesilversolutioninthedark. 5.5.1.3 Solutionforaluminium Thealuminiumusedforthissolutionshallbeinaformofcleanwire,foil,orpiecescutormilledfromaningot.Do notusealuminiumpowderbecauseofpossibleoxidationoftheverylargespecificsurfaceinvolved. Weigh(1,0000,001)gofaluminium(99
