SIST EN 12457-1:2004

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
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

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

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

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

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

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 bottle. Excessive abrasion leading to significant particle size reduction shall be avoided.SIST EN 12457-1:2004

5 min. Filter the eluate almost completely over a 0,45 µm membrane filter using a vacuum or pressure filtration device(4.2.3). Rinsing of the filter with water or another solvent is not allowed after filtration.NOTE 1When volatile components have to be analysed, vacuum filtration should not be used.When filtration as specified above is not possible in less than one hour with an eluate flow rate of at least30 ml/cm2/hour, a liquid-solid separation procedure, specific for the considered case, shall be applied and reportedin details in the test report. A recommended procedure is given in annex E. The specific procedure shall not includethe use of additives.NOTE 2It is always recommended to try first to filtrate and then to centrifugate.NOTE 3Such specific liquid-solid separation procedure can include settling, pre-filtration on coarser filter, centrifugation,filtration on large size membrane filter, filtration at high pressure, filtration at increasing high pressure following a first periodwithout pressure, etc.NOTE 4Examples of additives (which cannot be used) are calcium chloride, ammonium salt……etc Measure the volume of filtered eluate VE. Measure immediately conductivity (in mS/m), temperature and pH (and optionally redox potential Eh in mV) ofthe eluate.5.3 Further preparation of the eluate for analysis5.3.1Divide the eluate into an appropriate number of sub-samples for different chemical analysis and store themaccording to the requirements in EN ISO 5667-3.5.3.2Determine the concentrations of constituents of interest using the methods of eluate analysis (ENV 12506,ENV 13370 and others).NOTEIn cases where high contents of dissolved solids (conductivity
75 mS/cm) are leached, acidification of the eluatescan lead to precipitation of salts. This can be avoided by diluting such samples 5 to 10 times prior to acidification. This additionaldilution should be taken into account in the calculations. A quantity of the undiluted sample should be acidified and retained incase the 5 to 10 dilution takes the sample below the detection limit for some determinands. Such procedure should bedocumented in the test report.5.4 Blank test for the verification of the leaching procedureBlank tests shall be carried out. A 0,44 l volume of leachant is submitted to the whole procedure (except the sievingstep, the fragmentation step and the splitting step but including the eluate analysis step).The eluate of this blank test shall fulfill the following minimum requirements : in the eluate of the blank test, theconcentration of each considered element shall be less than 20 % of the concentration determined in the eluate ofthe tested waste or less than 20 % of the concentration in the eluate of a limit value to which the measurementresult is to be compared. The elements to be considered are all the elements which are to be determined in theeluate of the tested waste.If the above requirements are not fulfilled, it is necessary to reduce the contamination.The blank test results shall not be substracted from the results of the waste leaching test.SIST EN 12457-1:2004

[(L/MD) + (MC/100)](5)WhereAis the release of a constituent at a L/S = 2 (in mg/kg of dry matter) ;Cis the concentration of a particular constituent in the eluate (in mg/l) (5.3.2) ;Lis the volume of leachant used (in l) ;MCis the moisture content ratio as defined in 3.12, expressed as a percentage of the drymass (4.3.2) andcalculated as in 4.3.3 ;MDis the dry mass of the test portion (in kg) (4.3.4).7 Documentation and test reportIn order to comply with this European Standard, the following information shall be documented in such a way thatthey are immediately available on request. In the following list, at least, the items marked with an asterisk (*) shallbe included in the test report. All the deviation from the minimum requirements of this European Standard shall alsobe documented in the test report7.1 Sample preparation reference to this European Standard* ; nature of the waste (e.g. granular waste, sludge)* ; reference of the laboratory sample* and of the accompanying documents* stipulated in the sampling standard ; date of reception in the laboratory of the laboratory sample* ; address of the laboratory and name(s) of the responsible person(s)* ; mass of the laboratory sample* ; date of the preparation of the test portion for the determination of the dry matter content ratio ; date of the preparation of the test portion for the leaching test ; storage conditions between the three above dates ;SIST EN 12457-1:2004

preparation of thetest portion from the laboratory sample
before the leaching test); -the leaching test itself and the experimental parameter variations as allowed by the tolerances; -the chemical analysis (uncertainty in the determination of concentration in the eluates).In the interlaboratory exercise to establish the uncertainty of the compliance leaching test, the contributions of thefirst two items listed above were not included. The results of the validation study are relevant to all activities carriedout on the laboratory sample including its preparation from the primary field sample.8.2 Validation studyThe validation of EN 12457-1 was carried out with 11 - 14 European laboratories on four types of waste materials.One of the wastes was tested according to the four parts of EN 12457. The wastes selected for the validation werechosen to represent a range of wastes as broad as possible, because the standard will find general applicationacross many different types of waste materials. In the validation work of parts 2 and 4, all the wastes were tested.In the validation work of parts 1 and 3, only a selection from these 7 wastes were tested (detailed information canbe found in the final report on the Validation study mentioned in the Bibliography).In the validation study the following starting points were used: The laboratory samples were all taken from one large batch of the different wastes according to the normalpractice. The normal size reduction and the normal repeated mixing were carried out as needed to obtainrepresentative laboratory samples from the large batch sample. However in the case of metallurgical slag, aseparate laboratory sample was provided to assess the difference between size reduction down to 4 mmperformed in the laboratory and size reduction down to 4 mm performed in the course of the preparation of thelaboratory samples. The experimental plan was designed by CEN/TC 292 WG 2 on the basis of each laboratory being given twolaboratory samples of each waste to be tested. This is in accordance with ISO 5725-5:1998 clause 5 dedicatedto heterogeneous material (e.g. sand or aggregate samples etc.). However, in order to verify the contribution ofthe analysis of the eluate to the overall variability of the leaching test, the participating laboratories were askedto perform a single complete leaching test on each laboratory sample and to analyse the eluates in duplicate. The wastes examined cover all the grain size classes to which the compliance leaching test applies: powderedwastes and sludges (0 µm to about 125 µm), fine-grained materials (0 mm to 4 mm) and coarse-grainedmaterials (0 mm to greater than 4 mm) after the required size reduction. Not only was testing carried out on familiar waste/component combinations (where considerable experiencewith the testing procedure has already been reported in the technical literature) but also on less familiar andpotentially difficult waste-component combinations. Wastes were chosen in this latter category where it wasexpected that one or more of the requirements would not be easily fulfilled (for example heterogeneity inmetallurgical slag, biological instability of sewage sludge). These combinations were applied in the validationtrial to give insight into the level of uncertainty that might arise for these matrices.Table 1 provides a list of the waste types chosen for testing and the selected components.SIST EN 12457-1:2004

EWC 17 05 03Sand blasting waste (SBW)
EWC 12 01 16Incinerator bottom ash (MBA)
EWC 19 01 11Metallurgical slag (MES)
EWC 10 04 01As*, Pb*, Co, Cd, NiBa, Cu*, Mo*, F, ZnBa, Cu, Mo, Sb, SO4 2-Sb, Ba, B, As , PbaThe components marked with * were analysed but were not included in the determination of the testperformance characteristics for reasons justified in Table 28.3 Validation resultsThe statistical evaluation was conducted according to ISO 5725-5:1998 clause 6 providing "robust methods fordata analysis": The average values, the repeatability standard deviation (sr test) and the reproducibility standarddeviation (sR) were obtained (Table 2). In order to compare and contrast the contribution of the analysis of theeluate to the overall uncertainty in the leaching test, Table 2 lists the repeatability standard deviation for the eluateanalysis sr,anal as obtained in the validation study.The repeatability is determined as an interval around a measurement result (i.e. "repeatability limit"). This intervalcorresponds to the maximum difference that can be expected
(with a 95% statistical confidence) between one testresult and another, both test results being obtained under the following conditions : The tests are performed inaccordance with all the requirements of the present standard by the same laboratory using its own facilities andtesting laboratory samples obtained from the same primary field sample and prepared under identical procedures.The repeatability limit was calculated using the relationship:
r test = f
sr,test
with the critical range factor f = 2.For instance, for the second line of Table 2, the repeatability limit around a measurement result of0,23 mg Sb/kg
is ± 0,19 mg Sb/kg (i.e. ± 84 % of
0,23)NOTE 1The above relationship refers to the difference that may be found between two measurement results performed eachon two laboratory samples obtained under the same conditions. The value f = 2 used in the factor f
2 corresponds to thetheoretical factor of 1,96 for a pure normal distribution at 95 % statistical confidence. Also, this value
f = 2 corresponds to theusual value k = 2 of the coverage factor recommended in the Gu
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