1、BRITISH STANDARD BS EN 13657:2002 Characterization of waste Digestion for subsequent determination of aqua regia soluble portion of elements The European Standard EN 13657:2002 has the status of a British Standard ICS 13.030.40 BS EN 13657:2002 This British Standard, having been prepared under the d
2、irection of the Building and Civil Engineering Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee on 22 October 2002 BSI 22 October 2002 ISBN 0 580 40624 5 National foreword This British Standard is the official English language ver
3、sion of EN 13657:2002. The UK participation in its preparation was entrusted by Technical Committee B/508, Waste management, to Subcommittee B/508/3, Characterization of waste, which has the responsibility to: A list of organizations represented on this subcommittee can be obtained on request to its
4、 secretary. Cross-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
5、Catalogue or of British 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 underst
6、and the text; present 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
7、a front cover, an inside front cover, the EN title page, pages 2 to 26, an 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 publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EURO
8、PISCHENORM EN13657 October2002 ICS13.030.40 Englishversion CharacterizationofwasteDigestionforsubsequent determinationofaquaregiasolubleportionofelements CaractrisationdesdchetsDigestionenvuedela dterminationultrieuredelapartdeslmentssolubles dansleaurgalecontenusdanslesdchets CharakterisierungvonAb
9、fllenAufschlusszur anschlieendenBestimmungdesinKnigswasser lslichenAnteilsanElementeninAbfllen ThisEuropeanStandardwasapprovedbyCENon19August2002. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwith
10、outanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaC
11、ENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal,Spain,Sweden,Switzerland
12、andUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2002CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN13657:2002EEN13657:2002(E) 2 Contents pa
13、ge Foreword3 Introduction .4 1 Scope5 2 Normativereferences 5 3 Termsanddefinitions . 5 4 Safetyremarks .6 5 Sample6 5.1 Samplepretreatment .6 5.2 Massoftestportion .7 6 Equipment 7 6.1 Closedvesselsystem .7 6.1.1 Microwaveunit 7 6.1.2 Digestionvessels. .7 6.2 Semiopenvesselsystem . 8 6.2.1 Microwav
14、eunit 8 6.2.2 Digestionvessels. .8 6.3 Apparatusforthermalheatingdigestion . 8 6.3.1 Reactionvessels .8 6.3.2 Refluxcondenser 8 6.3.3 Absorptionvessel. .8 6.3.4 Roughenedglassbeards 8 6.3.5 Temperaturecontrolledheatingapparatus 8 6.4 Generalequipment. .8 7 Reagents.9 8 Interferencesandsourcesoferror
15、 9 8.1 Generalinformations .9 8.2 Closedvesselsystem .9 8.3 Semiopenvesselsystemformicrowaveorthermalheatingdigestion 10 9 Procedure.10 9.1 Blanktest .10 9.2 Procedureformicrowaveassisteddigestioninclosedvessels 10 9.3 Procedureformicrowaveassisteddigestioninsemiopenvessels. .11 9.3.1 Amountofsample
16、s . 11 9.3.2 Digestion .11 9.3.3 Preparationofthesolutionforanalysis 11 9.4 Procedureforthermalheatingdigestioninrefluxsystems . 11 9.4.1 Amountofsamples . 11 9.4.2 Digestion .12 9.4.3 Preparationofthesolutionforanalysis 12 10 Testreport 12 AnnexA (normative)Calibrationofthepoweradjustment .14 Annex
17、B (informative)Validation . .15 B.1 Interlaboratorystudy 15 B.2 Robustnessstudy .23 Bibliography 26EN13657:2002(E) 3 Foreword ThisdocumentEN13657:2002hasbeenpreparedbyTechnicalCommitteeCEN/TC292“Characterizationof waste“,thesecretariatofwhichisheldbyNEN. ThisEuropeanStandardshallbegiventhestatusofan
18、ationalstandard,eitherbypublicationofanidenticaltext orbyendorsement,atthelatestbyApril2003,andconflictingnationalstandardsshallbewithdrawnatthelatest byApril2003. InthisEuropeanStandardtheannexAisnormativeandtheannexeBisinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardso
19、rganizationsofthefollowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark, Finland,France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal, Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN13657:2002(E) 4 Introduction Theaimofthis
20、EuropeanStandardistodescribesuitablemethodsfortheextractionofelements inwaste, solublebydigestionwithaquaregia,i.e.aquaregiasolubleelements. Forthosetypesofwaste,wherethesamplematerialbythedescribeddigestionwithaquaregiaarenotbrought totallyinsolution,theobtainedresultswillnotbethetotalamountoftheel
21、ementsinthewaste. Theobtainedresultsofaquaregiasolubleelementscannotberegardedasavailableforleaching,asthe digestionwithaquaregiaistoovigoroustorepresentnaturalprocesses.EN13657:2002(E) 5 1Scope ThisEuropeanStandardspecifiesmethodsofdigestionwithaquaregia.Solutionsproducedbythemethodsare suitablefor
22、analysise.g.byatomicabsorptionspectrometry(FLAAS,HGAAS,CVAAS,GFAAS),inductively coupledplasmaemissionspectrometry(ICPOES)andinductivecoupledplasmamassspectrometry(ICPMS). Thedigestionwithaquaregiawillnotnecessarilyreleaseallelementscompletely.Howeverformost environmentalapplicationandwastecharacteri
23、zationtheresultsfitforthepurpose. Themethodisapplicabletothedigestionofwasteforexampleforthefollowingelements:Al,Sb,As,B,Ba,Be, Ca,Cd,Cr,Co,Cu,Fe,Pb,Mg,Mn,Hg,Mo,Ni,P,K,Se,Ag,S,Na,Sr,Sn,Te,Ti,Tl,V,Zn. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisionsfromotherp
24、ublications.These normativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthelatesteditio
25、nofthe publicationreferredtoapplies(includingamendments). ENISO3696:1995, WaterforanalyticallaboratoryuseSpecificationandtestmethods(ISO3696:1987). 3 Termsanddefinitions ForthepurposesofthisEuropeanStandard,thefollowingtermsanddefinitionsapply. 3.1 aquaregia digestionsolutionobtainedbymixing1volumeo
26、fnitricacid(65%m/mto70%m/m)and3volumesof hydrochloricacid(35%m/mto37%m/m) 3.2 digestion mineralizationoftheorganicmatterofasampleanddissolutionofitsmineralpart,moreorlesscompletely, whenreactedwithareagentmixture 3.3 sample portionofmaterialselectedfromalargerquantityofmaterial ENV12506:2001 3.4 lab
27、oratorysample sampleorsubsample(s)senttoorreceivedbythelaboratory ENV12506:2001 3.5 testsample;analyticalsample sample,preparedfromthelaboratorysample,fromwhichtestportionsareremovedfortestingoranalysis ENV12506:2001EN13657:2002(E) 6 3.6 testportion;analyticalportion quantityofmaterialofpropersizefo
28、rmeasurementoftheconcentrationorotherpropertiesofinterest,removed fromthetestsample ENV12506:2001 NOTE1 Thetestportionmaybetakenfromthelaboratorysampledirectlyifnopreparationofsampleisrequired(e.g.with liquids),butusuallyitistakenfromthepreparedtestsample. NOTE2 Aunitorincrementofproperhomogeneity,s
29、izeandfineness,needingnofurtherpreparation,maybeatestportion. 3.7 dryresidue drymatterexpressedasapercentagebymassafterdryingat105C5Ctotheconstancyofweight 3.8 digestionvessel specialflaskwherethetestportionandtheacidmixturearefilledinandthedigestionisperformed 3.9 microwaveunit wholemicrowavedigest
30、ionsystem(ovenandassociatedequipment) 3.10 microwaveunitcavity theinnerpartofthemicrowaveunitinwhichthedigestionvesselislocatedandthemicrowavedigestionis performed 3.11 focusedmicrowaveunit microwaveunitinwhichaprecisecontroloftheelectricfieldismadebyusingawaveguide NOTE Microwavesarefocusedatthebot
31、tompartofthedigestionvessel. 4 Safetyremarks Allthisworkhastobeperformedbyskilledpersons. ThereagentsusedwithinthisENarestronglycorrosiveandpartlyverytoxic.Safetyprecautionsareabsolutely necessaryduetostrongcorrosivereagents,hightemperatureandhighpressure. Allprocedureshavetobeperformedinahoodorincl
32、osedforceventilatedequipment.Bytheuseofstrong oxidisingreagentstheformationofexplosiveorganicintermediatesispossibleespeciallywhendealingwith sampleswithahighorganiccontent.Donotopenpressurisedvesselsbeforetheyhavecooleddown.Avoid contactwiththechemicalsandthegaseousreactionproducts.Samplesandsoluti
33、onshavetobedisposedof accordingtoregulations. 5Sample 5.1 Samplepretreatment Thetestportionshouldbetransferredintothevesselasitiswithoutanypretreatmentifpossible.Thisis applicableonlyifthetestportionisrepresentativeforthelaboratorysampleandtheeffectivenessofthe digestionisproven.EN13657:2002(E) 7 If
34、theseconditionsarenotmetapretreatmentofthelaboratorysampleisnecessary.Thisprocedureshallnot changetheconcentrationoftheelementsofinterest. Pretreatmentshouldincludedryingorgrainsizereductionbelowaparticlesizeof250mforsolidwasteor homogenizingbyuseofahighspeedmixerorsonificationforliquidsamples. Them
35、assoflaboratorysamplesshallbesufficientforthemultipledigestionproceduresanddeterminationof thedryresidue. 5.2 Massoftestportion Themassoftestportionforasingledigestionhastobeselectedinaway,that: itisrepresentativeforthelaboratorysample; itcomplieswiththespecificationsofmanufacturerofthedigestionunit
36、. NOTE Iftherepresentativetestportionexceedsthemanufacturersspecificationsthetestportionshouldbedevidedinto smallerquantitiesanddigestedseperately.Theindividualdigestsshouldbecombinedpriortoanalysis. Forrepresentativityreasonmassabove200mgistobepreferred.Unlessrecommendedbythemanufacturer theamounto
37、forganiccarbonshallnotexceed100mgbecauseofsafetyreasonsinthecaseofclosed digestionvessel. 6Equipment 6.1 Closedvesselsystem 6.1.1Microwave unit Themicrowaveunitshallprovideprogrammablepowerwhichcanbeprogrammedtowithin10Wofthe requiredpower.Typicalunitsprovideanominal600Wto1200Wofpower.Ifnecessary(re
38、ferringto manufacturesspecifications)calibrationofthemicrowaveunithastobeperformed(seeannexA). ThemicrowaveunithastocomplytoEuropeanandnationalregulationsrelevanttomicrowaveradiation. Themicrowaveunitcavityhastobewellventilated.Ithastohaveanexhaustairtubewhichisconnectedtoa corrosionresistantlaborat
39、oryairoutletsystemortheinstrumentisprovidedforuseinalaboratoryhood. Allelectronicsaresufficientlyprotectedagainstcorrosionforsafeoperation.Allpartswhichcouldhavecontact withacidsortheirvapourshavetobecorrosionresistant. Themicrowaveunitshallbedesignedinawaythatguaranteeshomogeneousheatingofthesample
40、s. Themicrowaveunitcavityhastobebuiltinawaythatevenincaseofleakageorexplosionofthevesselsthe safetyoftheoperatorscanbeguaranteed.Householdinstrumentsarenotsuitableforlaboratoryuse. NOTE Themicrowaveunitshouldincludeatemperatureand/orpressurecontrolsystem. 6.1.2 Digestionvessels Thevesselsusedinthemi
41、crowaveunitshallbeequipedwithapressurerelievevalveoranothertechnical equipmentwhichavoidstheburstingofthevesselsatsuddenlyoccuringexcesspressure.Thematerialofthe vesselshastobeinerttotheacidsusedfordigestion.Thedigestionvesselshallwithstandthepressureofat least8bar.Iftheamountoforganiccarbonexceeds1
42、00mgithastobeensuredthatthedigestionvesselis capableofwithstandinghigherpressures.EN13657:2002(E) 8 6.2 Semiopenvesselsystem 6.2.1Microwave unit Themicrowaveunitshallbeequipedwithpowercontrol.Typicalunitprovidesanominal200Wor300Wof releasedpower.Ifnecessary,calibrationofthemicrowaveunithastobeperfor
43、medbythemanufacturer. ThemicrowaveunitshallcomplywithEuropeanandnationalregulationsrelevanttomicrowaveradiation. Themicrowaveunitshallbedesignedforuseinalaboratoryhood. Fumeextractionequipment,usedtoextractacidvapoursfromthereactionvesselsduringthedigestion program,shallhavesufficientflowratetopreventthereleaseofdangerousvapoursintothelaboratory. Allelectronicsshallbesufficientlyprotectedagainstcorrosionforsafeoperation.Allpartswhichcanbein contactwithacidsortheirvapoursshallbecorrosionresistant. 6.2.2 Digestionvessels Thevesselisworkingatatmospher
