CEN/TS 15863:2012 (E)

CEN/TC 292

CEN/TS 15863:2012

CEN/TC 292

Secretariat: NEN

Characterization of waste — Leaching behaviour test for basic

characterization — Dynamic monolithic leaching test with periodic leachant
renewal, under fixed test conditions
Charakterisierung von Abfällen - Untersuchung des Auslaugungsverhaltens für die grundlegende Charakterisierung
- Dynamisches Auslaugungsverfahren für monolithische Abfälle mit periodischer Erneuerung des
Auslaugungsmittels unter festgelegten Prüfbedingungen

Caractérisation des déchets - Essais de comportement à la lixiviation pour la caractérisation de base - Essai de
lixiviation dynamique des monolithes avec rénovation périodique du lixiviant, dans des conditions d'essai fixes

ICS:

Descriptors:

Document type: Technical Specification

Document subtype:
Document stage: Publication
Document language: E

C:\Temp\XPGrpWise\prEN 15863_1.doc STD Version 2.2

CEN/TS 15863:2012 (E)

Contents Page

Foreword ..............................................................................................................................................................3
Introduction .........................................................................................................................................................4
1 Scope ......................................................................................................................................................6
2 Normative references ............................................................................................................................6
3 Terms and definitions ...........................................................................................................................7
4 Principle ..................................................................................................................................................8
5 Reagents .................................................................................................................................................9
6 Equipment ..............................................................................................................................................9
7 Sample preparation ............................................................................................................................ 10
7.1 General ................................................................................................................................................. 10
7.2 Preparation of the test portion .......................................................................................................... 11
7.3 Determination of the geometric surface area .................................................................................. 11
8 Procedure ............................................................................................................................................ 11
8.1 Testing conditions .............................................................................................................................. 11
8.2 Step 1 of the leaching procedure ...................................................................................................... 11
8.3 Steps 2 – 8 of the leaching procedure .............................................................................................. 12
8.4 Weight loss of the monolithic waste during the test ...................................................................... 13
8.5 Further preparation of the eluates for analysis ............................................................................... 13
8.6 Blank test ............................................................................................................................................. 14
9 Calculations......................................................................................................................................... 14
9.1 Expression of results ......................................................................................................................... 14
9.1.1 Expression of results in terms of area related release ................................................................... 14
9.1.2 Expression of results in concentrations .......................................................................................... 15
10 Documentation and test report ......................................................................................................... 15
11 Test performance ................................................................................................................................ 17
Annex A (informative) Identification of release mechanisms and use of test results .............................. 18
A.1 Introduction ......................................................................................................................................... 18
A.2 Examples of factors influencing the leaching of monolithic waste .............................................. 18
A.3 Long term release prediction ............................................................................................................ 21
Annex B (informative) Examples of data about the L/A ratio....................................................................... 23
Annex C (informative) Process map for CEN/TS 15863................................................................................ 25
Bibliography ..................................................................................................................................................... 27

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Foreword
This document (CEN/TS 15863:2012) 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: NEN 7345:1995.

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.

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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 Directive1 and
the Decision on Annex II of this Directive2 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 should always 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 fixed number of separate fractions.
Besides, the following test conditions are fixed: the type of leachant, the temperature, the liquid to surface
area ratio, and the duration of the test.

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,

1 Council Directive 1999/31/EC of 26 April 1999 on the landfill of waste.

2 Council Decision 2003/33/EC of 19 December 2002.

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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. For assessment of the leaching under equilibrium conditions (low L/A condition, pore water and/or
long contact times) there are other tools available, such as the pH dependence test CEN/TS 14429, the
percolation test for granular material CEN/TS 14405 (with L/S 0,1 l/kg to 0,5 l/kg) and the batch test for
granular waste EN 12457-1.

NOTE At low L/A conditions, pore water conditions in monolithic specimen can be approached.

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CEN/TS 15863:2012 (E)

1 Scope
This document is applicable for determining the leaching behaviour of monolithic wastes under dynamic
conditions. The test is performed under fixed experimental conditions in this document. 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).

This dynamic monolithic leaching test (DMLT) is a parameter specific test as specified in EN 12920 and is
therefore 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 recycling
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
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. In such cases relating the release to the geometric surface 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 release 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 referenced documents are indispensable for the application of this document. 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 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 16192 Characterization of waste — Analysis of eluates

EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696:1987)

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EN ISO 5667-3, Water quality — Sampling — Part 3: Guidance on the preservation and handling of water
samples (ISO 5667-3:2003)

3 Terms and definitions

For the purposes of this document, the following terms and definitions apply.

3.1
eluate
solution obtained from a leaching test

[EN 12457-1:2002]

3.2
laboratory sample
sample or sub-sample(s) sent to or received by the laboratory

[IUPAC, 1997]

NOTE 1 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 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.

3.3
leachant
liquid that is brought into contact with the test portion in the leaching procedure

NOTE For the purpose of this document the leachant is water as specified in 5.1.

3.4
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

[EN 12920:2006]

3.5
leachant renewal
selection of time intervals after which the leachant is renewed

3.6
liquid volume to surface area ratio
L/A
ratio between the amount of liquid (L) which in a given step of the test is in contact with the monolith, and the
surface area of the test portion (A)
-2
NOTE L/A is expressed in ml·cm .

3.7
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

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CEN/TS 15863:2012 (E)

(see EN 12457-1:2002)

3.8
release
emission of constituents from a waste, which pass through the external surface of the waste mass, as
specified in the considered scenario

[EN 12920:2006]

3.9
release mechanism
physico-chemical processes that control the release of constituents from a solid into solution (leaching)

NOTE In the case of monolithic materials, examples of these processes are diffusion, dissolution of constituents,
initial surface wash-off, dissolution of the matrix.

3.10
sample
quantity that is representative of a certain larger quantity

3.11
test portion
amount or volume of the test sample taken for analysis, usually of known weight or volume

[IUPAC, 1997]

3.12
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

3.13
test sample
sample, prepared from the laboratory sample, from which test portions are removed for testing or for analysis

[IUPAC, 1997]

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 in a
leachant. The leachant is introduced in the reactor up to a given volume of liquid to surface area ratio (L/A
ratio), at a given temperature and renewed at predetermined time intervals.

The following test conditions are fixed:

 the type of leachant;

 the temperature;


-2)
L/A ratio (ml·cm ;

 the total duration of the test;

 the number of eluates to be collected at fixed time intervals.

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The eluate is collected in a fixed number of separate fractions. The eluate collection scheme is designed such
that release mechanisms can be deduced from the analytical results.

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
2
per litre of eluate, and mg of constituents released cumulatively per m of geometric surface area of the waste
material exposed to leaching.

The test conditions (L/A ratio, leachant renewal scheme) have been designed such, that the identification of
leaching mechanisms and their relative importance is enabled. 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(HNO3) = 0,1 mol/l.

6 Equipment
6.1 General

Check the materials and equipment specified in 6.2.1 to 6.2.11 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 and 6.2.11.

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 CO2 from the air in case of leaching from alkaline
materials.

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The minimum distance between the test portion and the walls of the vessel or tank shall be 2 cm, all around
the test portion. Examples are given in Annex B.

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.

NOTE 3 Test specimen can also be placed in the tank e.g. by attaching it to the lid.

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).

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.

NOTE 2 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 laboratory sample consists of one or more specimens or test pieces.

NOTE 3 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

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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.
2
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

The dynamic leaching test for monolithic waste shall be carried out at room temperature (20 °C ± 5 °C).

An example of installation is illustrated in Annex C.

NOTE A constant temperature in the test can be achieved by either controlling the temperature of the lab, or by
controlling the temperature of the leachant and insulating the leaching vessel (6.2.1). This property is a subject for
ruggedness validation.

8.2 Step 1 of the leaching procedure

Calculate the leachant volume V1:

V1 = (8 ± 0,1) × A (1)

where

V1 is the volume of the leachant, in ml;

2
A is the surface area of the test portion, in cm .

Place the test portion in the leaching vessel (6.2.1) using the support (6.2.1), in order to prevent the test
portion from touching the inner side of the leaching vessel. If the test portion consists of more than one
specimen or test piece, the support shall be used in such a way that there is at least 2 cm space between the
specimens or test pieces.

Fill the vessel with the calculated volume of leachant (V1) (5.1), such that the top of the test portion is at least
2 cm submerged. Close the leaching vessel. Note the time t0.

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NOTE For specific scenarios in practice, it can be useful to apply another leachant (for instance ground water, sea
water, CO2 saturated water, etc.), a different temperature and/or another L/A ratio. This would constitute a deviation from
the document, and has to be reported.

Allow the leaching process of this first step until 2 h ± 0,1 h after the addition of the leachant.

At the end of the first step remove the eluate from the leaching vessel, without removing small parts of waste
material that may have fallen off the test portion. Note the time t1. Immediately continue with step 2 (8.3).

Filter the eluate fraction off-line over a 0,45 µm membrane filter (6.2.10). Immediately measure pH and
conductivity, and further prepare the eluate for analysis (see 8.5).

8.3 Steps 2 – 8 of the leaching procedure

Fill the leaching vessel again with the calculated volume of leachant (V1), such that the top of the test portion
is at least 2 cm submerged, and that the distance between the test portion and the wall of the vessel is at least
2 cm. Close the leaching vessel.

Allow the leaching process of each step until the time mentioned in Table 1.

NOTE The liquid renewal frequency is designed and carried out such that the concentration in solution does not
affect the release rate from the specimen significantly.

At the end of each step remove the eluate from the leaching vessel, without removing small parts of waste
material that may have fallen off the test portion. Note the time ti for i being the number of the subsequent
steps. Immediately continue with the next step, following the procedure described above.

Filter the eluate fraction off-line over a 0,45 µm membrane filter (6.2.10). Immediately measure pH and
conductivity, and further prepare the eluate for analysis (see 8.5).

Table 1 — Time intervals for eluates collection

Step/fraction Duration of the time Duration from the

interval start of the test (t0)
daysa days
1 0,08 ± 5 % 0,08 ± 5 %
2 0,92 ± 5 % 1±5%
3 1,25 ± 5 % 2,25 ± 5 %
4 5,75 ± 5 % 8±5%
5 6±5% 14 ± 5 %
6 1±5% 15 ± 5 %
7 13 ± 5 % 28 ± 5 %
8 8 days ± 1 day 36 days ± 0,25 day
a
The time intervals in this table allow to start the test three days per
week: Monday, Tuesday, Wednesday. When the test is started on one of
these days, the collection of the eluates fall in regular workdays.

NOTE 1 The short duration of step 6 is intended to check whether solubility controlled release occurs for certain
constituents. This is further explained in Annex A. One can also check this, using the results of one of the leaching tests,
aiming at equilibrium (e.g. the pH dependence test, CEN/TS 14429).

NOTE 2 If required (for instance to compare with results of tests performed earlier) the test can be extended to 64 days
th
± 0,25 day, by adding a 9 step.

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NOTE 3 The length of the time steps has been modified to give a better understanding of the actual mechanisms
controlling release. If the concentration-time graph of test results shows constant concentrations in all fractions, in spite of
this different length, solubility controls prevails, unless reported measurements are detection limits. In case of mainly
solubility control evaluation as diffusion is not possible. In case of diffusion controlled release the concentrations of the
fractions should be significantly different in each step. Plotting as cumulative release should then show the normal slope of
0,5.

8.4 Weight loss of the monolithic waste during the test

If the specimen(s) fall(s) apart during the test, stop the test and record the failure to withstand the contact with
water for prolonged time.

If it is required to check the weight loss of the specimen (for instance in order to assess the monolithic
character of the waste), after step 8 of the leaching procedure, remove the test portion from the leaching
vessel. Gather all solid parts and particles that have fallen off the test portion during the whole duration of the
test. Dry these solid parts and particles at 40 °C ± 2 °C according to EN 14346 and weigh the dried mat erial
(md).

NOTE 1 For glassy or vitrified monolithic waste, a higher temperature such as 105 °C ± 2 °C can be applied to shorten
the drying duration.

Calculate the mass loss Ml:

md
Ml = (2)
A

where
-2
Ml is the mass loss during the test, in g⋅m ;

md is the weight of dried particles that have fallen off the test portion, in g;
2
A is the geometric surface area of the test portion, in m .

NOTE 2 If Ml exceeds a certain value (to be specified in regulation or otherwise), the monolithic waste does not have
enough integrity to determine the leaching behaviour of the material in monolithic form, in accordance with the procedure,
described in this document.

8.5 Further preparation of the eluates for analysis

Measure the pH (6.2.8) and the conductivity (6.2.7) in accordance with EN 16192 (and optionally redox
potential Eh in mV) of each eluate fraction, just after collection. If the conductivity of an eluate fraction exceeds
7 500 mS/m, measure the volume (or density) of the eluate and dilute the eluate until the conductivity is below
7 500 mS/m. Ensure that the dilution factor is no more than 10.

Divide the eluates into an appropriate number of sub-samples for different chemical analysis, after shaking
well. Preserve the eluate sub-samples depending on the elements to be analyzed, according to
EN ISO 5667-3. Store the (sub) eluates in sealed bottles, according to EN ISO 5667-3.

Determine the concentrations of constituents of interest using the methods of eluate analysis (e.g. EN 16192).
Also measure the total concentration of dissolved organic carbon (DOC) using EN 16192.

NOTE DOC (dissolved organic carbon) can be of relevance when material containing organic matter is stabilized.
DOC is mobilized at high pH and is capable of mobilizing metals and organic contaminants well beyond its solubility
limitation under the common alkaline conditions.

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8.6 Blank test

A blank test shall be carried out on a regular basis, in order to detect, as far as possible, contamination from
equipment and reagents. Fill the leaching vessel (6.2.1) completely with leachant (5.1), and leave the leachant
in the vessel for (24 ± 1) h. Then submit it to the subsequent filtration, storage, preservation and analysis
steps as described in the procedure for the regular eluates. Fill the leaching vessel again with leachant (5.1)
and leave the leachant in the vessel for another (24 ± 1) h. Also submit this second blank eluate to the regular
filtration, and measure the conductivity.

Ensure that the eluates of this blank test fulfil the following minimum requirements:

 in the first eluate of the blank test the concentration of each considered element shall be less than 10 %
of the average concentration in the first three eluate fractions of the leaching procedure, or below the
detection limit;

 the conductivity of the second blank eluate shall be < 0,2 mS/m.

If these requirements are not fulfilled, take the necessary steps to reduce the contamination.

9 Calculations

9.1 Expression of results

9.1.1 General

The results of the leaching test shall be expressed as the cumulative amount of the constituents released,
-
relative to the geometric surface area of the test portion (unit mg⋅m ²), see 9.1.2. It is also possible to express
-1
the results as the concentration of the constituents released (unit mg⋅l ) in each step and/or, if done, at each
instantaneous sampling (see 9.1.3).

9.1.2 Expression of results in terms of area related release

The final results of the leaching tests are expressed as the cumulative amount of the constituents released,
-2
relative to the geometric surface area of the test portion (unit mg⋅m ).

Calculate the measured release of each constituent per step:

10 × c i × V1
ri = (3)
A

where
-2
ri is the measured release of a constituent in step i, in mg⋅m ;
-1
ci is the measured concentration of that constituent in the eluate of step i, in mg⋅l ;

V1 is the volume of the leachant, in ml;

2
A is the geometric surface area of the test portion, in cm .

For analysis results below the limit of quantification for the components concerned both the lower limit and the
upper limit of the release shall be calculated. For the lower limit calculate with ci = 0, and for the upper limit
calculate with ci = the limit of quantification.

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 CEN/TS 15863:2012 (E)

For every constituent, calculate the quantity that has been released cumulatively, up to a certain step of the
leaching procedure:

n
Rn = ∑ ri for n = 1 up to 8 (4)
i =1

where

Rn is the cumulative release of a constituent over a period of time, running from step 1 until step n
-2
(inclusive), in mg⋅m ;
-2
ri is the measured release of a constituent in step i, in mg⋅m .

In the case upper and lower limit values were calculated for the release of a certain constituent, also for the
cumulative release upper and lower limits shall be calculated. The lower limit value is obtained by
accumulating lower limit values for ri where relevant, and the upper limit value is obtained by accumulating
upper limit values for ri where relevant.

Plot the calculated cumulative release of the different constituents as a function of time, corresponding with
the end of the different steps. This graphical representation shall be documented on a double logarithmic
scale.

NOTE For the identification of release controlling factors, and of leaching mechanisms, see Annex A.

9.1.3 Expression of results in concentrations

The analysis of the eluates produced by the leaching test provides the value of the concentration of the
-1
constituents in the eluates of the individual time steps expressed in mg⋅l .

Plot the measured concentrations of the constituents released, the pH and the conductivity, as a function of
time.
-1
NOTE 1 If results are expressed in mg⋅l the results are only valid for the specimen size and shape tested and cannot
be compared to results for specimens with other size and shape.

NOTE 2 When information on equilibrium based tests (e.g. pH dependence leaching test data) is available for the
same material, this information can be used to identify if solubility limitations play a role (see Annex A).

10 Documentation and test report

10.1 General

In order to comply with the present document, the following information shall be documented in such a way
that they are immediately available on request. In the following list, at least, the items marked with an asterisk
(*) shall be included in the test report. All the deviation from the minimum requirements of this document shall
also be documented in the test report.

10.2 General data

 reference to this document*;

 date of receipt of the laboratory sample*;

 sampling report, according to 7.1;

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CEN/TS 15863:2012 (E)

 identification of the laboratory sample*;

 way in which the test portion is obtained from the laboratory sample (e.g. selection of specimens / test
pieces, moulding specimens in the laboratory, cutting/sawing/coring), and justification of this way of
preparation of the test portion*;

 curing time and conditions of the laboratory sample (if carried out by the laboratory)*;

 storage conditions of the laboratory sample and test portion*;

 mass and dimensions of the test portion, and calculation method of the geometric surface area (A) of the
test portion, as well as the geometric surface area itself.

10.3 Leaching test conditions

 date of the test (beginning and end)*;

 identification of the test equipment and instruments used, including the dimensions of the leaching
vessel*;

 volume V1 of the leachant, added to the test portion each step*;

 leachant renewal times of all steps;

 temperature range during the performance of the test;

 mass loss (Ml) during the test;

 any deviation from the test method and the reason of this deviation together with all circumstances that
may have influenced the results*.

10.4 Analytical report

 pH and conductivity of the eluate fractions collected (optional: redox potential)*;

 any dilutions that were carried out*;

 methods of preservation of the eluate fractions for the different elements to be analysed, in accordance
with 8.5*;

 quantities of preservation fluid added in accordance with 8.5 where this is more than 1 ml per 100 ml
eluate;

 all measured concentrations.

10.5 Results of the leaching test


-1
the measured concentrations per step for each constituent, in mg⋅l , presented in a table of results and
graphically presented plotted against time*;


-2
the released quantities ri calculated per step for each constituent, in mg⋅m geometric surface area of the
monolithic waste; for analysis results below the limit of quantification for the components concerned both
the lower limit and the upper limit of the released quantity shall be indicated;

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 CEN/TS 15863:2012 (E)


-2
the cumulatively released quantities Ri calculated per step for each constituent, in mg⋅m geometric
surface area of the monolithic waste, plotted against time (on a double logarithmic scale). Again, if
relevant, lower and upper limits shall be indicated*.

11 Test performance
The test specified in this Technical Specification is not validated and no data are available on robustness,
repeatability and reproducibility.

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CEN/TS 15863:2012 (E)

Annex A
(informative)

Identification of release mechanisms and use of test results

A.1 Introduction
The main reason for developing the dynamic monolith leach test is that the release from monolithic specimen
is surface area related and not, like in granular material, dictated largely by percolation and equilibrium
between solid and leachant. This implies that the test is carried out on a specimen with a quantifiable surface
area and of sufficient size to minimise depletion effects during the test.

Examples of factors controlling release are discussed in more detail in A.2. More detailed data can be found in
various scientific publications which are cited in the bibliography of this document or in the state of the art [4].

The field of application is rather wide and not limited to stabilised waste as the same release phenomena are
relevant for monolithic materials as construction products (as discussed in CEN/TC 51, CEN/TC 104,
CEN/TC 125, CEN/TC 229 etc.) and radioactive waste forms [8].

A.2 Examples of factors influencing the leaching of monolithic waste

There are several factors influencing dynamic release from monolithic specimen, which obviously are not
equally relevant for any one given specimen. Below the different factors are discussed briefly:

Two types of factors can be distinguished. On the one hand, those which cannot be influenced by laboratory
people performing this document. Those factors are linked to the material itself (e.g. intrinsic characteristics),
including the possible curing stage.

Nature of the material – the nature of the material is already in part addressed in view of tortuosity, porosity,
dimensions, pH, etc. The nature of a product will be of relevance for the substances that are likely to be of
relevance. Cement-based materials, sintered bricks, light weight concrete, bituminous materials each have
their specific characteristics and most relevant substances.

Porosity – the porosity of a specimen is of relevance as together with tortuosity, it controls the rate of
transport by diffusion within the matrix. This relates to connected porosity, as closed porosity (as in light
weight concrete) does not contribute to release from the specimen.

Tortuosity – the tortuosity is the extended path length for diffusion due to the non-linear nature of pores. This
parameter is a property, that is unique for any one specimen as it depends on curing time, water to cement
ratio (relevant for products based on hydraulic or pozzolanic properties), production conditions, degree of
compaction, constituents, sintering temperature, etc.

pH – the pH of a monolithic specimen is important as solubility is strongly controlled by pH. In particular,

cement based materials undergo carbonation with time depending on the scenario of use. In general, a pH
front will develop, where in the modified zone leaching will be different from the leaching of the bulk matrix. In
case of materials with a neutral pH (e.g. bitumen, sintered products) the release in a neutral pH environment
is not as sensitive to pH. On the other hand materials with a very low ANC are sensitive to field imposed pH
conditions (e.g. from acid rain or acidic groundwater).

Redox – in case of stabilised waste with reducing properties (e.g. sulphide addition), a redox front may
develop, when the product is exposed to the atmosphere. This strongly affects the release behaviour of
specific constituents (R.E.C.O.R.D. study on reduced metallurgical slag) [10].

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 CEN/TS 15863:2012 (E)

Availability – the availability of constituents is a fraction of the total content that is relevant for modelling
release and can be seen as relevant to assess the maximum released amount that might occur under the
most extreme field exposed conditions. This quantity can be derived from the pH dependence leaching test
(CEN/TS 14429 or CEN/TS 14997).

On the other hand, factors which can be changed and/or need to be controlled by laboratory people
performing this document. Those factors are linked to the test itself (excluding the possible curing stage).

Shape – specimen can be tested in different shapes, e.g. block, cube, cylinder, block with open spaces.
Important for expressing the results and interpreting release is the need to be able to quantify the surface area
as results are expressed per unit surface area. Monolithic materials with irregular surfaces are therefore more
difficult to handle. In that case the geometric surface area can be estimated, or a specimen sampled from an
irregular form by cutting or coring can be used as test portion.

Dimensions – the dimension of specimen to be tested is important from the viewpoint of depletion. I.e. in
case of small dimensions mobile species can become depleted. This depletion is a function of the porosity,
tortuosity and the interaction of the constituent of interest with the solid matrix in a given period of time. For
concrete in general 4 cm cubes will be adequate, for stabilised waste specimen larger specimen (10 cm
diameter) are generally provide better representative results.

Temperature – the temperature plays a role as diffusion is a temperature controlled parameter. The Arrhenius
equation applies, which in the case of testing at 10 °C and 25 °C amounts to about a factor of 2 diffe rence in
release. The temperature has also a strong effect on the solubility of some key substances. For translating
effects from lab to field this factor can not be ignored.

Degree of water contact – the degree of water contact is crucial for assessing impact. In dry periods, there is
no transfer of substance. Depending on the degree of water saturation in the product gradient relaxation can
occur from the core to the surface of the material. From some studies it has been shown that summing the wet
periods provides an acceptable estimate of the actual release in case of wet-dry periods. In other cases when
relaxation effect occurs, the portion of the material close to the surface is re-concentrated during each dry
period and this leads to a significative increase in release versus liquid to solid ratio. Full mechanistic
modelling is, however, the preferred prediction approach.

Leachant – the leachant used in the test is water. For standardisation purposes and to ensure comparability
of data, this choice was made. When assessment of a given aquatic environment is aimed at (salted,
containing DOC, acidic, etc.), the composition of the leachant can be adapted in the procedure.

Solubility, diffusion, wash off – Different release mechanisms lead to different release patterns in the
dynamic leaching test:

 solubility;

 diffusion from the interior of the matrix to the surface;

 surface wash-off is a process where as a results of the process, substances may be concentrated on
the surface and be released at the first contact with water.

In addition, the porosity may be extremely low in molten products, like slag or vitrified material. In case of
highly soluble constituents, depletion of substance may occur. Within the matrix as well as at the surface of
the specimen in contact with a solution solubility limitations and changes in solubility may occur. In Figure A.1,
typical patterns are shown as examples.

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CEN/TS 15863:2012 (E)

E. 1 Di f f us i on- c ont r ol l e d r e l e a s e E. 2 De pl e t i on m obi l e c ons t i t ue nt

20000 2000000

B
10000 A 1000000
R el ease (mg/2m
)

1000
100000

300 40000
0. 1 1 10 100 0. 1 1 10 100
E. 4 Sur f a c e wa s h- of f E. 5 Cha nge i n c ont r ol l i ng c ondi t i ons

100 20000
C D
10000

10

1000

1 300
0. 1 1 10 100 0. 1 1 10 100
E. 3 De l a ye d r e l e a s e E. 6 Cha nge i n r e dox c ondi t i ons

50000 3000

E 1000 F
10000

100

1000

10

100
50 1
0. 1 1 10 100 0. 1 1 10 100

T i me (d ay s)

Key
-2
●●●● = main release behaviour, which represent release per time interval, in mg⋅m ;

-2
++++ = cumulative release, expressed in mg⋅m ;

--------- = line with slope of 0,5, representing release by diffusion (in case, or in phases of, release by diffusion the
release per time interval (black dots) is parallel to the dotted line).

E1 leaching is dominated by diffusion;

E2 leaching, after short period of full diffusion ending with depletion;
E3 release by diffusion, but in the first steps far dominated by wash-off;
E4 release starts with fast release of mobile species of a substance, followed by release (by diffusion) of less-mobile
species of that substance;
E5 release (by diffusion) starts delayed;
E6 change in release with time due to major changes in matrix chemistry.

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 CEN/TS 15863:2012 (E)

NOTE Explanation:

 graphs are in a double logarithmic presentation (both X- and Y-axe);

 in double logarithmic graphs diffusion is theoretically represented by a line with a slope 0,5;

 the cumulative graph shows the total release from the start; it is possible, but less easy to derive relevant mechanism
from this curve;

 in case of full solubility control, the concentration in all time intervals is the same. If a time schedule with a square
root of time relation is applied this may lead wrongly to a conclusion of diffusion control. The time intervals have been
adjusted to prevent this problem.

Figure A.1 — Overview of characteristic release curves for monolithic specimen, each figure showing
a specific release mechanism

A.2 Solubility control versus diffusion controlled release - Three options can be identified here for
checking if solubility control is likely to control release of substances from a monolithic specimen:

 The best option is by comparing the measured concentrations in the dynamic leaching test eluates with
the results from the pH dependence test (CEN/TS 14429 or CEN/TS 14497) at the corresponding pH. When
dynamic leaching test data match with the pH dependence test ones, solubility control as depicted by the pH
dependence test is very likely controlling release.Other possibilities are:

 By modifying of the leachant renewal cycles to ensure maximum difference in concentration between
renewal intervals, it is possible to distinguish diffusion or largely diffusion controlled release from
solubility controlled release or detection limit issues, which can falsely lead to the conclusion of an
apparent diffusion controlled release.

 By comparing concentration data as obtained from the first fractions of a percolation test on size
reduced monolithic material with data from the pH dependence test. A low L/S condition in the field is
likely to lead to solubility controlled conditions. In case data from the percolation test on crushed
monolithic material and pH dependence test data match, then that is an indication of solubility control
over a wide range of pH and L/S conditions and thus will be a controlling factor in release from
monolithic waste as well.

A.3 Long term release prediction

A proper understanding of the mechanisms of release for the constituents of interest is of importance to be
able to make predictions on long term release from monolithic waste. Based on this understanding simplified
and more sophisticated model predictions can be made.

These calculations are to be made in the framework of the methodology described / standardised in
EN 12920. Especially, the results of the dynamic leaching test cannot be used alone for the prediction /
assessment of the long term release. In order to conduct properly these calculations, this mostly requires the
use of results of other tests as the ones developed within CEN/TC 292, such as CEN/TS 14405,
CEN/TS 14429.

Since the publication of EN 12920, numerous studies have been conducted in the aim of long term release
prediction. An abundant bibliography is included in the state of the art [4] which can be completed with more
recent publications cited in the bibliography part of this document.

A pitfall can be the use of results from this test to predict behaviour in a specific application without properly
-2
taking the mechanism of release into account. When results are expressed in mg⋅m at a given exposure
time, the direct multiplication with time is incorrect as a square root of time relationship underlies these data.
-1 -2
Data expressed in mg⋅kg can not be transposed to release (only after recalculation to mg⋅m units).

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CEN/TS 15863:2012 (E)

A simplified approach assumes diffusion controlled release corrected for temperature and degree of water
contact. A further refinement of this approach involves a mass balance evaluation to correct for already
leached material (decrease of available quantity). For non-interacting species (e.g. chlorides), this approach
will provide quite reasonable estimates of release however not for other species of interest (e.g. Si, Ca, heavy
metals).

In recently more sophisticated model predictions have been published that take physical form and full
chemistry into account [5, 6].

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 CEN/TS 15863:2012 (E)

Annex B
(informative)

Examples of data about the L/A ratio

In the table below for some specimen types (cube, rectangular and cylinder) and the most common
dimensions, minimum and maximum vessel diameters are calculated, in the case cylindrical vessels are used.
The minimum diameter is calculated in order to fulfil the criterion, mentioned in 6.2.1, stating that the minimum
distance between the test portion and the walls shall be 2 cm. The maximum diameter is calculated in order to
fulfil the criterion, mentioned in 8.2, stating that the top of the test portion shall be at least 2 cm submerged.

Table B.1 — Vessel dimensions in relation with specimen of different sizes and/or shapes (based on
L/A = 8)

Specimen

Type Height Diameter Length Width Volume Surface Vtotala Distance Distance Diameter
between between cylindrical
vessel specimen vessel c
and and
specimen water
b
level b
V A min. to
max.

cm cm cm cm ml cm2 ml cm cm cm

cube 10 - 10 10 1 000 600 5 800 2,0 10,4 18 to 23

4,4 2,0

cube 4 - 4 4 64 96 832 2,0 5,4 9,7 to 11,5

2,9 2,0

cylinder 10 10 - - 785 471 4 553 2,0 17,6 14 to 20

5,2 2,0

rectangular 5 - 20 10 1 000 700 6 600 2,0 5,1 26 to 30

4,1 2,0

rectangular 16 - 4 4 256 288 2 560 2,0 17,0 9,7 to 12,8

3,6 2,0

a
Vtotal is the sum of the volume of the specimen and leachant volume as calculated according to Equation 1.
b
The distance of 2,0 cm is fixed, the non-fixed distance is calculated based on size and/or shape of the specimen type.
c
The minimum diameter is calculated in order to fulfil the criterion, mentioned in 6.2.1, stating that the minimum distance between the test
portion and the walls shall be 2 cm. The maximum diameter is calculated in order to fulfil the criterion, mentioned in 8.2, stating that the top
of the test portion shall be at least 2 cm submerged.

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CEN/TS 15863:2012 (E)

If the most adapted calculated size (e.g. height) of the vessel cannot be bought easily, or if several test
portions with slightly different sizes have to be tested, it is recommended to acquire a slightly bigger vessel.
The volume is then corrected by adding inert material (e.g. glass balls) to comply with the L/A ratio of
-2
8 ml⋅cm . The minimum distance between test portion and inert material still need to be equal or greater than
2 cm.

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 CEN/TS 15863:2012 (E)

Annex C
(informative)

Process map for CEN/TS 15863

25
CEN/TS 15863:2012 (E)

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 CEN/TS 15863:2012 (E)

Bibliography

EN 12457-1, 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)

CEN/TS 14405, Characterization of waste — Leaching behaviour test — Up-flow percolation test (under
specified conditions)

CEN/TS 14429, Characterization of waste — Leaching behaviour tests — Influence of pH on leaching with
initial acid/base addition

EN 14899, Characterization of waste — Sampling of waste materials — Framework for preparation of a

sampling plan

CEN/TS 14997, Characterization of waste — Leaching behaviour test — Influence of pH on leaching with
continuous pH-control

CEN/TS 15862, Characterization of waste — Compliance leaching test — One stage batch leaching test for
monoliths at fixed liquid to surface area ration (L/A) for test portions with fixed minimum dimensions

CEN/TS 15864, Characterization of waste — Leaching behaviour test for basic characterization — Dynamic
monolithic leaching test with continuous leachant renewal under conditions relevant for specified scenario(s)

NEN 7345:1995, Leaching characteristics of solid earthy and stony building and waste materials — Leaching
tests — Determination of the leaching of inorganic components from building and monolithic waste materials
with the diffusion test

ÖNORM S 2116-4:2001, Examinations of solidified wastes — Elution tests during 24 hours, 64 days, 2 days

[1] De Windt L., Badreddine R. Modelling of long term dynamic leaching test applied to solidified/stabilised
waste. Waste Management, 2007, 27 (11) 1638-1647

[2] Méhu J, Brons-Laot G, Girod M and Schiopu N. Application of ENV 12920 – French experience. In
Problems around soil and waste I – Horizontal aspects of leaching. Workshop proceeding. DG JRC
Workshop, Ispra, 14-15 february 2005. EUR 21659 EN. 2005

[3] Méhu J and Van der Sloot H.A. Étude du couple “matrice-déchets”/“Réactifs solidifiants” vis-à-vis de la
lixiviation. Aspects théoriques et expérimentaux. RECORD association. Study n°91-0305/1A. Final report
1992

[4] State of the art review from a standardization point of view on dynamic leaching test for monolithic waste
materials, 2001, CEN/TC 292 document N548.

[5] Piantone P, Guyonnet D, Chateau L. Workshop source term from characterization to prediction. Final
report BRGM-RP-55500-FR, 2007

[6] Van der Sloot H.A., Van Zomeren A., Meeussen J.C.L., Seignette P.F.A.B. and Bleyerveld R., Test
method selection, validation against field data, and predictive modelling for impact evaluation of stabilised
waste disposal. Journal of Hazardous Materials 141, 2007, pp 354-369.

[7] Nomenclature for sampling in analytical chemistry (recommendations 1990) - W. Horwitz IUPAC 1990 -
Pure and Appl. Chem. Vol. 62, No6, pp 1193-1208.

[8] American Nuclear Society (ANS) ANSI/ANS 16.1 (1986). Measurement of the leachability of solidified low-
level radioactive wastes by a short term procedure.

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[9] Tiruta-Barna L., Rethy Z. and Barna R., Release dynamic process identification for a cement based
material in various leaching conditions. Part II. Modelling the release dynamics for different leaching
conditions. Journal of Environmental Management. 74, 2, 2005, pp 127-139.

[10] POLDEN INSAVALOR, ECN (1992). Study of couples waste matrix / solidication reagents in relation to
leaching. Theoretical and experimental aspects. Association RECORD, Contract no. 91-0305/1A (in
French).

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