SIST-TS CEN/TS 15863:2013
(Main)Characterisation of waste - Leaching behaviour test for basic characterisation - Dynamic Monolithic Leaching Test with periodic leachant renewal, under fixed test conditions
Characterisation of waste - Leaching behaviour test for basic characterisation - Dynamic Monolithic Leaching Test with periodic leachant renewal, under fixed test conditions
This Technical Specification 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. NOTE 2 For monolithic waste materials with a saturated hydraulic conductivity higher than 10-8 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.
Charakterisierung von Abfällen - Untersuchung des Auslaugungsverhaltens für die grundlegende Charakterisierung - Dynamisches Auslaugungsverfahren für monolithische Abfälle mit periodischer Erneuerung des Auslaugungsmittels unter festgelegten Prüfbedingungen
Diese Technische Spezifikation ist für die Bestimmung des Auslaugungsverhaltens von monolithischen Abfällen unter dynamischen Bedingungen anwendbar. Diese Untersuchung wird unter den festgelegten experimentellen Bedingungen diesem Dokument durchgeführt. Diese Untersuchung ist auf die Bestimmung der Freisetzung von anorganischen Bestandteilen aus monolithischem Abfall in Bezug auf die Zeit gerichtet, zu der er in Kontakt mit der wässrigen Lösung (Auslaugungsmittel) kommt.
Dieses dynamische Auslaugungsverfahren für monolithische Abfälle (DMLT, en: Dynamic Monolithic Leaching Test) ist ein Parameter einer in EN 12920 festgelegten besonderen Untersuchung und gilt deshalb nicht für die Simulation tatsächlicher Situationen. Die Anwendung dieses Untersuchungsverfahrens ist allein nicht aus¬reichend für die Bestimmung des ausführlichen Auslaugungsverhaltens von monolithischen Abfällen unter festgelegten Bedingungen.
Im Rahmen der EN 12920 und in Kombination mit zusätzlichen chemischen Angaben werden die Unter-suchungsergebnisse zur Identifizierung der Auslaugungsmechanismen und ihres Stellenwertes angewendet. Die eigentlichen Eigenschaften können zur Vorhersage der Freisetzung der Bestandteile in einem festgelegten Zeitrahmen angewendet werden, um das Auslaugungsverhalten von monolithischen Abfallstoffen zu bewerten, die unterschiedlichen Situationen oder Szenarien (einschließlich Szenarien der Deponierung und der Wiederverwertung) ausgesetzt wurden.
Das Untersuchungsverfahren ist bei regelmäßig geformten Prüfmengen von monolithischen Abfällen mit Mindestmaßen von 40 mm in alle Richtungen anwendbar, bei denen vorausgesetzt wird, dass sie ihre Unver-sehrtheit über einen für die Beobachtung des Szenarios relevanten Zeitrahmen behalten. Das Untersuchungsverfahren ist für Prüfmengen geeignet, bei denen die geometrische Oberfläche mit einfachen geometrischen Gleichungen bestimmt werden kann. Das Untersuchungsverfahren ist für weniger durchlässige monolithische Stoffe geeignet.
ANMERKUNG 1 Wenn die Prüfmenge durch Schneiden oder Bohren vorbereitet wurde, um die Anforderung nach einer regelmäßigen Form zu erfüllen, dann werden neue Oberflächen freigelegt, was zu einer Änderung/zu Änderungen der Auslaugungseigenschaften führen könnte. Andererseits, wenn die Prüfmenge durch Formpressen vorbereitet wird, wird die Oberfläche von der Art des Pressens und den Lagerungsbedingungen abhängen. Bei beabsichtigter Bewertung des Verhaltens des Stoffkerns muss der Prüfkörper ohne jeden Kontakt mit Luft aufbewahrt werden, um eine Karbonisierung zu vermeiden.
ANMERKUNG 2 Bei monolithischen Abfallstoffen mit einer gesättigten hydraulischen Leitfähigkeit von mehr als 108 m/s wird Wasser wahrscheinlich durch den Monolithen durchsickern anstatt um ihn herum zu fließen. In solchen Fällen kann es in Bezug auf die Freisetzung von der geometrischen Oberfläche zu Fehlinterpretationen führen. Eine Perkolations¬prüfung ist dann besser geeignet (z. B. CEN/TS 14405).
Dieses Verfahren darf nicht bei Stoffen angewendet werden, die mit dem Auslaugungsmittel reagieren, was z. B. zu einer übermäßigen Gasemission oder einer unverhältnismäßigen Wärmefreisetzung führt.
Dieses Dokument wurde entwickelt, um vor allem die Freisetzung anorganischer Bestandteile aus Abfällen zu bestimmen. Es berücksichtigt nicht die besonderen Eigenschaften der organischen Bestandteile und auch nicht die Folgen der mikrobiologischen Prozesse in den organisch abbaubaren Abfällen.
Caractérisation des déchets - Essais de comportement à la lixiviation pour la caractérisation de base - Essai de lixiviation dynamique des monolithes avec renouvellement périodique du lixiviant, dans des conditions d'essai fixes
La présente Spécification technique s'applique à la détermination du comportement à la lixiviation des déchets
monolithiques dans des conditions dynamiques. L'essai est réalisé dans des conditions expérimentales fixées dans le
présent document. L’essai a pour objectif de déterminer le relargage en fonction du temps des constituants
inorganiques de déchets monolithiques lorsqu'ils entrent en contact avec une solution aqueuse (lixiviant).
Le présent essai de lixiviation dynamique des monolithes (DMLT) est un essai paramétrique tel que spécifié dans
l'EN 12920, il n'a donc pas pour objectif de simuler des situations réelles. L'application de la présente méthode d'essai
seule ne suffit pas à déterminer le comportement détaillé à la lixiviation d'un déchet monolithique dans des conditions
spécifiées.
Dans le cadre de l'EN 12920 et en association avec des informations chimiques supplémentaires, les résultats d'essai
sont utilisés pour identifier les mécanismes de lixiviation et leur importance relative. Ces propriétés intrinsèques
peuvent être utilisées pour prévoir le relargage des constituants sur une période donnée, afin d'évaluer le
comportement à la lixiviation des déchets monolithiques dans différentes situations ou scénarios (y compris les
scénarios d'élimination et de recyclage).
Karakterizacija odpadkov - Izluževalni preskus za osnovno karakterizacijo - Dinamični izluževalni preskus pri določenih pogojih za izluževanje monolitnih odpadkov z občasnim obnavljanjem izluževalnega medija
Ta tehnična specifikacija se uporablja za določanje izluževanja monolitnih odpadkov pri dinamičnih pogojih. Ta preskus se izvaja pod preskusnimi pogoji, določenimi v tem dokumentu. S tem preskusom se ugotavlja izpust kot funkcija časa neorganskih sestavin iz monolitnih odpadkov, ko pridejo v stik z vodno raztopino (izluževalnim medijem). Ta dinamični izluževalni preskus za monolitne odpadke (DMLT) je preskus z določenimi parametri, ki so navedeni v standardu EN 12920, zato ne simulira dejanskih pogojev. Uporaba samo te preskusne metode ne zadostuje za določanje podrobnega izluževanja monolitnih odpadkov pod določenimi pogoji. V okviru standarda EN 12920 in v kombinaciji z dodatnimi kemijskimi podatki se rezultati preskusa uporabljajo za identifikacijo izluževalnih mehanizmov in njihove relativne pomembnosti. Bistvene lastnosti se lahko uporabijo za napoved izpusta sestavin v danem časovnem okviru, da se oceni izluževanje monolitnih odpadnih materialov v različnih okoliščinah ali načrtih (vključno z recikliranjem in odstranitvijo). Ta preskusna metoda se uporablja za preskusne vzorce monolitnih odpadkov pravilne oblike z najmanjšimi merami 40 mm v vse smeri, za katere se predvideva, da v časovnem okviru, ustreznem za zadevni načrt, ohranijo svojo neoporečnost. Ta preskusna metoda se uporablja za preskusne vzorce, pri katerih se lahko geometrijska površina določi s preprostimi geometrijskimi enačbami. Ta preskusna metoda se uporablja za slabo prepustne monolitne materiale. OPOMBA 1 Če se preskusni vzorec zaradi izpolnjevanja zahteve po pravilni obliki pripravi z rezanjem ali vrtanjem, se izpostavijo nove površine, pri čemer se lahko lastnosti izluževanja spremenijo. Če se preskusni vzorec pripravi z oblikovanjem, je površina odvisna od vrste kalupa in pogojev shranjevanja. Če je namen merjenja ocena obnašanja jedra snovi, mora biti primerek shranjen tako, da ne pride v stik z zrakom, pri čemer se prepreči karbonatizacija. OPOMBA 2 Pri monolitnih odpadkih z nasičeno hidravlično prevodnostjo, ki je višja od 10-8 m/s, se lahko voda skozi monolit precedi, namesto da se pretaka okoli. V takih primerih lahko zaradi izpusta na geometrijsko površino pride do napačne interpretacije. Takrat je bolj primeren preskus precejanja (npr. CEN/TS 14405). Ta postopek se ne sme uporabljati za materiale, ki reagirajo z izluževalnim medijem, ker lahko nastanejo prekomerni izpusti plina ali prekomerno sproščanje toplote. Ta dokument je bil pripravljen za ugotavljanje izpusta pretežno neorganskih sestavin iz odpadkov. Ne upošteva posebnih značilnosti organskih sestavin in posledic mikrobioloških procesov v organskih razgradljivih odpadkih.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
SIST-TS CEN/TS 15863:2013
01-januar-2013
.DUDNWHUL]DFLMDRGSDGNRY,]OXåHYDOQLSUHVNXV]DRVQRYQRNDUDNWHUL]DFLMR
'LQDPLþQLL]OXåHYDOQLSUHVNXVSULGRORþHQLKSRJRMLK]DL]OXåHYDQMHPRQROLWQLK
RGSDGNRY]REþDVQLPREQDYOMDQMHPL]OXåHYDOQHJDPHGLMD
Characterisation of waste - Leaching behaviour test for basic characterisation - 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
renouvellement périodique du lixiviant, dans des conditions d'essai fixes
Ta slovenski standard je istoveten z: CEN/TS 15863:2012
ICS:
13.030.10 Trdni odpadki Solid wastes
SIST-TS CEN/TS 15863:2013 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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SIST-TS CEN/TS 15863:2013
TECHNICAL SPECIFICATION
CEN/TS 15863
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 periodic
leachant renewal, under fixed test conditions
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
périodique du lixiviant, dans des conditions d'essai fixes für monolithische Abfälle mit periodischer Erneuerung des
Auslaugungsmittels unter festgelegten Prüfbedingungen
This Technical Specification (CEN/TS) was approved by CEN on 27 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 15863:2012: E
worldwide for CEN national Members.
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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 . 14
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 . 15
9.1.2 Expression of results in concentrations . 15
10 Documentation and test report . 16
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.
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.
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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
1
different tests in relation to the objective. The following test hierarchy is taken from the Landfill Directive and
2
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 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 specimens can be approached.
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1 Scope
This Technical Specification 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 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, Characterisation of waste — Methodology for the determination of the leaching behaviour of
waste under specified conditions
EN 14346, Characterisation of waste — Calculation of dry matter by determination of dry residue or water
content
EN 15002, Characterisation of waste — Preparation of test portions from the laboratory sample
EN 16192 Characterisation of waste — Analysis of eluates
EN ISO 3696, Water for analytical laboratory use — Specification and test methods (ISO 3696)
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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)
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
[SOURCE: EN 12457-1:2002, 3.1]
3.2
laboratory sample
sample or sub-sample(s) sent to or received by the laboratory
[SOURCE: IUPAC:1997, 3.2]
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.
3.3
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.
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
[SOURCE: EN 12920:2006, 3.4]
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 1 to entry: L/A is expressed in ml·cm .
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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
(SOURCE: EN 12457-1:2002, 3.7)
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
[SOURCE: EN 12920:2006, 3.8]
3.9
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.
3.10
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
[SOURCE: IUPAC:1997, 3.11]
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
[SOURCE: IUPAC:1997, 3.13]
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;
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L/A ratio (ml·cm ;
the total duration of the test;
the number of eluates to be collected at fixed time intervals.
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(HNO ) = 0,1 mol/l.
3
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.
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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
2
materials.
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 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.
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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.
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
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