Characterisation of waste - Leaching - Compliance test for leaching of granular waste materials and sludges - Part 1: One stage batch test at a liquid to solid ratio of 2 l/kg for materials with high solid content and with particle size below 4 mm (without or with size reduction)

This part of European Standard specifies a compliance test providing information on leaching of granular wastes and sludges under the experimental conditions specified hereafter, and particularly a liquid to solid ratio of 2 l/kg dry matter. It applies to waste which has a particle size below 4 mm without or with size reduction. The test procedure specified in this Standard produces an eluate which shall subsequently be characterized physically and chemically according to appropriate standard methods.

Charakterisierung von Abfällen - Auslaugung - Übereinstimmungsuntersuchung für die Auslaugung von körnigen Abfällen und Schlämmen - Teil 1: Einstufiges Schüttelverfahren mit einem Flüssigkeits-/Feststoffverhältnis von 2 l/kg für Materialien mit hochem Feststoffgehalt und mit einer Korngröße unter 4 mm (ohne oder mit Korngrößenreduzierung)

Dieser Teil der Europäischen Norm legt eine Übereinstimmungsuntersuchung fest, die Informationen zur Auslaugung von körnigen Abfällen und Schlämmen unter den im Weiteren genannten experimentellen Bedingungen und insbesondere bei einem Flüssigkeits-/Feststoffverhältnis von 2 l/kg Trockenmasse liefert. Er gilt für Abfälle mit einer Korngröße unter 4 mm ohne oder mit Korngrößenreduzierung (wie in 4.3.2 angegeben).
Diese Europäische Norm wurde erstellt, um vorwiegend anorganische Bestandteile von Abfällen zu untersuchen. Sie berücksichtigt weder die besonderen Eigenschaften von nicht-polaren organischen Bestandteilen noch die Folgen von mikrobiologischen Prozessen in organischen abbaubaren Abfällen.
Durch das in der vorliegenden Norm beschriebene Prüfverfahren wird ein Eluat hergestellt, das anschließend physikalisch und chemisch nach den entsprechenden Standardmethoden charakterisiert wird.
Dieses Verfahren gilt nur für Abfall und Schlämme mit einem hohen Feststoffgehalt: der Trockenmassegehalt muss mindestens 33 % betragen. Zusätzlich ist das für die physikalische und chemische Charakterisierung des Eluats erforderliche Volumen des Eluats zu berücksichtigen. Außerdem muss der Mindesttrockenmassegehalt ausreichend groß sein, um eine akzeptable Durchmischung des Auslaugungsmittels mit der Messprobe zu ermöglichen.
ANMERKUNG 1   Dieses Verfahren kann nicht für Materialien  mit einem Wassergehalt oder Wasseraufnahmevermögen angewendet werden, die eine gute Durchmischung des Feststoffes mit der vorher bestimmten Menge der Flüssigkeit nicht ermöglichen.
ANMERKUNG 2   Dieses Verfahren  kann nicht für Materialien angewendet werden, die mit dem Auslaugungsmittel reagieren, was z. B. zu starken Gasemissionen, einer Verfestigungswirkung oder einer übermäßigen Wärmefreisetzung führen kann.
ANMERKUNG 3   Durch das Zerkleinern von Abfall werden neue Oberflächen freigesetzt, was zu einer Veränderung der Auslaugungseigenschaften führen kann.
ANMERKUNG 4   In Bezug auf den Mindesttroc

Caractérisation des déchets - Lixiviation - Essai de conformité pour la lixiviation des déchets fragmentés et des boues - Partie 1: Essai en bâchée unique avec un rapport liquide-solide de 2 l/kg et une granularité inférieure à 4 mm (sans ou avec réduction de la granularité)

La présente partie de la Norme européenne spécifie un essai de conformité fournissant des informations sur la lixiviation des déchets fragmentés et des boues dans les conditions expérimentales spécifiées ci après, et en particulier un rapport liquide solide de 2 l/kg de matière sèche. Cet essai s'applique aux déchets ayant une granularité inférieure à 4 mm sans ou avec réduction de la granularité (comme spécifié en 4.3.2).La présente Norme européenne a principalement été conçue pour étudier les constituants inorganiques des déchets. Elle ne tient pas compte des caractéristiques particulières des constituants organiques non polaires ni des conséquences de l'évolution microbiologique des déchets organiques dégradables.Le mode opératoire d'essai spécifié dans la présente Norme européenne permet d'obtenir un éluat qui doit ensuite être caractérisé du point de vue physique et chimique selon des méthodes normalisées appropriées.Ce mode opératoire s'applique uniquement aux déchets et aux boues à forte teneur en solide :  le taux de matière sèche doit être au moins supérieur à 33 %. En outre la quantité nécessaire d'éluat pour effectuer la caractérisation physique et chimique de celui-ci doit être obtenue. Le taux minimal de matière sèche doit être suffisamment important pour permettre de bien mélanger le lixiviant et la prise d'essai.
NOTE 1   Ce mode opératoire ne peut pas être appliqué aux matières ayant une teneur en eau ou une affinité avec l'eau telle qu'il est impossible de bien mélanger le solide avec la quantité prédéterminée de liquide.
NOTE 2   Ce mode opératoire ne peut pas être appliqué aux matériaux réagissant avec le lixiviant, ce qui donnerait, par exemple, une émission gazeuse excessive, un effet de solidification ou à un dégagement de chaleur trop élevé.
NOTE 3   En fragmentant le matériau, de nouvelles surfaces sont exposées, ce qui peut conduire à un changement des propriétés de lixiviation.
NOTE 4   S'agissant du taux minimal de matière sèche nécessaire pou

Karakterizacija odpadkov - Izluževanje - Preskus skladnosti za izluževanje granuliranih odpadkov in blata - 1. del: Enostopenjski šaržni preskus pri razmerju tekoče/trdno 2 l/kg za materiale z visoko vsebnostjo suhe snovi in z velikostjo delcev pod 4 mm (brez drobljenja ali z njim)

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2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.OXåHYDQMHCharakterisierung von Abfällen - Auslaugung - Übereinstimmungsuntersuchung für die Auslaugung von körnigen Abfällen und Schlämmen - Teil 1: Einstufiges Schüttelverfahren mit einem Flüssigkeits-/Feststoffverhältnis von 2 l/kg für Materialien mit hochem Feststoffgehalt und mit einer Korngröße unter 4 mm (ohne oder mit Korngrößenreduzierung)Caractérisation des déchets - Lixiviation - Essai de conformité pour la lixiviation des déchets fragmentés et des boues - Partie 1: Essai en bâchée unique avec un rapport liquide-solide de 2 l/kg et une granularité inférieure a 4 mm (sans ou avec réduction de la granularité)Characterisation of waste - Leaching - Compliance test for leaching of granular waste materials and sludges - Part 1: One stage batch test at a liquid to solid ratio of 2 l/kg for materials with high solid content and with particle size below 4 mm (without or with size reduction)13.030.20Liquid wastes. Sludge13.030.10Trdni odpadkiSolid wastesICS:Ta slovenski standard je istoveten z:EN 12457-1:2002SIST EN 12457-1:2004en01-januar-2004SIST EN 12457-1:2004SLOVENSKI

STANDARD
SIST EN 12457-1:2004

EUROPEAN STANDARDNORME EUROPÉENNEEUROPÄISCHE NORMEN 12457-1September 2002ICS 13.030.10; 13.030.20English versionCharacterization of waste - Leaching - Compliance test forleaching of granular waste materials and sludges - Part 1: Onestage batch test at a liquid to solid ratio of 2 l/kg for materialswith high solid content and with particle size below 4 mm(without or with size reduction)Caractérisation des déchets - Lixiviation - Essai deconformité pour la lixiviation des déchets fragmentés et desboues - Partie 1: Essai en bâchée unique avec un rapportliquide-solide de 2 l/kg et une granularité inférieure à 4mm(sans ou avec réduction de la granularité)Charakterisierung von Abfällen - Auslaugung -Übereinstimmungsuntersuchung für die Auslaugung vonkörnigen Abfällen und Schlämmen - Teil 1: EinstufigesSchüttelverfahren mit einem Flüssigkeits-/Feststoffverhältnis von 2 l/kg für Materialien mit hohemFeststoffgehalt und mit einer Korngröße unter 4 mm (ohneoder mit Korngrößenreduzierung)This European Standard was approved by CEN on 17 August 2002.CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this EuropeanStandard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such nationalstandards may be obtained on application to the Management Centre or to any CEN member.This European Standard exists in three official versions (English, French, German). A version in any other language made by translationunder the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the officialversions.CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.EUROPEAN COMMITTEE FOR STANDARDIZATIONCOMITÉ EUROPÉEN DE NORMALISATIONEUROPÄISCHES KOMITEE FÜR NORMUNGManagement Centre: rue de Stassart, 36

B-1050 Brussels© 2002 CENAll rights of exploitation in any form and by any means reservedworldwide for CEN national Members.Ref. No. EN 12457-1:2002 ESIST EN 12457-1:2004

EN 12457-1:2002 (E)2ContentsForeword......................................................................................................................................................................3Introduction.................................................................................................................................................................41Scope..............................................................................................................................................................52Normative references....................................................................................................................................53Terms and definitions....................................................................................................................................64Compliance test.............................................................................................................................................74.1Principle..........................................................................................................................................................74.2Equipment and reagents...............................................................................................................................74.3Sampling strategy and sample preparation................................................................................................85Procedure.....................................................................................................................................................105.1Testing conditions.......................................................................................................................................105.2Description of the procedure......................................................................................................................105.3Further preparation of the eluate for analysis..........................................................................................115.4Blank test for the verification of the leaching procedure........................................................................116Calculation....................................................................................................................................................127Documentation and test report...................................................................................................................127.1Sample preparation.....................................................................................................................................127.2Production of eluate....................................................................................................................................137.3Analytical determination.............................................................................................................................137.4Calculations and blank test information...................................................................................................138Performance characteristics.......................................................................................................................148.1Objective of the validation..........................................................................................................................148.2Validation study...........................................................................................................................................148.3Validation results.........................................................................................................................................158.4Summary of the performance characteristics evaluation.......................................................................17Annex A (informative)

Information on the influence on the test results

of the parameters that affectleaching.........................................................................................................................................................19Annex B (informative)

Test for determining whether waste is in the liquid state...............................................21Annex C (informative)

Example of datasheet for EN 12457-1...............................................................................22Annex D (informative)

Process map for EN 12457-1..............................................................................................23Annex E (informative)

Example of a specific liquid-solid separation procedure for soil sample.....................25Annex ZA (Informative)

National deviation A from France...................................................................................26Bibliography..............................................................................................................................................................27SIST EN 12457-1:2004

EN 12457-1:2002 (E)3ForewordThis document (EN 12457-1:2002) has been prepared by Technical Committee CEN /TC 292, "Characterisation ofwaste", the secretariat of which is held by NEN.This European Standard shall be given the status of a national standard, either by publication of an identical text orby endorsement, at the latest by June 2003, and conflicting national standards shall be withdrawn at the latest byJune 2003.This document has been prepared under a mandate given to CEN by the European Commission and the EuropeanFree Trade Association, and supports essential requirements of EU Directive(s).For relationship with EU Directive(s), see informative annex ZA, which is an integral part of this document.According to the CEN/CENELEC Internal Regulations, the national standards organizations of the followingcountries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland,France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Malta, Netherlands, Norway, Portugal, Spain,Sweden, Switzerland and the United Kingdom.This document has been developed primarily to support the requirements for compliance testing within the EU andEFTA countries.This document was elaborated on the basis of :DIN 38414-S4:1984AFNOR X-31 210:1992NEN 7343:1992ÖNORM S 2072:1990No existing European Standard is superseded by the publication of this European Standard.Annexes A, B, C, D, E and ZA are informative.This document includes a Bibliography.SIST EN 12457-1:2004

EN 12457-1:2002 (E)4IntroductionIn the different European countries, tests have been developed to characterise and assess the constituents whichcan be leached from waste materials. The release of soluble constituents upon contact with water is regarded as amain mechanism of release which results in a potential risk to the environment during the reuse or disposal ofwaste materials. The intent of these tests is to identify the leaching properties of waste materials. The complexity ofthe leaching process makes simplifications necessary.Not all of the relevant aspects of leaching behaviour can be addressed in one standard. Tests to characterisewaste materials and their behaviour can generally be divided into three categories :(1)"Basic Characterisation" tests are used to obtain information on the short and long term leachingbehaviour and characteristics properties of waste materials. Liquid/solid (L/S) ratios, leachant composition,factors controlling leachability such as pH, redox potential, complexing capacity and physical parameters areaddressed in these tests ;(2)"Compliance" tests are used to determine whether the waste complies with specific reference values. Thetests focus on key variables and leaching behaviour identified by basic characterisation tests ;(3)"On-site verification" tests are used as a rapid check to confirm that the waste is the same as that whichhas been subjected to the compliance test(s).The procedures described in this European Standard fall in category 2 : compliance tests.The four procedures described in the four following European Standards are based on different liquid to solid (L/S)ratios and different particle sizes because these parameters, among others, play an important role in the leachingprocess:EN 12457-1, One stage batch test at a liquid to solid ratio of 2 l/kg for materials with high solid content and withparticle size below 4 mm (without or with size reduction).EN 12457-2, One stage batch test at a liquid to solid ratio of 10 l/kg for materials with particle size below 4 mm(without or with size reduction).EN 12457-3, Two stage batch test at a liquid to solid ratio of 2 l/kg and 8 l/kg for materials with high solid contentand with particle size below 4 mm (without or with size reduction).EN 12457-4, One stage batch test at a liquid to solid ratio of 10 l/kg for materials with particle size below 10 mm(without or with size reduction).Each part specifies a distinct procedure. The specific features of each part are described in the scope and principleof each part. For given wastes the results can be different for the different procedures. There are six annexes tothis European Standard giving useful information on the selection of the appropriate procedure, referencedocuments and guidance on the limitations of these procedures.The choice of the procedure depends on the degree and type of information required for compliance testing. Thischoice has to be made by the organisation establishing the compliance requirements.This European Standard specifies a compliance test. For basic characterisation, a methodology for thedetermination of the leaching behaviour of waste has been developed within TC 292 and formulated in ENV 12920.SIST EN 12457-1:2004

EN 12457-1:2002 (E)51 ScopeThis part of four European Standards specifies a compliance test providing information on leaching of granularwastes and sludges under the experimental conditions specified hereafter, and particularly a liquid to solid ratioof 2 l/kg dry matter. It applies to waste which has a particle size below 4 mm without or with size reduction (asspecified in 4.3.2)This European Standard has been developed to investigate mainly inorganic constituents from wastes. It does nottake into account the particular characteristics of non-polar organic constituents nor the consequences ofmicrobiological processes in organic degradable wastes.The test procedure specified in this European Standard produces an eluate which shall subsequently becharacterised physically and chemically according to appropriate standard methods.This procedure is only applicable to waste material and sludges having a high solid content : the dry matter contentratio shall be at least higher than 33%. In addition, the necessary quantity of eluate shall be obtained to perform thephysical and chemical characterisation of the eluate. Furthermore, the minimum dry matter content ratio shall behigh enough to allow a sufficient mixing of the leachant and the test portion.NOTE 1This procedure cannot be applicable to materials with a water content or such a water affinity that a good mixing ofthe solid with the predetermined quantity of liquid is not achievable.NOTE 2This procedure cannot be applicable to materials reacting with the leachant, leading, for example, to excessive gasemission, a solidifying effect or an excessive heat release.NOTE 3By crushing the material, new surfaces are exposed which may lead to a change in leaching properties.NOTE 4In relation with the minimum dry matter content ratio required for obtaining enough eluate, the test portion specifiedin this European Standard of 175 gram dry matter results in a maximum volume of eluate of

175 ml if its dry matter content ratiois 50 %.When this part 1 is not applicable, the leaching test at L/S = 10 specified in part 2 can be performed.This test cannot be used alone to determine the leaching behaviour of a waste, as specified in ENV 12920.This European Standard does not address issues related to health and safety.2 Normative referencesThis European Standard incorporates by dated or undated reference, provisions from other publications. Thesenormative references are cited at the appropriate places in the text, and the publications are listed hereafter. Fordated references, subsequent amendments to or revisions of any of these publications apply to this EuropeanStandard only when incorporated in it by amendment or revision. For undated references the latest edition of thepublication referred to applies (including amendments).ENV 12506, Characterization of waste - Analysis of eluates - Determination of pH, As, Cd, Cl-, Co, Cr(Vl), Cu, Mo,Ni, NO2-, Pb, total S, SO4 2-, V and ZnENV 13370, Characterization of waste – Analysis of eluates – Determination of Ammonium–N, AOX, conductivity,Hg, phenol index, TOC, CN- easily liberatable, F-EN 12880, Characterisation of sludges – Determination of dry residue and water content.EN ISO 3696, Water for analytical laboratory use – Specification and test methods (ISO 3696:1987).EN ISO 5667-3, Water Quality - Sampling - Part 3 : Guidance on the preservation and handling of samples (ISO5667-3:1994).SIST EN 12457-1:2004

EN 12457-1:2002 (E)6ISO 5725-5:1998, Accuracy (trueness and precision) of measurement methods and results – Part 5: Alternativemethods for the determination of the precision of a standard measurement method.ISO 11465, Soil Quality - Determination of dry matter and water content on a mass basis - Gravimetric method.3 Terms and definitionsFor the purposes of this European Standard, the following terms and definitions apply.3.1 leaching testtest during which a material is put into contact with a leachant and some constituents of the material are extracted3.2 leachantliquid used in a leaching testNOTEFor the purpose of this European Standard the leachant is water as specified in 4.2.153.3 eluatesolution recovered from a leaching test3.4 single batch leaching testleaching test in which a fixed amount of material is leached in one step with a fixed amount of leachant3.5 serial batch leaching testleaching test for two or more subsequent extractions of the same portion of material with a fresh amount ofleachant3.6 liquid to solid ratio L/S (abbreviation : L/S)ratio between the total amount of liquid (L in litre), which in a leaching test is in contact with the waste, and the drymass of the sample (S in kg of dry matter) abbreviated L/S and expressed in l/kg3.7 liquid wastewaste that completely flows out of a calibrated opening, down to the upper level of the opening within a limitedperiod of time less than 8 h (annex B informative)3.8 sludgemixture of liquid and solids separated from various types of liquids as a result of natural or artificial processesNOTEIn the field of water treatment, the prevailing standards (EN 1085 and EN 12880) use the word water instead of theword liquid.3.9 monolithic wastematerial which has certain minimum dimensions and physical and mechanical properties that ensure its integrityover a certain period of time3.10 granular wastewaste that is neither monolithic, liquid, gas nor sludgeSIST EN 12457-1:2004

EN 12457-1:2002 (E)73.11 dry matter content ratio (abbreviation : DR)ratio expressed in percent between the mass of the dry residue, determined according to ISO 11465, or EN 12880for sludges, and the corresponding raw mass3.12 moisture content ratio (abbreviation MC)ratio expressed in percent between the mass of water contained in the material and the corresponding dry mass ofthe materialNOTEThe basis for the calculation of the moisture content is the mass of the dry residue in this European Standard, asspecified in ISO 11465 (for the determination of the water content of soil). It is to be noted that in EN 12880 (for thedetermination of water content of sludges), the water content is calculated on the basis of the raw mass.3.13 laboratory samplesample or sub-sample(s) sent to or received by the laboratory ( IUPAC definition )NOTE 1When the laboratory sample is further prepared (reduced) by subdividing, mixing, grinding or by combinations ofthese operations, the result is the test sample. When no preparation of the laboratory sample is required, the laboratory sampleis the test sample. A test portion is removed from the test sample for the performance of the test or for analysis.

The laboratorysample is the final sample from the point of view of sample collection but it is the initial sample from the point of view of thelaboratory.NOTE 2Several laboratory samples can be prepared and sent to different laboratories or to the same laboratory for differentpurposes.

When sent to the same laboratory, the set is generally considered as a single laboratory sample and is documentedas a single sample.3.14 test samplesample, prepared from the laboratory sample, from which test portions are removed for testing or for analysis( IUPAC definition )3.15 test portionamount or volume of the test sample taken for analysis, usually of known weight or volume ( IUPAC definition )4 Compliance test4.1 PrincipleThe sample material, which originally or after pre-treatment has a particle size below 4 mm as defined in 4.3.2, isbrought into contact with water (4.2.15) under defined conditions. This European Standard is based on theassumption that equilibrium or near-equilibrium is achieved between the liquid and solid phases during the testduration (see 5.2.1). The solid residue is separated by filtration. The properties of the eluate are measured usingmethods developed for water analysis adapted to meet criteria for analysis of eluates (ENV 12506, ENV 13370 andothers under development).After the test the leaching conditions in terms of pH, conductivity and optionally redox potential dictated by thewaste are recorded.NOTEThese parameters often control the leaching behaviour of wastes and are therefore important for checking theleaching test.4.2 Equipment and reagents4.2.1Glass or high density polyethylene (HDPE)/polypropylene (PP) bottles in accordance with EN ISO 5667-3,with a nominal volume of 500 ml, glass bottles having caps of inert material, for example PTFE(polytetrafluoroethylene). Rinsing is compulsory.NOTE 1For inorganic constituents HDPE/PP bottles are preferred, except for samples analysed for mercury.SIST EN 12457-1:2004

EN 12457-1:2002 (E)8NOTE 2The volume of 500 ml is selected in combination with the mass MD of 175 gram as specified in 4.3.4 in order tominimise headspace. In case of material with low density, deviation from this requirement can be necessary while stillattempting to minimise headspace. This deviation should be documented in the test report.4.2.2An end-over-end tumbler (5 rpm - 10 rpm) or roller-table inducing rotation of the bottle at about 10 rpm.NOTEOther shaking or mixing devices can be used provided that they are proven to be equivalent.4.2.3Filtering apparatus, either a vacuum filtration device (between 30 kPa and 70 kPa) (300 mbar to 700 mbar)or a high pressure filtration apparatus ( 0,5 MPa) (5 bar). Rinsing is compulsory.NOTE 1Water ejection pump generally operates in the vicinity of 50 kPa.NOTE 2When volatile components are to be analysed, vacuum filtration should not be used.4.2.4Pre-rinsed or similarly clean 0,45 m membrane filters for filtration (e.g. rinsed with 0,1 mol/l HNO3 asdescribed in 4.2.16 and water as described in 4.2.15).NOTEDepending on the test requirements, PTFE filter material can be required. Filter made of PTFE are hydrophobic.Before filtration of eluate, they should be wetted using ethanol or methanol provided it doesn't influence the results of analysis.4.2.5Crushing equipment : jaw crusher or cutting device.NOTEDue to crushing, contamination of the sample can occur to an extent which affects the leaching of someconstituents of concern e.g. cobalt and tungsten from tungsten carbide equipment or chromium, nickel and molybdenum fromstainless steel equipment.4.2.6Sieving equipment with sieves of 4 mm nominal screen size.NOTEDue to sieving, contamination of the sample can occur to an extent which affects the leaching of some constituentsof concern e.g. cobalt and tungsten from tungsten carbide equipment or chromium, nickel and molybdenum from stainless steelequipment.4.2.7A centrifuge operating between 3 000 and 4 000 g.4.2.8A device for measuring electrical conductivity.4.2.9A pH meter according to ENV 12506.4.2.10Two thermometers for air and leachant temperature measurement.4.2.11A redox potential meter (optional).4.2.12A balance with accuracy of at least 0,1 g.4.2.13Measuring cylinders for volume determination with 1 % accuracy.4.2.14A sample splitter or utensils for cone and quartering for sub-sampling of test samples (optional).4.2.15Distilled water, demineralised water, de-ionised water or water of equivalent purity (5 < pH < 7,5) with aconductivity < 0,5 mS/m according to grade 3 specified in EN ISO 3696.4.2.16Nitric acid (HNO3) 0,1 mol/l (analytical grade).4.3 Sampling strategy and sample preparation4.3.1 Sampling strategyObtain a laboratory sample of at least 2 kg of the material. Use a sample splitter (4.2.14) or apply coning andquartering to split the sample.SIST EN 12457-1:2004

EN 12457-1:2002 (E)9NOTE 1Sampling should have been performed according to the framework for the preparation of a sampling plan for liquidand granular waste materials including paste-like materials and sludges, under development by CEN/TC 292, in order to obtaina representative laboratory sample.NOTE 2Depending on the maximum grain size, the splitting can require reduction of the coarser particles to comply with therules of sampling.4.3.2 Particle size reductionThe tests shall be made on material with a grain size of at least 95 % (mass) less than 4 mm. Therefore thelaboratory sample shall be sieved (4.2.6). If oversized material exceeds 5 % (mass) the entire oversized fractionshall be crushed with a crushing equipment (4.2.5). On no account shall the material be finely ground. Non-crushable material (e.g. metallic parts such as nuts, bolts, scrap) in the sample shall be separated and the weightand nature of the material shall be recorded. The method of size-reduction applied shall be documented andrecorded in the test report. Irrespective of any necessary size reduction, the separate fractions with the exceptionof the non-crushable material and the material that may be used according to note under 5.4, shall be mixed toconstitute the test sample. If the laboratory sample cannot be crushed or sieved because of its moisture content, itis allowed, only in this case, to dry the laboratory sample. The drying temperature shall not exceed 40 °C.NOTE 1Fibrous materials and plastics can often be size-reduced after cryogenic treatment.NOTE 2Any drying step can change other properties of the waste. Care should be taken to minimise such changes.NOTE 3In order to minimise a possible contamination during sieving, fragmentation and splitting, it is recommended, beforepreparing the test sample, to process a portion of the laboratory sample through the devices for sieving, fragmentation, splitting,and to discard such material thereafter. This recommendation does not cover the possible contamination described in the notesunder 4.2.5 and 4.2.6.NOTE 4Important differences may occur in the leaching test results for a given material depending on the crushingprocedure and the waste material being crushed. Particle size related differences may be made evident by determining theparticle size distribution. It is to be noted that in the case of very narrow size distribution, such differences in the leaching resultmay be enhanced especially in the upper part of the size range.4.3.3 Determination of the dry matter content ratio and the moisture content ratioThe whole test sample, complying with the size criterion in 4.3.2, shall not be further dried. The mass of the dryresidue shall be determined at 105 °C

5 °C according to ISO 11465 or for sludges according to EN 12880. Thisdetermination shall be made in parallel on a test portion different from the test portion for leaching. The dry mattercontent ratio is calculated as follows :DR = 100

MD/MW(1)whereDRis the dry matter content ratio (%) ;MDis the mass of the dried test portion (kg) ;Mwis the mass of undried test portion (kg).The moisture content ratio (MC in %) is calculated as follows :MC = 100

(MW - MD)/MD(2)NOTE 1The basis for the calculation of the moisture content is the mass of the dry residue in this European Standard, asspecified in ISO 11465 (for the determination of the water content of soil). It is to be noted that in EN 12880 (for thedetermination of water content of sludges), the water content is calculated on the basis of the raw mass.NOTE 2The above moisture content determination could be not accurate enough in some cases (e.g. large amount ofvolatile or unstable compounds). In such cases a direct determination of the true water content should be performed and themoisture content calculated accordingly.SIST EN 12457-1:2004

EN 12457-1:2002 (E)104.3.4 Preparation of test portionPrepare from the test sample a test portion with a total mass MW (measured with an accuracy of 0,1 g) containing0,175 kg

0,005 kg of dry mass (MD). Use a sample splitter (4.2.14) or apply coning and quartering to split thesample.MW = 100

MD/DR(3)whereDRis the dry matter content ratio (%) ;MDis the mass of the dried test portion (kg) ;Mwis the mass of undried test portion (kg).NOTEIn view of the minimum requirements of sample volume for analytical purposes, it can be necessary to use a largertest portion size and a correspondingly larger volume of leachant. This deviation from this European Standard should bedocumented in the test report.5 Procedure5.1 Testing conditionsThe compliance test for leaching shall be carried out at room temperature (20

5) °C.5.2 Description of the procedure5.2.1 Leaching step Place the test portion with the total mass Mw corresponding to 0,175 kg

0,005 kg of dry mass MD in a bottle(4.2.1). Add an amount of leachant (L) establishing a liquid to solid ratio (L/S) = 2 l/kg

2 % during the extraction. Careshould be taken to obtain good mixing of solid and liquid.L = ( 2 – MC/100 )

MD(4)WhereLis the volume of leachant used (in l) ;MDis the dry mass of the test portion (in kg) ;MCis the moisture content ratio (in %). Place the capped bottle in an agitation device (4.2.2). Agitate for 24 h

0,5 h. During the extraction care should be taken to prevent settlement of solids in the bott

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