1、BRITISH STANDARD BS EN 13137:2001 Characterization of waste Determination of total organic carbon (TOC) in waste, sludges and sediments The European Standard EN 13137:2001 has the status of a British Standard ICS 13.030.01 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN 1
2、3137:2001 This British Standard, having been prepared under the direction of the Sector Policy and Strategy Committee for Building and Civil Engineering, was published under the authority of the Standards Policy and Strategy Committee on 28 September 2001 BSI 28 September 2001 ISBN 0 580 38053 X Nat
3、ional foreword This British Standard is the official English language version of EN 13137:2001. The UK participation in its preparation was entrusted by Technical Committee B/508, Waste management, to Subcommittee B/508/3, Waste characterization, which has the responsibility to: A list of organizati
4、ons represented on this subcommittee 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 the BSI Standards Catalogue under the section entitled “International Standards
5、 Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does 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 d
6、oes not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and
7、promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN title page, pages 2 to 20, 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 pu
8、blication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN13137 August2001 ICS13.030.10,13.030.20 Englishversion CharacterizationofwasteDeterminationoftotalorganiccarbon (TOC)inwaste,sludgesandsediments CaractrisationdesdchetsDosageducarbone organiquetotal(COT)danslesdchets,bo
9、ueset sdiments CharakterisierungvonAbfallBestimmungdesGesamten OrganischenKohlenstoffs(TOC)inAbfall,Schlmmenund Sedimenten ThisEuropeanStandardwasapprovedbyCENon18June2001. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthesta
10、tusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation
11、undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spai
12、n,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN13137:2001EEN13137:2
13、001(E) 2 Contents page Foreword . 3 Introduction 3 1 Scope 3 2 Normativereferences . 4 3 Termsanddefinitions. 4 4 Principle . 4 5Interferences. 5 6Hazards. . 5 7Reagents . 6 8Equipment. 6 9Samplestorage . 7 10ProcedureMethodA(indirectmethod). . 7 11ProcedureMethodB(directmethod). 11 12Performancecha
14、racteristics . 14 13Testreport . 15 AnnexA informative) Additionalresultsofinterlaboratorytests. 16EN13137:2001(E) 3 Foreword ThisEuropeanStandardhasbeenpreparedbyTechnicalCommitteeCEN/TC292“Characterizationof waste“,thesecretariatofwhichisheldbyNEN. ThisEuropeanStandardshallbegiventhestatusofanatio
15、nalstandard,eitherbypublicationofan identicaltextorbyendorsement,atthelatestbyFebruary2002,andconflictingnationalstandardsshall bewithdrawnatthelatestbyFebruary2002. AnnexAofthisEuropeanStandardisinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthe followi
16、ngcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic, Denmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway, Portugal,Spain,Sweden,SwitzerlandandtheUnitedKingdom. Introduction Organiccarboninwasteaswellasinsludgesandsedimentsisfoundinva
17、riousforms.Duetothe diversityofpossibleorganiccarboncompounds,thequantitativedeterminationofallindividualorganic componentsofnaturalandanthropogenicoriginisnotpossible.Therefore,itisnecessarytorelyonthe measurementoftotalquantities.Oneoftheseistotalorganiccarbon(TOC). Thisparametermaybeusedforassess
18、ingthesuitabilityofwasteforlandfilling. 1 Scope ThisEuropeanStandardspecifiestwomethodsforthedeterminationoftotalorganiccarbon(TOC)in undriedwastesamplescontainingmorethan1gcarbonperkgofdrymatter(0,1%). Thisstandardcanbeappliedaswelltosludges,sedimentsandcomparablematerials. Whenpresent,elementalcar
19、bon,carbides,cyanides,cyanates,isocyanates,isothiocyanatesand thiocyanatesaredeterminedasorganiccarbonusingthemethodsdescribedinthisstandard.An interpretationofthemeasuredvaluemaythereforebeproblematicalincaseswherethewastecontains relevantlevelsoftheabovementionedcomponents.Ifneeded,thesecomponents
20、shallbedetermined separatelybymeansofasuitablevalidatedprocedureandberecordedinthetestreport. NOTE AtthetimeofpublicationofthisEuropeanStandardastandardizedprocedurefordeterminationof elementalcarboninwasteisnotavailable.EN13137:2001(E) 4 2 Normativereferences ThisEuropeanStandardincorporatesbydated
21、orundatedreference,provisionsfromotherpublications. Thesenormativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelisted hereafter.Fordatedreferences,subsequentamendmentstoorrevisionsofanyofthesepublications applytothisEuropeanStandardonlywhenincorporatedinitbyamendmentorrevis
22、ion.Forundated referencesthelatesteditionofthepublicationreferredtoapplies(includingamendments). ISO3733, PetroleumproductsandbituminousmaterialsDeterminationofwaterDistillationmethod. ISO84661,WaterqualityCalibrationandevaluationofanalyticalmethodsandestimationof performancecharacteristicsPart1:Sta
23、tisticalevaluationofthelinearcalibrationfunction. ISO6296 ,PetroleumproductsDeterminationofwaterPotentiometricKarlFischertitrationmethod. ISO11465, SoilqualityDeterminationofdrymatterandwatercontentonamassbasisGravimetric method. EN12880, CharacterizationofsludgesDeterminationofdryresidueandwatercon
24、tent . 3 Termsanddefinitions ForthepurposesofthisEuropeanStandard,thefollowingtermsanddefinitionsapply: 3.1 totalcarbon(TC) thequantityofcarbonpresentinwasteintheformoforganic,inorganicandelementalcarbon 3.2 totalinorganiccarbon(TIC) thequantityofcarbonthatisliberatedascarbondioxidebyacidtreatment 3
25、.3 totalorganiccarbon(TOC) thequantitycarbonthatisconvertedintocarbondioxidebycombustionandwhichisnotliberatedas carbondioxidebyacidtreatment NOTE BeawarethattheabovedefinitionsarevalidforthisEuropeanStandardonlyanddonotcomply completelywithscientificdefinitionsofTC,TOCandTIC. 4P r i n c i p l e The
26、TOCcanbemeasuredeitherbyMethodA(indirectprocedure)orbyMethodB(directprocedure). 4.1 MethodA(indirectprocedure) InthisproceduretheTOCisobtainedbythedifferencebetweentheresultsofthemeasurementsofTC andTIC. Thetotalcarbon(TC)presentintheundriedsampleisconvertedtocarbondioxidebycombustioninan oxygencont
27、aininggasflowfreeofcarbondioxide.Toensurecompletecombustion,catalystsand/or modifierscanbeused.Thereleasedamountofcarbondioxideismeasuredbyinfraredspectrometry, gravimetry,coulometry,conductometry,thermalconductivitydetection,flameionizationdetectionafter reductiontomethane,orothersuitabletechniques
28、.EN13137:2001(E) 5 TheTICisdeterminedseparatelyfromanothersubsamplebymeansofacidificationandpurgingofthe releasedcarbondioxide.Thecarbondioxideismeasuredbyoneofthetechniquesmentionedabove. 4.2MethodB(directprocedure) Inthisprocedurethecarbonatespresentintheundriedsamplearepreviouslyremovedbytreating
29、the samplewithacid.Thecarbondioxidereleasedbythefollowingcombustionstepismeasuredbyoneof thetechniquesmentionedin4.1andindicatestheTOCdirectly. 4.3ApplicabilityofMethodsAorB MethodsAandBhavethesameapplicabilityinthetermsofTOCcontentand/orTICtoTOCratio. MethodBmayleadtoincorrectresultsinfollowingcase
30、s: thesamplecontainsvolatilesubstancesthatevaporateduringtheacidification(e.g.volatile hydrocarbonsfromsludgeofoilseparators); sidereactionsbetweenthesampleandtheacidtakeplace(e.g.decarboxylation,volatilereaction products). Iftheserestrictionscanbeexcluded,MethodsAandBleadtocomparableresults.Incaseo
31、fdoubt, MethodAshouldbepreferred. NOTE ThequalityofresultsofMethodBismoredependantonexperienceandpractice,especiallyregarding thestepsbeforecombustion. 5Interferences Volatileorganicsubstancesmaybelostduringsamplepreparation.Ifnecessary,thecarboncontent resultingfromvolatileorganicsubstancesshallbed
32、eterminedseparately. TheproceduresmayleadtounreliableTOCresultsiftheTICtoTOCratioisveryhigh(e.g. 10). Dependingonthedetectionmethodused,differentinterferencesmayoccur,forinstance: thepresenceofcyanidecaninterferewiththecoulometricdetectionofTICbymodifyingthepHvalue (dissolutionofHCN); highcontentofh
33、alogenatedcompoundsmayleadtoanoverestimationofTOCwhencoulometric detectionisused;insomecasestheclassicalsilverorcoppertrapcanbeinsufficienttoabsorball halides. 6Hazards Samplesmaybeliabletofermentationandmaybeinfectious.Duetothisitisrecommendedtohandle thesesampleswithspecialcare.Thegaseswhichmayocc
34、urduetothemicroorganismactivitiesare potentiallyflammable.Excessivepressurebuildupmaycausethesamplecontainertoburst,potentially resultingintheformationofinfectiousaerosolsandcontaminatedshrapnel. Harmfulcompoundsmayariseduringthecombustionprocessandduringtheacidtreatment.Theuser hastotakeappropriate
35、precautions(e.g.activatedcarbonfilters)toavoidthesegettingintothelaboratory environment. Sampleswithahighorganiccontentmayexplodeatintroductionintothefurnace.Thisriskcanbe reducedbyusinglesssampleorcoveringthesamplewithinertmaterial.EN13137:2001(E) 6 7Reagents 7.1General Allreagentsusedshallbeatleas
36、tofanalyticalgradeandsuitablefortheirspecificpurposes. Hygroscopicsubstancesshallbestoredinadesiccator. 7.2Calciumcarbonate ,CaCO 3 7.3Sodiumcarbonate ,Na 2 CO 3 ,anhydrous 7.4Tetrasodiumethylenediaminetetraacetatetetrahydrate ,Na 4 EDTA4H 2 O, C 10 H 12 N 2 O 8 Na 4 4H 2 O,heatedat80Cfortwohours. N
37、OTE OtherformsofNa 4 EDTAhydratesmaybeusedifthewatercontentisexactlyknown.Thenthe compositionofthecontrolmixtureshastoberecalculatedaccordingly(seealso7.8and7.9). 7.5Potassiumhydrogenphthalate ,C 8 H 5 O 4 K 7.6Sodiumsalicylate ,C 7 H 5 O 3 Na 7.7Aluminiumoxide ,Al 2 O 3 ,neutral,granularsize200m,an
38、nealedat600C 7.8ControlmixtureA :sodiumcarbonate(7.3),Na 4 EDTA4H 2 O(7.4)andaluminiumoxide(7.7)ina massratioof2,34:1,00:1,97. Themixtureshallbehomogenized.Itshouldcontain50,00g/kgTICand50,00g/kgTOC(e.g.44,13gof sodiumcarbonate,18,83gofNa 4 EDTA4H 2 O,37,04gofaluminiumoxide). 7.9ControlmixtureB :sod
39、iumsalicylate(7.6),calciumcarbonate(7.2),Na 4 EDTA4H 2 O(7.4)and aluminiumoxide(7.7)inamassratioof1,00:4,36:1,97:8,40. Themixtureshallbehomogenized.Itshouldcontain33,3g/kgTICand66,6g/kgTOC(e.g.6,36gof sodiumsalicylate,27,78gofcalciumcarbonate,12,50gofNa 4 EDTA4H 2 O,53,36gofaluminium oxide). 7.10Non
40、oxidizingmineralacid usedforcarbondioxideexpulsion,e.g.phosphoricacidH 3 PO 4 (w=85%) 7.11Synthetic air, nitrogen, oxygen, argon ,freeofcarbondioxideandorganicimpuritiesin accordancewiththemanufacturersinstructions 8Equipment 8.1Homogenizationdevice ,forexamplemixers,stirrers,grinders,mills 8.2Analy
41、ticalbalance ,accuratetoatleast0,5%oftestportionweight 8.3Equipmentfordeterminationofcarbon insolids;withaccessories 8.4PurgingunitforTICdetermination (toMethodAonly)EN13137:2001(E) 7 9Samplestorage Thesamplesarecollectedinglassorothersuitablecontainers.Biologicallyactivesamplesshouldbe analysedimme
42、diatelyorstoredat,atleast18C.Forbiologicallyinactivesamplesspecialpreservation maynotbenecessary. 10ProcedureMethodA(indirectmethod) 10.1Samplepreparation Thesamplessuppliedforanalysisshouldbeashomogeneousaspossibleandundried. Dependingonthenatureandappearanceofthesampledifferentprocedurescanbeused,
43、forexample: a) Solidsamplesmaybedirectlycomminuted(avoidingheat)andreducedtoagranularpowder, preferableparticlesizelessthan200m. b) Moistorpastelikesamplesmaybemixedwithaluminiumoxide(7.7)untilgranularmaterialis obtainedandthencomminuted,preferableparticlesizelessthan200m.Inthiscasetheratioof aluminiumoxidetosampleshallbeconsideredinthecalculationofTOC(10.6or11.6). Ifsamplescontainaccordingtotheaccuracyofthemethodnegligibleamountsofvolatilecompounds exceptwater,thesamplesmaybedriedat105Cbeforehomogenization.Foranalysingliquidsludges, especiallysewages
