CEN/TS 15864:2012

SLOVENSKI STANDARD
01-januar-2013
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Characterisation of waste - Leaching behaviour test for basic characterisation - Dynamic
Monolithic Leaching Test with continuous leachant renewal under conditions relevant for
specified scenario(s)
Charakterisierung von Abfällen - Untersuchung des Auslaugungsverhaltens für die
grundlegende Charakterisierung - Dynamisches Auslaugungsverfahren für monolithische
Abfälle mit kontinuierlicher Erneuerung des Auslaugungsmittels unter Bedingungen für
festgelegte Szenarien
Caractérisation des déchets - Essais de comportement à la lixiviation pour la
caractérisation de base - Essai de lixiviation dynamique des monolithes avec
renouvellement continu du lixiviant dans des conditions pertinentes pour des scénarios
spécifiés
Ta slovenski standard je istoveten z: CEN/TS 15864:2012
ICS:
13.030.10 Trdni odpadki Solid wastes
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

TECHNICAL SPECIFICATION
CEN/TS 15864
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
July 2012
ICS 13.030.10
English Version
Characterisation of waste - Leaching behaviour test for basic
characterisation - Dynamic monolithic leaching test with
continuous leachant renewal under conditions relevant for
specified scenario(s)
Caractérisation des déchets - Essais de comportement à la
Charakterisierung von Abfällen - Untersuchung des
lixiviation pour la caractérisation de base - Essai de Auslaugungsverhaltens für die grundlegende
lixiviation dynamique des monolithes avec renouvellement Charakterisierung - Dynamisches Auslaugungsverfahren
continu du lixiviant dans des conditions pertinentes pour für monolithische Abfälle mit kontinuierlicher Erneuerung
des scénarios spécifiés des Auslaugungsmittels unter Bedingungen für festgelegte
Szenarien
This Technical Specification (CEN/TS) was approved by CEN on 20 December 2010 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to submit their
comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS available
promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in parallel to the CEN/TS)
until the final decision about the possible conversion of the CEN/TS into an EN is reached.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United
Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2012 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 15864:2012: E
worldwide for CEN national Members.

Contents Page
Foreword . 3
Introduction . 4
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 7
4 Principle . 9
5 Reagents . 10
6 Equipment . 10
7 Sample preparation . 12
7.1 General . 12
7.2 Preparation of the test portion . 12
7.3 Determination of the geometric surface area . 12
8 Procedure . 12
8.1 Testing conditions . 12
8.1.1 General case (intermediate range of renewal rate) . 12
8.1.2 Particular case "critical renewal rate" . 14
8.1.3 Particular case “low renewal rate” . 14
8.1.4 Particular case under fixed conditions when no specific scenario is under consideration
(“not scenario-related”) . 14
8.2 Test procedure . 15
8.3 Contact periods – collection scheme . 16
8.4 Weight loss of the monolithic waste during the test . 16
8.5 Further preparation of the eluates for analysis . 17
8.6 Blank test . 17
9 Calculations . 18
9.1 Expression of results . 18
9.1.1 Expression of results in concentrations . 18
9.1.2 Expression of result in terms of surface related release . 18
9.2 Average surface-related release rate . 19
10 Documentation and test report . 19
11 Test performance . 21
Annex A (informative) Identification of release mechanisms and use of test results . 22
A.1 Introduction . 22
A.2 Examples of factors influencing the leaching of monolithic waste . 22
A.3 Long term release prediction . 25
Annex B (normative) Particular case "renewal rate without retro-action" . 27
B.1 Introduction . 27
B.2 Determination of the critical surface-related flow rate . 27
Annex C (informative) Examples of scheme of installation . 29
Annex D (normative) Particular case “low renewal rate” . 31
D.1 Introduction . 31
D.2 Procedure . 31
Annex E (informative) Process map for CEN/TS 15864 . 33
Bibliography . 35

Foreword
This document (CEN/TS 15864:2012) has been prepared by Technical Committee CEN/TC 292
“Characterization of waste”, the secretariat of which is held by NEN.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent rights.
This document has been developed primarily to support the requirements for leaching behaviour testing
within EU and EFTA countries.
This document was elaborated on the basis of:
 AFNOR XP X30-450:2002;
 AFNOR XP X30-467:2002;
 AFNOR XP X30-469:2007.
This document specifies a dynamic leaching test for monolithic waste materials, to determine key
parameters to address the leaching behaviour of monolithic waste materials.
For the complete characterization of the leaching behaviour of waste under specified conditions the
application of other test methods is required, (see EN 12920).
Anyone dealing with waste and sludge analysis should be aware of the typical risks of that kind of material
irrespective of the parameter to be determined. Waste and sludge samples can contain hazardous (e.g. toxic,
reactive, flammable, infectious) substances, which can be liable to biological and/or chemical reaction.
Consequently these samples should be handled with special care. Gases which can be produced by
microbiological or chemical activity are potentially flammable and will pressurise sealed bottles. Bursting
bottles are likely to result in hazardous shrapnel, dust and/or aerosol. National regulations should be
followed with respect to all hazards associated with this method.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to announce this Technical Specification: Austria, Belgium, Bulgaria, Croatia, Cyprus,
Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany,
Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.

Introduction
In the different European countries, tests have been developed to characterize and assess the constituents
which can be leached from waste materials. The release of soluble constituents upon contact with water is
regarded as one of the main mechanism of release which results in a potential risk to the environment during
life-cycle of waste materials (disposal or re-use scenario). 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 single standard.
Procedures to characterize the behaviour of waste materials can generally be divided into three steps, using
different tests in relation to the objective. The following test hierarchy is taken from the Landfill Directive
and the Decision on Annex II of this Directive for disposal of waste.
a) Basic characterization constitutes a full characterization of the waste by gathering all the necessary
information for a safe management of the waste in the short and long term. Basic characterization may
provide information on the waste (type and origin, composition, consistency, leachability,etc.),
information for understanding the behaviour of waste in the considered management scenario,
comparison of waste properties against limit values, and detection of key variables (critical parameters
as liquid/solid (L/S) ratios, leachant composition, factors controlling leachability such as pH, redox
potential, complexing capacity and physical parameters) for compliance testing and options for
simplification of compliance testing. Characterization may deliver ratios between test results from basic
characterization and results from simplified test procedures as well as information on a suitable
frequency for compliance testing. In addition to the leaching behaviour, the composition of the waste
should be known or determined by testing. The tests used for basic characterization shouldlways
include those to be used for compliance testing.
b) Compliance testing is used to demonstrate that the sample of today fits the population of samples
tested before by basic characterization and through that, is used to carry out compliance with regulatory
limit values. The compliance test should therefore always be part of the basic characterization program.
The compliance test focuses on key variables and leaching behaviour identified by basic
characterization tests. Parts of basic characterization tests can also be used for compliance purposes.
c) 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 characterization or compliance tests. On-site verification tests are not necessarily
leaching tests.
The test procedure described in this document is a basic characterization test and falls in category a).
According to EN 12920 the evaluation of the release of constituents from waste materials in a certain
scenario involves the performance of various tests. This document describes one of the parametric test that
can be used for such purposes, especially for monolithic waste.
The test procedure allows the determination of the release under dynamic conditions of constituents from a
monolithic waste material, as a function of time. This release is calculated from the concentrations of the
constituents measured in the solution (eluate) that is collected in a certain number of separate fractions.
The composition, the temperature and the renewal rate of this solution are chosen for the test in order to
study the behaviour of the waste material under fixed conditions when no specific scenario is under
consideration or according to the conditions defined by the disposal or utilisation scenario under
consideration.
Three main ranges of renewal rates can be distinguished and addressed by this document:

Council Directive 1999/31/EC of 26 April 1999 on the landfill of waste.
Council Decision 2003/33/EC of 19 December 2002.
 high renewal rate above a so-called “critical renewal rate” for which the released elements do not
influence the release (so-called “no retro-action situation”);
 “low renewal rate” which corresponds to a quasi “saturation” of the solution in the reactor in order to
reach stationary conditions (i.e. close to “saturation” equilibrium);
 intermediate range for which the released elements influence the release, but the concentrations remain
significantly below saturation.
Results of this test, combined with those from other tests (e.g. CEN/TS 14429) and the use of more or less
sophisticated models, allow the identification of the main leaching mechanisms that can be distinguished,
such as diffusion, dissolution of constituents, initial surface wash-off, dissolution of the matrix (see Annex A).
These intrinsic properties can be used to predict the release of constituents at a given time frame, in order to
assess the leaching behaviour of monolithic waste materials in practical situations or scenarios as defined in
EN 12920.
NOTE At low L/A conditions, pore water conditions in monolithic specimens can be approached.
1 Scope
This Technical Specification is applicable for determining the leaching behaviour of monolithic wastes under
dynamic conditions. The test is performed under experimental conditions relevant to assess the leaching
behaviour in view of the considered scenario(s). This test is aimed at determining the release as a function
of time of inorganic constituents from a monolithic waste, when it is put into contact with an aqueous solution
(leachant).
In general, the composition, the temperature and the continuous renewal rate of the leachant are chosen
such that the leaching behaviour of the waste material can be studied in view of the considered disposal or
recovery scenario. When the release is to be determined without any reference to a specific scenario, the
leachant is demineralised water, the temperature and the continuous renewal rate are fixed.
This dynamic monolithic leaching test (DMLT) is a parameter specific test as specified in EN 12920 and is
then not aimed at simulating real situations. The application of this test method alone is not sufficient for the
determination of the detailed leaching behaviour of a monolithic waste under specified conditions.
In the framework of EN 12920 and in combination with additional chemical information, the test results are
used to identify the leaching mechanisms and their relative importance. The intrinsic properties can be used
to predict the release of constituents at a given time frame, in order to assess the leaching behaviour of
monolithic waste materials, placed in different situations or scenarios (including disposal and utilisation
scenarios).
The test method applies to regularly shaped test portions of monolithic wastes with minimum dimensions of
40 mm in all directions that are assumed to maintain their integrity over a time frame relevant for the
considered scenario. The test method applies to test portions for which the geometric surface area can be
determined with the help of simple geometric equations. The test method applies to low permeable
monolithic materials.
NOTE 1 If, in order to comply with the requirements of regular shape, the test portion is prepared by cutting or coring,
then new surfaces are exposed which can lead to change(s) in leaching properties. On the other hand if the test portion
is prepared by moulding, the surface will be dependent to the type of mould and the conditions of storage. If the intention
is to evaluate the behaviour of the material core, the specimen needs to be stored without any contact with air to avoid
carbonation.
-8 -1
NOTE 2 For monolithic waste materials with a saturated hydraulic conductivity higher than 10 m⋅s , water is likely to
percolate through the monolith rather than flow around it. In such cases, relating the release to the geometric surface
area can lead to misinterpretation. A percolation test is then more appropriate (e.g. CEN/TS 14405).
This procedure may not be applicable to materials reacting with the leachant, leading for example to
excessive gas emission or an excessive heat release.
This document has been developed to determine the transfer of mainly inorganic constituents from wastes. It
does not take into account the particular characteristics of organic constituents nor the consequences of
microbiological processes in organic degradable wastes.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated references,
the latest edition of the referenced document (including any amendments) applies.
EN 12920:2006, Characterization of waste — Methodology for the determination of the leaching behaviour
of waste under specified conditions
EN 16192, Characterization of waste  Analysis of eluates
EN 14346, Characterization of waste — Calculation of dry matter by determination of dry residue or water
content
EN 15002, Characterization of waste — Preparation of test portions from the laboratory sample
EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696)
EN ISO 5667-3, Water quality — Sampling — Part 3: Guidance on the preservation and handling of water
samples (ISO 5667-3)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
critical surface-related flow rate
C
SF
R
minimum surface-related flow rate above which the no-retro action situation is fulfilled for a given
temperature and composition of the leachant (see Annex B)
-2 -1 -1
Note 1 to entry: The critical surface-related flow rate is expressed in ml⋅cm ⋅h or cm⋅h .
3.2
eluate
solution obtained from a leaching test
[SOURCE: EN 12457-1:2002, 3.2]
3.3
flow rate
F
R
quantity of leachant, expressed in volume unit, passing through the reactor containing the sample holder and
the test portion per time unit
-1
Note 1 to entry: The flow rate is expressed in ml⋅h .
3.4
laboratory sample
sample or sub-sample(s) sent to or received by the laboratory
[SOURCE: IUPAC:1997, 3.4]
Note 1 to entry: When the laboratory sample is further prepared (reduced) by subdividing, cutting, sawing, coring, 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 sampling but it is the initial
sample from the point of view of the laboratory.
Note 2 to entry: Several laboratory samples may 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.
3.5
leachant
liquid that is brought into contact with the test portion in the leaching procedure
Note 1 to entry: For the purpose of this document the leachant is water as specified in 5.1 for the case described
under 8.1.4 or a specific leachant for the cases described in 8.1.1, 8.1.2 and 8.1.3.
3.6
leachant renewal
continuous addition of leachant that flows through the tank as specified in 6.2.2 in an open curl
3.7
leaching behaviour of a waste
release and change with time in release from the waste upon contact with a leachant under the conditions
specified in the scenario, especially within the specified time frame
[SOURCE: EN 12920:2006, 3.7]
3.8
liquid volume to surface area ratio
L/A
ratio between the amount of liquid (L) in the reactor which, at any time of the test, is in contact with the
monolith, and the surface area of the test portion (A)
-2
Note 1 to entry: L/A is expressed in ml·cm .
Note 2 to entry: L/A has a constant value all along the test.
3.9
monolithic waste
waste which has certain minimum dimensions and physical and mechanical properties that ensure its
integrity over a certain period of time in the considered scenario
[SOURCE: EN 12457-1:2002, 3.9]
3.10
no retro-action situation
situation in which the release of constituents into the leachant does not depends on the constituents already
released from the test portion
3.11
release
emission of constituents from a waste, which pass through the external surface of the waste mass, as
specified in the considered scenario
[SOURCE: EN 12920:2006, 3.11]
3.12
release mechanism
physico-chemical processes that control the release of constituents from a solid into solution (leaching)
Note 1 to entry: In the case of monolithic materials, examples of these processes are diffusion, dissolution of
constituents, initial surface wash-off, dissolution of the matrix.
3.13
renewal rate
ratio of the flow rate to the volume V of the solution in the reactor containing the sample holder and test
portion
-1
Note 1 to entry: The renewal rate is the number of renewal per day and is expressed in h . The renewal rate is
equivalent to a residence time.
3.14
sample
quantity that is representative of a certain larger quantity
3.15
surface-related flow rate
SF
R
ratio of the flow rate F to the surface area of the test portion
R
-2 -1 -1
Note 1 to entry: The surface-related flow rate is expressed in ml⋅cm ⋅h or cm⋅h .
3.16
surface-related release rate
mass of material that is transferred into the leachant per surface area unit and per time unit
Note 1 to entry: This rate is calculated from the concentrations of the main constituents measured in the eluate. It
can vary as a function of time.
-2 -1
Note 2 to entry: The release rate is expressed in mg⋅cm ⋅h .
3.17
test portion
amount or volume of the test sample taken for analysis, usually of known weight or volume test
[SOURCE: IUPAC:1997, 3.17]
3.18
test portion of monolithic waste of regular shape
test portion of monolithic waste for which the surface area of the test portion can be calculated on the basis
of simple geometric equations
3.19
test sample
sample, prepared from the laboratory sample, from which test portions are removed for testing or for
analysis
[SOURCE: IUPAC:1997, 3.19]
4 Principle
This document describes a method to determine as a function of time the release of constituents from a
monolithic waste material, with a leachant in contact with its surface.
The test portion of monolithic waste is placed in a reactor/leaching vessel and completely submerged all
along the leaching process.
The following set of test conditions is chosen in order to study the leaching behaviour of the waste material
in view of the considered scenario(s):
 the type of leachant;
 the leaching temperature;
-1
 the continuous renewal rate of the leachant (in h );
 the total duration of the test;
 the time intervals for eluates collection.
Three main ranges of renewal rates can be distinguished:
 high renewal rate above a so-called “critical renewal rate” for which the released elements do not
influence the release;
 “low renewal rate” which corresponds to a quasi “saturation” of the solution in the reactor in order to
reach stationary conditions (i.e. close to equilibrium);
 intermediate range for which the released elements influence the release, but the concentrations remain
significantly below saturation.
The test procedure addressed these three kinds of renewal rate.
NOTE For different scenarios in practice, which are characterized by different exposure conditions (e.g. specific
leachant or leachant renewal rate), it is generally desirable to use different set of the test conditions listed above.
When the release is to be determined without any reference to a specific scenario (see 8.1.4), a fixed set of
parameters is to be used as a basis for comparison purposes between waste materials:
 the type of leachant;
 the temperature;
 the continuous renewal surface-related flow rate (SF ) of the leachant;
R
 the total duration of the test;
 the time intervals for eluates collection.
The leachant is stirred during the leaching procedure, in order to prevent concentration gradients to occur in
the liquid phase.
The eluate is collected in several separate fractions. The eluate collection scheme is designed such that
release dynamics can be deduced from the analytical results (8.3).
The eluate fractions are filtered, and characterized physically and chemically according to existing standards
(e.g. EN 16192).
The results of the test are expressed as a function of time, in terms of both mg of the constituents released
per litre of eluate, and mg of constituents released cumulatively per m of geometric surface area of the
waste material exposed to leaching.
The main leaching mechanisms that can be distinguished and identified are:
 dissolution of constituents/solubility controlled release;
 diffusion (through the pores and/or from the surface to the bulk of the leachant);
 initial surface wash-off;
 dissolution of the matrix.
5 Reagents
Use only reagents of recognized analytical grade, unless otherwise specified.
5.1 Distilled water, demineralised water, de-ionised water or water of equivalent purity (5 < pH < 7,5) with
a conductivity < 0,1 mS/m according to grade 2 specified in EN ISO 3696.
5.2 Nitric acid, c(HNO ) = 0,1 mol/l.
6 Equipment
6.1 General
Check the materials and equipment specified in 6.2.1 to 6.2.14 before use for proper operation and absence
of interfering elements that may affect the result of the test (see 8.6).
Calibrate the equipment specified in 6.2.3, 6.2.7, 6.2.8, 6.2.9, 6.2.11 and 6.2.13.
6.2 Laboratory equipment
Usual laboratory apparatus, and in particular the following:
6.2.1 Leaching vessels or tanks of different size, glass or plastics (e.g. polymethyl methacrylate
(PMMA), polytetrafluoroethylene (PTFE), polyethylene (PE), polypropylene (PP), polyvinylchloride (PVC)),
which can be closed and/or sealed to avoid prolonged contact with the air, and apply vacuum if necessary.
Clean the vessel or tank before use by filling it with nitric acid (5.2), leaving it for at least 24 h and then
flushing it out with water (5.1).
NOTE 1 The vessel or tank may have connections to allow to apply vacuum at the beginning of the leaching
procedure.
NOTE 2 The contact with the air is kept limited to avoid uptake of CO from the air in case of leaching from alkaline
materials.
The minimum distance between the test portion and the walls of the vessel or tank shall be 1 cm, all around
the test portion.
Supports made of inert material shall be used to allow direct contact with water also on the bottom sides of
the specimen. Supports shall not affect significantly the surface area of the sample exposed to the leachant.
6.2.2 Diamond blade cutting device and/or core drilling device (dry process).
6.2.3 Analytical balance, with an accuracy of at least 1 g.
6.2.4 Device for measuring sample dimensions, with an accuracy of at least 1 mm.
6.2.5 Filtering device, 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 bars). Rinsing is compulsory.
6.2.6 Glass or plastic bottles, e.g. high density polyethylene (HDPE)/polypropylene
(PP)/polytetrafluoroethylene (PTFE)/polyethyleneterephtalate (PET).
Use bottles with an appropriate volume, and with screw cap, for eluate collection and preservation of eluate
samples (rinsed in accordance with EN ISO 5667-3).
NOTE For inorganic constituents HDPE/PP bottles are preferred, except for samples analysed for mercury.
6.2.7 Conductivity meter, with an accuracy of at least 0,1 mS/m.
6.2.8 pH meter, with an accuracy of at least 0,05 pH units.
6.2.9 Thermometer.
6.2.10 Membrane filters for filtration of the eluates, with a pore size of 0,45 µm.
6.2.11 Measuring cylinders for volume determination, with 1 % accuracy.
6.2.12 Redox potential meter, (optional).
6.2.13 Pump, peristaltic pump or equivalent device allowing the renewal of the leachant at the consider
renewal rate.
The range of flow rate covered by the pump shall be sufficiently wide so that the value of the flow rate to be
applied for renewing the leachant and/or stirring the reactor is far enough the range’s boundaries.
6.2.14 Stirring device, magnetic bar (made of or coated by inert material) or pump (6.2.13) ensuring the
recirculation of the leachant in the leaching vessels or tanks (6.2.1).
Stirring with a pump shall be done at a higher flow rate value than the range of leachant renewal rate, even
in particular case "critical renewal rate" (8.1.2).
7 Sample preparation
7.1 General
For the performance of the DMLT a test portion is required, consisting of at least one monolithic specimen or
test piece, the structure, homogeneity and composition of which shall be representative for the waste
material that is to be investigated. The specimen(s) or test piece(s) shall have a minimum dimension in all
directions of 40 mm.
NOTE 1 In order to increase the representativeness of the test portion, it can be useful to test more than one
specimen or test piece, together. The surface area of the test portion is, in that case, the total surface area of the
individual specimens or test pieces.
Minimum dimensions are relevant, in order to ensure that, even for easily leachable constituents, no
depletion occurs during the test. Minimum dimensions of 40 mm in nearly all cases suffice. However, in case
of high release rates, it is recommended to justify afterwards that no depletion has taken place (see Annex
A).
The age of waste materials/specimens is an important factor, which can influence on leaching properties. In
case the waste material results from a stabilization process (performed in the laboratory or in the practical
situation) the waste material should be cured sufficiently long to avoid major variations in leaching due to
ongoing changes in pore structure and in formation of release controlling mineral phases. When possible the
production date and/or curing time of the laboratory sample (at least if prepared in the laboratory) should be
reported in the test report.
7.2 Preparation of the test portion
A test portion is obtained from the laboratory sample, by applying EN 15002.
NOTE If, in order to comply with the requirement of regular shape, the test portion is prepared by cutting or coring,
new surfaces are exposed, which can lead to change(s) in leaching properties, compared with aged surfaces.
Store the test portion in accordance with EN 15002 to minimize changes due to the exposure to atmosphere
(drying, carbonation, etc.).
7.3 Determination of the geometric surface area
Shortly before the start of the leaching test remove dust and loose particles from the test portion by blowing
gently using compressed air (quality sufficient to avoid oil contamination).
Determine the geometric shape of the test portion by measuring the length, width, height and/or diameter of
the test portion, with an uncertainty of ± 1 mm.
Calculate the whole geometric surface area A (in cm ) based on normal calculation rules for the defined
geometric shape.
8 Procedure
8.1 Testing conditions
8.1.1 General case (intermediate range of renewal rate)
A test portion, of known mass M (g) and surface area A (cm ), of the material to be tested is inserted into a
i
reactor (leaching vessel) where it is placed in contact with, and completely submerged by all along the
leaching procedure, the leachant whose composition, temperature and renewal rate are chosen for the test
in order to study the behaviour of the material according to the conditions defined by the disposal or
utilisation scenario under consideration.
The temperature of the leachant in the reactor is maintained at a constant value (± 5 °C). The leachant is
-2 -1
renewed by a continuous supply at a constant surface related flow rate SF (in ml⋅cm ⋅h ) from a supply
R
tank containing the leachant chosen for the test, so that the release of constituents of the waste material
remains dynamic. The eluate output from the reactor is directed into a collection bottle for analysis purposes.
The surface-related flow rate is chosen in an intermediate range for which the released elements influence
the release, but the concentrations remain significantly below saturation. This range is included in the
interval between the critical flow-rate (see 8.1.2) and the low renewal rate (see 8.1.3).
When determining SF , both volumes of the reactor, and the tubing in case stirring by recirculation of the
R
leachant is performed, shall be considered.
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NOTE 1 In that general case, a surface-related flow rate of the leachant of 0,5 ml⋅cm ⋅h (0,5 cm⋅h ) can be chosen
as a starting point for cement-based monolithic waste or monolithic waste obtained by mixing waste with mineral
reagents leading to cement-like forms. It is recommended to check it afterwards, for instance by ensuring that the
measured concentrations of the considered elements in the different eluates are in the range (10 % to 90 %) of the
concentrations of the same elements measured at the same pH in the pH dependence tests (either CEN/TS 14429 or
CEN/TS 14497). See Figure A.1 in Annex A.
NOTE 2 In this procedure, the test portion is continuously submitted to a constant flow rate so that the leaching
conditions remain dynamic and unchanged all along the duration of the test.
NOTE 3 For different scenarios in practice, which are characterized by different exposure conditions (e.g. specific
leachant or leachant renewal rate), it is generally desirable to use different set of the test conditions listed above.
As the surface related flow rate SF can be insufficient to meet all the requirements of a stirred reactor (i.e.
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with homogenous concentrations in the reactor), the reactor is fitted with a stirring device either as a
dedicated device (e.g. recirculation device) or as a result of the design of the reactor. It shall fulfil the
following condition: the stirring action shall be sufficient to expose the entire surface area of the test portion
to the same conditions, also taking into account the elements previously transferred in the solution and
therefore the concentrations obtained in the solution.
The criterion to set stirring conditions is that for the selected flow rate of leachant through the reactor, the
increase of the stirring intensity does not increase anymore the selected parameter (pH or constituents’
concentration) at the output of the reactor.
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NOTE 4 For example for a surface-related flow rate of 0,5 cm⋅h (water flow rate of 50 ml⋅h and geometric surface
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area of the test portion of 96 cm ) and a static L/A ratio of 5 ml⋅cm , the water flow in the recirculation device used as
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stirring device is about 300 ml⋅min .
NOTE 5 The purpose of these requirements is to qualify an experimental setting and operating conditions. Only if a
link with a previous qualification can be demonstrated, is a new qualification unnecessary.
NOTE 6 Excessive stirring can cause the test portion to be eroded.
NOTE 7 The solution specified for the aqueous solution may reflect certain scenario conditions (according to
EN 12920).
NOTE 8 The above criterion is a requirement for the main elements. In principle it may also apply to secondary or
trace elements, with similar limitations.
The entire test portion is continuously immersed in the solution and the reactor is closed to prevent
phenomena, such as carbonation by the CO in the air.
NOTE 9 The continuous flow rate and the stirring action ensure that the test portion in contact with the leachant is not
subjected to discontinuous variations (pH excursions for instance).
The eluates are collected at the output of the reactor. The total content (eluates and deposit) of the collection
bottle is removed at different dates for analysis, with or without concentration by limited evaporation.
NOTE 10 For specific modelling purposes, it can be useful to also perform “instantaneous” eluates sampling by
collecting small fractions at specific dates at the output of the reactor. The minimum collected volume required for the
analysis is about 20 ml for most of the inorganic elements (see Annex A).
Attention should be paid that in case of concentration by heating organic substances (like DOC) could be
altered and could subsequently modify the availability of the considered elements (including inorganic
elements).
Two examples of installation are illustrated in Annex C.
8.1.2 Particular case "critical renewal rate"
The particular case specified in Annex B allows to put into contact a material with an aqueous solution in the
which is higher than
same manner as in the general case, but with a constant surface related flow rate SF
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the critical flow rate, defined and determined according to Annex A, to ensure that the released constituents
cannot affect the release (so-called no retro-action situation).
NOTE When this option is used, the criterion specified in 8.1.1 above is replaced with the critical surface-related
flow rate criterion specified in Annex B.
8.1.3 Particular case “low renewal rate”
The particular specified in Annex D allows to put into contact a material with a leachant in the same manner
as in the general case, but with a constant low surface related flow rate SF (then a low renewal rate). The
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experimental setting operates then in a “quasi-static” mode. This test allows to determine if a steady state
concentration, e.g. close to “saturation” equilibrium, is reached in the solution.
8.1.4 Particular case under fixed conditions when no specific scenario is under consideration (“not
scenario-related”)
When the release is to be determined without any reference to a specific scenario, the following set of
parameters shall be used as a basis for comparison purposes between waste materials:
 the type of leachant: demineralised water as specified in 5.1;
 the leaching temperature: room temperature: (20 ± 5) °C;
 the L/A ratio: (see NOTE 3);
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 the continuous surface-related flow rate SF : (0,5 ± 0,07) cm⋅h ;
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 the total duration of the test: 36 days ± 0,25 day;
 the time intervals for eluates collection: see Table 1.
Table 1 — Time intervals for eluates collection
Step/fraction Duration of the time Duration from the
a
interval, in days start of the test (t ), in
days
1 0,08 ± 5 % 0,08 ± 5 %
2 0,92 ±
...