SIST EN 12457-4:2004

SLOVENSKI STANDARD
SIST EN 12457-4:2004
01-januar-2004
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Characterisation of waste - Leaching - Compliance test for leaching of granular waste
materials and sludges - Part 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)
Charakterisierung von Abfällen - Auslaugung - Übereinstimmungsuntersuchung für die
Auslaugung von körnigen Abfällen und Schlämmen - Teil 4: Einstufiges
Schüttelverfahren mit einem Flüssigkeits-/Feststoffverhältnis von 10 l/kg für Materialen
mit einer Korngröße unter 10 mm (ohne oder mit Korngrößereduzierung)
Caractérisation des déchets - Lixiviation - Essai de conformté pour la lixiviation des
déchets fragmentés et des boues - Partie 4: Essai en bâchée unique avec un rapport
liquide/solide de 10 l/kg et une granularité inférieure a 10 mm (sans ou avec réduction de
la granularité)
Ta slovenski standard je istoveten z: EN 12457-4:2002
ICS:
13.030.10 Trdni odpadki Solid wastes
13.030.20 7HNRþLRGSDGNL%ODWR Liquid wastes. Sludge
SIST EN 12457-4:2004 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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EUROPEAN STANDARD
EN 12457-4
NORME EUROPÉENNE
EUROPÄISCHE NORM
September 2002
ICS 13.030.10; 13.030.20
English version
Characterization of waste - Leaching - Compliance test for
leaching of granular waste materials and sludges - Part 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)
Caractérisation des déchets - Lixiviation - Essai de Charakterisierung von Abfällen - Auslaugung -
conformité pour la lixiviation des déchets fragmentés et des Übereinstimmungsuntersuchung für die Auslaugung von
boues - Partie 4: Essai en bâchée unique avec un rapport körnigen Abfällen und Schlämmen - Teil 4: Einstufiges
liquide/solide de 10 l/kg et une granularité inférieure à 10 Schüttelverfahren mit einem Flüssigkeits-
mm (sans ou avec réduction de la granularité) /Feststoffverhältnis von 10 l/kg für Materialen mit einer
Korngröße unter 10 mm (ohne oder mit
Korngrößereduzierung)
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 European
Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national
standards 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 translation
under the responsibility of a CEN member into its own language and notified to the Management Centre has the same status as the official
versions.
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 STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2002 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 12457-4:2002 E
worldwide for CEN national Members.

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EN 12457-4:2002 (E)
Contents
Foreword.3
Introduction .4
1 Scope .5
2 Normative references .5
3 Terms and definitions.6
4 Compliance test .7
4.1 Principle.7
4.2 Equipment and reagents .7
4.3 Sampling strategy and sample preparation.8
5 Procedure .10
5.1 Testing conditions .10
5.2 Description of the procedure.10
5.3 Further preparation of the eluate for analysis .11
5.4 Blank test for the verification of the leaching procedure .11
6 Calculation.12
7 Documentation and test report.12
7.1 Sample preparation .12
7.2 Production of eluate .13
7.3 Analytical determination .13
7.4 Calculations and blank test information .13
8 Performance characteristics.14
8.1 Objective of the validation .14
8.2 Validation study .14
8.3 Validation results .15
8.4 Summary of the performance characteristics evaluation .17
Annex A (informative) Information on the influence on the test results of the parameters that affect
leaching.19
Annex B (informative) Test for determining whether waste is in the liquid state.21
Annex C (informative) Example of datasheet for EN 12457-4 .22
Annex D (informative) Process map for EN 12457-4.23
Annex E (informative) Example of a specific liquid-solid separation procedure for soil sample.25
Annex ZA Informative National deviation A from France.26
Bibliography .27
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EN 12457-4:2002 (E)
Foreword
This document (EN 12457-4:2002) has been prepared by Technical Committee CEN /TC 292, "Characterisation of
waste", 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 or
by endorsement, at the latest by June 2003, and conflicting national standards shall be withdrawn at the latest by
June 2003.
This document has been prepared under a mandate given to CEN by the European Commission and the European
Free 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 following
countries 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 and
EFTA countries.
This document was elaborated on the basis of :
DIN 38414-S4:1984
AFNOR X-31 210:1992
NEN 7343:1992
ÖNORM S 2072:1990
No 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.
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EN 12457-4:2002 (E)
Introduction
In the different European countries, tests have been developed to characterise and assess the constituents which
can be leached from waste materials. The release of soluble constituents upon contact with water is regarded as a
main mechanism of release which results in a potential risk to the environment during the reuse or disposal of
waste materials. The intent of these tests is to identify the leaching properties of waste materials. The complexity of
the leaching process makes simplifications necessary.
Not all of the relevant aspects of leaching behaviour can be addressed in one standard. Tests to characterise
waste 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 leaching
behaviour 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 are
addressed in these tests ;
(2) "Compliance" tests are used to determine whether the waste complies with specific reference values. The
tests 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 which
has 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 leaching
process:
EN 12457-1, 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).
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 content
and 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 principle
of each part. For given wastes the results can be different for the different procedures. There are six annexes to
this European Standard giving useful information on the selection of the appropriate procedure, reference
documents 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. This
choice has to be made by the organisation establishing the compliance requirements.
This European Standard specifies a compliance test. For basic characterisation, a methodology for the
determination of the leaching behaviour of waste has been developed within TC 292 and formulated in ENV 12920.
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EN 12457-4:2002 (E)
1 Scope
This part of four European Standards 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 10 l/kg dry matter. It applies to waste which has a particle size below 10 mm without or with size reduction (as
specified in 4.3.2)
NOTE 1 In some cases, it could be useful to test the material with coarser particles up to 40 mm in diameter. This requires a
larger amount for material and liquid. In this particular case, particle size distribution related differences in leaching may be
more pronounced than in the standard procedure.
This European Standard has been developed to investigate mainly inorganic constituents from wastes. It does not
take into account the particular characteristics of non-polar organic constituents nor the consequences of
microbiological processes in organic degradable wastes.
The test procedure specified in this European Standard produces an eluate which shall subsequently be
characterised physically and chemically according to appropriate standard methods.
NOTE 2 This procedure cannot be applicable to materials with a water content or such a water affinity that a good mixing of
the solid with the predetermined quantity of liquid is not achievable.
NOTE 3 This procedure cannot be applicable to materials reacting with the leachant, leading, for example, to excessive gas
emission, a solidifying effect or an excessive heat release.
NOTE 4 By crushing the material, new surfaces are exposed which may lead to a change in leaching properties.
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 references
This European Standard incorporates by dated or undated reference, provisions from other publications. These
normative references are cited at the appropriate places in the text, and the publications are listed hereafter. For
dated references, subsequent amendments to or revisions of any of these publications apply to this European
Standard only when incorporated in it by amendment or revision. For undated references the latest edition of the
publication referred to applies (including amendments).
ENV 12506, Characterization of waste - Analysis of eluates - Determination of pH, As, Cd, Cl-, Co, Cr(Vl), Cu, Mo,
2-
Ni, NO2-, Pb, total S, SO , V and Zn
4
ENV 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 (ISO
5667-3:1994).
ISO 5725-5:1998, Accuracy (trueness and precision) of measurement methods and results – Part 5: Alternative
methods 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.
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EN 12457-4:2002 (E)
3 Terms and definitions
For the purposes of this European Standard, the following terms and definitions apply.
3.1
leaching test
test during which a material is put into contact with a leachant and some constituents of the material are extracted
3.2
leachant
liquid used in a leaching test
NOTE For the purpose of this European Standard the leachant is water as specified in 4.2.15
3.3
eluate
solution recovered from a leaching test
3.4
single batch leaching test
leaching test in which a fixed amount of material is leached in one step with a fixed amount of leachant
3.5
serial batch leaching test
leaching test for two or more subsequent extractions of the same portion of material with a fresh amount of
leachant
3.6
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 dry
mass of the sample (S in kg of dry matter) abbreviated L/S and expressed in l/kg
3.7
liquid waste
waste that completely flows out of a calibrated opening, down to the upper level of the opening within a limited
period of time less than 8 h (annex B informative)
3.8
sludge
mixture of liquid and solids separated from various types of liquids as a result of natural or artificial processes
NOTE In the field of water treatment, the prevailing standards (EN 1085 and EN 12880) use the word water instead of the
word liquid.
3.9
monolithic waste
material which has certain minimum dimensions and physical and mechanical properties that ensure its integrity
over a certain period of time
3.10
granular waste
waste that is neither monolithic, liquid, gas nor sludge
3.11
dry matter content ratio (abbreviation : DR)
ratio expressed in percent between the mass of the dry residue, determined according to ISO 11465, or EN 12880
for sludges, and the corresponding raw mass
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EN 12457-4:2002 (E)
3.12
moisture content ratio (abbreviation : MC)
ratio expressed in percent between the mass of water contained in the material and the corresponding dry mass of
the material
NOTE The basis for the calculation of the moisture content is the mass of the dry residue in this European Standard, as
specified in ISO 11465 (for the determination of the water content of soil). It is to be noted that in EN 12880 (for the
determination of water content of sludges), the water content is calculated on the basis of the raw mass.
3.13
laboratory sample
sample or sub-sample(s) sent to or received by the laboratory ( IUPAC definition )
NOTE 1 When the laboratory sample is further prepared (reduced) by subdividing, mixing, grinding or by combinations of
these operations, the result is the test sample. When no preparation of the laboratory sample is required, the laboratory sample
is the test sample. A test portion is removed from the test sample for the performance of the test or for analysis. The laboratory
sample is the final sample from the point of view of sample collection but it is the initial sample from the point of view of the
laboratory.
NOTE 2 Several laboratory samples can be prepared and sent to different laboratories or to the same laboratory for different
purposes. When sent to the same laboratory, the set is generally considered as a single laboratory sample and is documented
as a single sample.
3.14
test sample
sample, prepared from the laboratory sample, from which test portions are removed for testing or for analysis
( IUPAC definition )
3.15
test portion
amount or volume of the test sample taken for analysis, usually of known weight or volume ( IUPAC definition )
4 Compliance test
4.1 Principle
The sample material, which originally or after pre-treatment has a particle size below 10 mm as defined in 4.3.2, is
brought into contact with water (4.2.15) under defined conditions. This European Standard is based on the
assumption that equilibrium or near-equilibrium is achieved between the liquid and solid phases during the test
duration (see 5.2.1). The solid residue is separated by filtration. The properties of the eluate are measured using
methods developed for water analysis adapted to meet criteria for analysis of eluates (ENV 12506, ENV 13370 and
others under development).
After the test the leaching conditions in terms of pH, conductivity and optionally redox potential dictated by the
waste are recorded.
NOTE These parameters often control the leaching behaviour of wastes and are therefore important for checking the
leaching test.
4.2 Equipment and reagents
4.2.1 Glass or high density polyethylene (HDPE)/polypropylene (PP) bottles in accordance with EN ISO 5667-3,
with a nominal volume of 1 l, glass bottles having caps of inert material, for example PTFE
(polytetrafluoroethylene). Rinsing is compulsory.
NOTE 1 For inorganic constituents HDPE/PP bottles are preferred, except for samples analysed for mercury.
NOTE 2 The volume of 1 l is selected in combination with the mass MD of 90 gram as specified in 4.3.4 in order to minimise
headspace. In case of material with low density, deviation from this requirement can be necessary while still attempting to
minimise headspace. This deviation should be documented in the test report.
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EN 12457-4:2002 (E)
4.2.2 An end-over-end tumbler (5 rpm - 10 rpm) or roller-table inducing rotation of the bottle at about 10 rpm.
NOTE Other shaking or mixing devices can be used provided that they are proven to be equivalent.
4.2.3 Filtering 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 1 Water ejection pump generally operates in the vicinity of 50 kPa.
NOTE 2 When volatile components are to be analysed, vacuum filtration should not be used.
4.2.4 Pre-rinsed or similarly clean 0,45 m membrane filters for filtration (e.g. rinsed with 0,1 mol/l HNO as
3
described in 4.2.16 and water as described in 4.2.15).
NOTE Depending 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.
4.2.5 Crushing equipment : jaw crusher or cutting device.
NOTE Due to crushing, contamination of the sample can occur to an extent which affects the leaching of some
constituents of concern e.g. cobalt and tungsten from tungsten carbide equipment or chromium, nickel and molybdenum from
stainless steel equipment.
4.2.6 Sieving equipment with sieves of 10 mm nominal screen size.
NOTE Due to sieving, contamination of the sample can occur to an extent which affects the leaching of some constituents
of concern e.g. cobalt and tungsten from tungsten carbide equipment or chromium, nickel and molybdenum from stainless steel
equipment.
4.2.7 A centrifuge operating between 3 000 and 4 000 g.
4.2.8 A device for measuring electrical conductivity.
4.2.9 A pH meter according to ENV 12506.
4.2.10 Two thermometers for air and leachant temperature measurement.
4.2.11 A redox potential meter (optional).
4.2.12 A balance with accuracy of at least 0,1 g.
4.2.13 Measuring cylinders for volume determination with 1 % accuracy.
4.2.14 A sample splitter or utensils for cone and quartering for sub-sampling of test samples (optional).
4.2.15 Distilled water, demineralised water, de-ionised water or water of equivalent purity (5 < pH < 7,5) with a
conductivity < 0,5 mS/m according to grade 3 specified in EN ISO 3696.
4.2.16 Nitric acid (HNO ) 0,1 mol/l (analytical grade).
3
4.3 Sampling strategy and sample preparation
4.3.1 Sampling strategy
Obtain a laboratory sample of at least 2 kg of the material. Use a sample splitter (4.2.14) or apply coning and
quartering to split the sample.
NOTE 1 Sampling should have been performed according to the framework for the preparation of a sampling plan for liquid
and granular waste materials including paste-like materials and sludges, under development by CEN/TC 292, in order to obtain
a representative laboratory sample.
NOTE 2 Depending on the maximum grain size, the splitting can require reduction of the coarser particles to comply with the
rules of sampling.
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EN 12457-4:2002 (E)
4.3.2 Particle size reduction
The tests shall be made on material with a grain size of at least 95 % (mass) less than 10 mm. Therefore the
laboratory sample shall be sieved (4.2.6). If oversized material exceeds 5 % (mass) the entire oversized fraction
shall 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 weight
and nature of the material shall be recorded. The method of size-reduction applied shall be documented and
recorded in the test report. Irrespective of any necessary size reduction, the separate fractions with the exception
of the non-crushable material and the material that may be used according to note under 5.4, shall be mixed to
constitute the test sample. If the laboratory sample cannot be crushed or sieved because of its moisture content, it
is allowed, only in this case, to dry the laboratory sample. The drying temperature shall not exceed 40 °C.
NOTE 1 Fibrous materials and plastics can often be size-reduced after cryogenic treatment.
NOTE 2 Any drying step can change other properties of the waste. Care should be taken to minimise such changes
NOTE 3 In order to minimise a possible contamination during sieving, fragmentation and splitting, it is recommended, before
preparing 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 notes
under 4.2.5 and 4.2.6.
NOTE 4 Important differences may occur in the leaching test results for a given material depending on the crushing
procedure and the waste material being crushed. Particle size related differences may be made evident by determining the
particle size distribution. It is to be noted that in the case of very narrow size distribution, such differences in the leaching result
may 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 ratio
The whole test sample, complying with the size criterion in 4.3.2, shall not be further dried. The mass of the dry
residue shall be determined at 105 °C 5 °C according to ISO 11465 or for sludges according to EN 12880. This
determination shall be made in parallel on a test portion different from the test portion for leaching. The dry matter
content ratio is calculated as follows :
DR = 100 M /M (1)
D W
where
DR is the dry matter content ratio (%) ;
M is the mass of the dried test portion (kg) ;
D
M is the mass of undried test portion (kg).
w
The moisture content ratio (MC in %) is calculated as follows :
MC = 100 (M - M )/M (2)
W D D
NOTE 1 The basis for the calculation of the moisture content is the mass of the dry residue in this European Standard, as
specified in ISO 11465 (for the determination of the water content of soil). It is to be noted that in EN 12880 (for the
determination of water content of sludges), the water content is calculated on the basis of the raw mass.
NOTE 2 The above moisture content determination could be not accurate enough in some cases (e.g. large amount of
volatile or unstable compounds). In such cases a direct determination of the true water content should be performed and the
moisture content calculated accordingly.
4.3.4 Preparation of test portion
Prepare from the test sample a test portion with a total mass M (measured with an accuracy of 0,1 g) containing
W
0,090 kg 0,005 kg of dry mass (M ). Use a sample splitter (4.2.14) or apply coning and quartering to split the
D
sample.
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EN 12457-4:2002 (E)
M = 100 M /DR (3)
W
D
where
DR is the dry matter content ratio (%) ;
M is the mass of the dried test portion (kg) ;
D
M is the mass of undried test portion (kg).
w
NOTE In view of the minimum requirements of sample volume for analytical purposes, it can be necessary to use a larger
test portion size and a correspondingly larger volume of leachant. This deviation from this European Standard should be
documented in the test report.
5 Procedure
5.1 Testing conditions
The compliance test for leaching shall be carried out at room temperature (20 5) °C.
5.2 Description of the procedure
5.2.1 Leaching step
Place the test portion with the total mass M corr
...