EN ISO 21268-3:2019
(Main)Soil quality - Leaching procedures for subsequent chemical and ecotoxicological testing of soil and soil-like materials - Part 3: Up-flow percolation test (ISO 21268-3:2019)
Soil quality - Leaching procedures for subsequent chemical and ecotoxicological testing of soil and soil-like materials - Part 3: Up-flow percolation test (ISO 21268-3:2019)
This document specifies a test, which is aimed at determining the leaching behaviour of inorganic and organic substances from a soil and soil-like materials. The method is a once-through up-flow percolation test under standardized conditions of flow rate. The material is leached under dynamic hydraulic conditions. The document has been developed to measure the release of inorganic and organic substances from soil and soil-like material as well as to produce eluates for subsequent ecotoxicological testing. For ecotoxicological testing, see ISO 15799[6] and ISO 17616[7]. The test results enable the distinction between different release patterns, for instance wash-out and release under the influence of interaction with the matrix, when approaching local equilibrium between material and leachant.
This test method produces eluates, which can subsequently be characterized by physical, chemical and ecotoxicological methods in accordance with existing standard methods. The results of eluate analysis are presented as a function of the liquid/solid (L/S) ratio. The test is not suitable for substances that are volatile under ambient conditions.
NOTE 1 Volatile organic substances include the low-molecular-weight substances in mixtures such as mineral oil.
NOTE 2 It is not always possible to optimize test conditions simultaneously for inorganic and organic substances and optimum test conditions can also vary between different groups of organic substances. Test requirements for organic substances are generally more stringent than those for inorganic substances. The test conditions suitable for measuring the release of organic substances will generally also be applicable to inorganic substances.
NOTE 3 Within the category of organic substances, a significant difference in behaviour exists between the more polar, relatively water-soluble compounds and apolar, hydrophobic organic substances (HOCs). In the latter case, mechanisms of release (e.g. particle-bound or dissolved organic carbon-bound) can be more crucial as well as sorption losses of soluble HOCs on different materials with which they come in contact (e.g. bottles, filters). The test and the results should be used for leaching of organic substances only with thorough consideration of the specific properties of the substances in question and the associated potential problems.
NOTE 4 For ecotoxicological testing, eluates representing the release of both inorganic and organic substances are needed. In this document, ecotoxicological testing is also meant to include genotoxicological testing.
NOTE 5 The test is generally not suitable for soils with hydraulic conductivities below 10−8 m/s (see also Annex B). It can be difficult to maintain the designated flow rate already in the range of saturated hydraulic conductivity between 10−7 m/s and 10−8 m/s.
The application of this test method alone is not sufficient for the determination of the leaching behaviour of a material under specified conditions different to those from the test procedure, since this generally requires the application of several test methods, behavioural modelling and model validation. This document does not address issues related to health and safety. It only determines the leaching properties as outlined in Clause 4.
Bodenbeschaffenheit - Elutionsverfahren für die anschließende chemische und ökotoxikologische Untersuchung von Boden und von Bodenmaterialien - Teil 3: Perkolationstest im Aufwärtsstrom (ISO 21268-3:2019)
Dieses Dokument legt eine Prüfung fest, deren Ziel die Bestimmung des Elutionsverhaltens von anorganischen und organischen Substanzen aus Boden und bodenähnlichen Materialien ist. Bei dem Verfahren handelt es sich um eine Perkolationsprüfung mit einmaligem Durchlaufen im Aufwärtsstrom unter standardisierten Bedingungen der Fließgeschwindigkeit. Das Material wird unter hydraulisch dynamischen Bedingungen ausgelaugt. Dieses Dokument wurde erstellt, um die Freisetzung anorganischer und organischer Bestandteile aus Boden und bodenähnlichem Material zu untersuchen und um Eluate für nachfolgende ökotoxikologische Untersuchungen herzustellen. Hinsichtlich der ökotoxikologischen Untersuchungen siehe ISO 15799 [6] und ISO 17616 [7]. Die Prüfergebnisse ermöglichen die Unterscheidung zwischen verschiedenen Freisetzungs¬mustern, wie z. B. Auswaschung und Freisetzung unter Einfluss einer Wechselwirkung mit der Matrix, wenn das lokale Gleichgewicht zwischen Material und Elutionsmittel annähernd erreicht ist.
Durch das vorliegende Prüfverfahren werden Eluate hergestellt, die anschließend mit physikalischen, chemischen und ökotoxikologischen Verfahren nach bestehenden Standardverfahren charakterisiert werden können. Die Ergebnisse der Eluatanalyse werden als Funktion des Flüssigkeits /Feststoffverhältnisses (L/S) dargestellt. Die Prüfung ist nicht geeignet für Substanzen, die unter Umgebungsbedingungen flüchtig sind.
ANMERKUNG 1 Zu den flüchtigen organischen Substanzen gehören niedermolekulare Substanzen in Mischungen wie z. B. Mineralöl.
ANMERKUNG 2 Es ist nicht immer möglich, die Prüfbedingungen gleichzeitig für anorganische und organische Substanzen zu optimieren, und die optimalen Prüfbedingungen können sich auch für unterschiedliche Gruppen von organischen Substanzen unterscheiden. Die Prüfanforderungen für organische Substanzen sind im Allgemeinen strenger als für anorganische Substanzen. Die Prüfbedingungen, die für die Messung der Freisetzung von organischen Substanzen geeignet sind, sind im Allgemeinen auch auf anorganische Substanzen anwendbar.
ANMERKUNG 3 Innerhalb der Kategorie organischer Substanzen besteht ein deutlicher Verhaltensunterschied zwischen den mehr polaren, relativ wasserlöslichen Verbindungen und den nichtpolaren, hydrophoben organischen Substanzen (en: hydrophobic organic substances, HOCs). Im letzteren Fall können die Freisetzungsmechanismen (z. B. teilchengebundene oder gelöste organische Kohlenstoffverbindungen) sowie die Sorptionsverluste löslicher HOCs bei unterschiedlichen Materialien, mit denen sie in Kontakt kommen (z. B. Flaschen, Filter), von entscheidenderer Bedeutung sein. Die Prüfung und die Ergebnisse sollten nur unter sorgfältiger Berücksichtigung der spezifischen Eigenschaften der zu betrachtenden Substanzen und damit verbundenen möglichen Probleme zur Elution organischer Substanzen angewendet werden.
ANMERKUNG 4 Für ökotoxikologische Untersuchungen sind Eluate erforderlich, die die Freisetzung sowohl von anorganischen als auch von organischen Substanzen widerspiegeln. Im vorliegenden Dokument umfasst die ökotoxikologische Untersuchung auch die genotoxikologische Untersuchung.
Qualité du sol - Modes opératoires de lixiviation en vue d'essais chimiques et écotoxicologiques ultérieurs des sols et matériaux du sol - Partie 3: Essai de percolation à écoulement ascendant (ISO 21268-3:2019)
Le présent document spécifie un essai destiné à déterminer le comportement à la lixiviation de substances inorganiques et organiques issues de sols et de matériaux analogues au sol. La méthode est un essai de percolation à écoulement ascendant mené dans des conditions de débit normalisées. Le matériau est lixivié dans des conditions hydrauliques dynamiques. Le présent document a été conçu pour étudier le relargage de substances organiques et inorganiques à partir du sol et des matériaux analogues au sol et produire des éluats destinés aux essais écotoxicologiques. Pour en savoir plus sur les essais écotoxicologiques, voir l'ISO 15799[6] et l'ISO 17616.[7] Les résultats de l'essai permettent de faire la distinction entre différents types de relargage, tels que le lessivage ou le relargage sous l'effet de l'interaction avec la matrice, à l'approche de l'équilibre local entre le matériau et le lixiviant.
Cette méthode d'essai produit des éluats qui peuvent ensuite être caractérisés par des méthodes physiques, chimiques et écotoxicologiques selon des méthodes normalisées existantes. Les résultats de l'analyse des éluats sont présentés en fonction du rapport liquide/solide (L/S). L'essai n'est pas adapté aux substances qui sont volatiles dans des conditions ambiantes.
NOTE 1 Les substances organiques volatiles comprennent les substances à faible masse moléculaire contenues dans des mélanges tels que les huiles minérales.
NOTE 2 Il n'est pas toujours possible d'optimiser les conditions d'essai à la fois pour les substances organiques et les substances inorganiques. Les conditions d'essai optimales peuvent également varier entre les différents groupes de substances organiques. Les exigences d'essai pour les substances organiques sont généralement plus strictes que celles applicables aux substances inorganiques. En règle générale, les conditions d'essai appropriées à la mesure du relargage des substances organiques s'appliquent également aux substances inorganiques.
NOTE 3 Au sein de la catégorie des substances organiques, une différence de comportement notable existe entre les composés les plus polaires, relativement solubles dans l'eau et les composés organiques hydrophobes (COH), apolaires. Concernant ces derniers, les mécanismes de relargage (par exemple liés à des particules ou liés au carbone organique dissous) peuvent avoir plus d'importance, de même que les pertes dues à la sorption de COH solubles sur différents matériaux avec lesquels ils entrent en contact (par exemple flacons, filtres). Il convient d'utiliser les essais et les résultats pour la lixiviation des substances organiques, uniquement en ayant une connaissance approfondie des propriétés spécifiques des substances en question et des problèmes potentiels qui y sont associés.
NOTE 4 Pour les essais d'écotoxicité, des éluats avec à la fois des substances inorganiques et organiques sont nécessaires. Dans le présent document, les essais d'écotoxicité englobent les essais de génotoxicité.
NOTE 5 En général, l'essai n'est pas adapté aux sols dont la conductivité hydraulique est inférieure à 10−8 m/s (voir également l'Annexe B). Il peut déjà s'avérer difficile de maintenir le débit indiqué pour une conductivité hydraulique saturée comprise entre 10−7 m/s et 10−8 m/s.
L'application de la présente méthode d'essai seule ne suffit pas pour déterminer le comportement à la lixiviation d'un matériau dans des conditions spécifiées différentes de celles applicables au mode opé
Kakovost tal - Postopki izluževanja za nadaljnje kemijsko in ekotoksikološko preskušanje tal in tlem podobnih materialov - 3. del: Preskus v koloni s tokom navzgor (ISO 21268-3:2019)
Ta standard določa preskus, ki je namenjen ugotavljanju izluževanja anorganskih in organskih snovi iz prsti in prsti podobnih materialov. Metoda je preskus s precejanjem ob enkratnem toku navzgor v standardiziranih pogojih pretoka. Izluževanje materiala poteka pri dinamičnih hidravličnih pogojih. Dokument je bil pripravljen za merjenje sproščanja anorganskih in organskih snovi iz prsti in prsti podobnih materialov ter za izdelavo izlužkov za nadaljnje ekotoksikološke preskuse. Za ekotoksikološke preskuse glej standard ISO 15799[6] in ISO 17616[7]. Rezultati preskusa določajo razliko med različnimi vzorci sproščanja, na primer izpiranje in sproščanje pod vplivom interakcije z matriko pri približevanju lokalnemu ravnovesju med materialom in izluževalnim medijem. Ta preskusna metoda proizvede izlužke, ki jih je nato mogoče določiti s fizikalnimi, kemijskimi in ekotoksikološkimi metodami v skladu z obstoječimi standardnimi metodami. Rezultati analize izlužkov so predstavljeni kot funkcija razmerja tekoče/trdno. Preskus ni primeren za snovi, ki so hlapne pri okoljskih pogojih.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-januar-2020
Nadomešča:
SIST-TS CEN ISO/TS 21268-3:2010
Kakovost tal - Postopki izluževanja za nadaljnje kemijsko in ekotoksikološko
preskušanje tal in tlem podobnih materialov - 3. del: Preskus v koloni s tokom
navzgor (ISO 21268-3:2019)
Soil quality - Leaching procedures for subsequent chemical and ecotoxicological testing
of soil and soil-like materials - Part 3: Up-flow percolation test (ISO 21268-3:2019)
Bodenbeschaffenheit - Elutionsverfahren für die anschließende chemische und
ökotoxikologische Untersuchung von Boden und von Bodenmaterialien - Teil 3:
Perkolationstest im Aufwärtsstrom (ISO 21268-3:2019)
Qualité du sol - Modes opératoires de lixiviation en vue d'essais chimiques et
écotoxicologiques ultérieurs des sols et matériaux du sol - Partie 3: Essai de percolation
à écoulement ascendant (ISO 21268-3:2019)
Ta slovenski standard je istoveten z: EN ISO 21268-3:2019
ICS:
13.080.05 Preiskava tal na splošno Examination of soils in
general
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN ISO 21268-3
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2019
EUROPÄISCHE NORM
ICS 13.080.05 Supersedes CEN ISO/TS 21268-3:2009
English Version
Soil quality - Leaching procedures for subsequent chemical
and ecotoxicological testing of soil and soil-like materials -
Part 3: Up-flow percolation test (ISO 21268-3:2019)
Qualité du sol - Modes opératoires de lixiviation en vue Bodenbeschaffenheit - Elutionsverfahren für die
d'essais chimiques et écotoxicologiques ultérieurs des anschließende chemische und ökotoxikologische
sols et matériaux du sol - Partie 3: Essai de percolation Untersuchung von Boden und von Bodenmaterialien -
à écoulement ascendant (ISO 21268-3:2019) Teil 3: Perkolationstest im Aufwärtsstrom (ISO 21268-
3:2019)
This European Standard was approved by CEN on 1 September 2019.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2019 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 21268-3:2019 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
European foreword
This document (EN ISO 21268-3:2019) has been prepared by Technical Committee ISO/TC 190 "Soil
quality" in collaboration with Technical Committee CEN/TC 444 “Test methods for environmental
characterization of solid matrices” the secretariat of which is held by NEN.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by April 2020, and conflicting national standards shall be
withdrawn at the latest by April 2020.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
This document supersedes CEN ISO/TS 21268-3:2009.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the
United Kingdom.
Endorsement notice
The text of ISO 21268-3:2019 has been approved by CEN as EN ISO 21268-3:2019 without any
modification.
INTERNATIONAL ISO
STANDARD 21268-3
First edition
2019-09
Soil quality — Leaching procedures
for subsequent chemical and
ecotoxicological testing of soil and
soil-like materials —
Part 3:
Up-flow percolation test
Qualité du sol — Modes opératoires de lixiviation en vue d'essais
chimiques et écotoxicologiques ultérieurs des sols et matériaux du
sol —
Partie 3: Essai de percolation à écoulement ascendant
Reference number
ISO 21268-3:2019(E)
©
ISO 2019
ISO 21268-3:2019(E)
© ISO 2019
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting
on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address
below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved
ISO 21268-3:2019(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 2
3 Terms and definitions . 2
4 Principle . 3
5 Reagents and materials . 4
6 Apparatus . 4
7 Sample pre-treatment . 6
7.1 Preparation of laboratory sample and specification of particle size . 6
7.2 Preparation of the test sample . 7
7.3 Test portion . 7
7.4 Determination of dry matter content . 7
8 Procedure. 8
8.1 Temperature . 8
8.2 Preparation of the eluent . 8
8.3 Preparation of the column . 8
8.4 Packing of the column . 8
8.5 Start of the test . 9
8.6 Sample Collection and Liquid/Solid separation step .10
8.7 Collection of additional eluate fractions .11
8.8 Further preparation of the eluates for analysis .12
8.9 Blank test .12
9 Calculation .12
10 Test report .13
11 Analytical determination .13
11.1 General .13
11.2 Blank test information .13
12 Performance characteristics .14
12.1 General .14
12.2 Validation trials performed in Japan .15
12.2.1 Round robin tests performed in accordance with ISO/TS 21268-3:2007 .15
12.2.2 Robustness testing and validation results considering equilibration
period and flow rate . .15
[5]
12.3 Validation results obtained in Germany (DIN 19528 ) .16
12.3.1 General.16
12.3.2 Results for validation trial 1 .17
12.3.3 Results for validation trial 2 .20
Annex A (informative) Suggestions for packing the column, water saturationand
establishment of equilibrium conditions .25
Annex B (informative) Justification of the choices made in developing the test procedure .27
Annex C (informative) Calculation of centrifugation duration depending on centrifugation
speed and rotor dimensions.31
Annex D (informative) Additional information on robustness testing and validation results
based on waste materials .33
Bibliography .34
ISO 21268-3:2019(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular, the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www .iso .org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation of the voluntary nature of standards, the meaning of ISO specific terms and
expressions related to conformity assessment, as well as information about ISO's adherence to the
World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see www .iso
.org/iso/foreword .html.
This document was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 7,
Impact assessment.
This first edition of ISO 21268-3:2019 cancels and replaces (ISO/TS 21268-3:2007), which has been
technically revised. The main changes compared to the previous edition are as follows:
— the maximum grain size has been changed to <2 mm as usual for soil;
— demineralized water has been added as possible leachant;
— the column diameter has been changed from "5 cm or 10 cm" to "5 cm to 10 cm";
— flow rate of 30 cm/d has been added as option based on robustness testing;
— 7.1 and 7.2 has been exchanged to read 7.1 "Particle size" and 7.2 "Sample preparation";
— 11.1 "General", 11.2 "Validation trials performed in Japan" and 12.3 "Validation results obtained in
Germany (DIN 19528)" have been added;
— B.2 "Particle size distribution" has been deleted;
— a new informative Annex C "Calculation of centrifugation duration depending on centrifugation
speed and rotor dimensions" has been added;
— references in Clause 2 and Bibliography has been updated.
A list of all parts in the ISO 21268 series can be found on the ISO website.
Any feedback or questions on this document should be directed to the user’s national standards body. A
complete listing of these bodies can be found at www .iso .org/members .html.
iv © ISO 2019 – All rights reserved
ISO 21268-3:2019(E)
Introduction
In various countries, tests have been developed to characterize and assess the substances which can
be released from materials. The release of soluble substances upon contact with water is regarded as
a main mechanism of release, which results in a potential risk to the environment during the use or
disposal of materials. The intent of these tests is to identify the leaching properties of materials. The
[1]
complexity of the leaching process makes simplifications necessary .
Not all of the relevant aspects of leaching behaviour can be addressed in one standard (see description
of influencing factors in Annex A).
Tests to characterise the behaviour of materials can generally be divided into three categories addressed
[2] [3]
in ISO 18772 and EN 12920 . The relationships between these tests are summarized below.
a) “Basic characterization” tests are used to obtain information on the short- and long-term
leaching behaviour and characteristic properties of materials. Liquid/solid (L/S) ratios, leachant
composition, factors controlling leachability, such as pH, redox potential, complexing capacity, role
of dissolved organic carbon (DOC), ageing of material and physical parameters, are addressed in
these tests.
b) “Compliance” tests are used to determine whether the material complies with a specific behaviour
or with specific reference values. The tests focus on key variables and leaching behaviour previously
identified by basic characterisation tests.
c) “On-site verification” tests are used as a rapid check to confirm that the material is the same as that
which has been subjected to the compliance test(s). On-site verification tests are not necessarily
leaching tests.
The test procedure described in this method belongs to category a): basic characterization tests.
[4]
This document was originally elaborated on the basis of CEN/TS 14405:2004 . Especially,
modifications considering requirements on subsequent ecotoxicological testing and analysis of organic
[5]
substances have been included. Validation results have been adopted from DIN 19528 and from
[15,16]
Japanese validation studies .
INTERNATIONAL STANDARD ISO 21268-3:2019(E)
Soil quality — Leaching procedures for subsequent
chemical and ecotoxicological testing of soil and soil-like
materials —
Part 3:
Up-flow percolation test
1 Scope
This document specifies a test, which is aimed at determining the leaching behaviour of inorganic
and organic substances from a soil and soil-like materials. The method is a once-through up-flow
percolation test under standardized conditions of flow rate. The material is leached under dynamic
hydraulic conditions. The document has been developed to measure the release of inorganic and organic
substances from soil and soil-like material as well as to produce eluates for subsequent ecotoxicological
[6] [7]
testing. For ecotoxicological testing, see ISO 15799 and ISO 17616 . The test results enable the
distinction between different release patterns, for instance wash-out and release under the influence of
interaction with the matrix, when approaching local equilibrium between material and leachant.
This test method produces eluates, which can subsequently be characterized by physical, chemical and
ecotoxicological methods in accordance with existing standard methods. The results of eluate analysis
are presented as a function of the liquid/solid (L/S) ratio. The test is not suitable for substances that are
volatile under ambient conditions.
NOTE 1 Volatile organic substances include the low-molecular-weight substances in mixtures such as
mineral oil.
NOTE 2 It is not always possible to optimize test conditions simultaneously for inorganic and organic
substances and optimum test conditions can also vary between different groups of organic substances. Test
requirements for organic substances are generally more stringent than those for inorganic substances. The test
conditions suitable for measuring the release of organic substances will generally also be applicable to inorganic
substances.
NOTE 3 Within the category of organic substances, a significant difference in behaviour exists between the
more polar, relatively water-soluble compounds and apolar, hydrophobic organic substances (HOCs). In the latter
case, mechanisms of release (e.g. particle-bound or dissolved organic carbon-bound) can be more crucial as well
as sorption losses of soluble HOCs on different materials with which they come in contact (e.g. bottles, filters).
The test and the results should be used for leaching of organic substances only with thorough consideration of
the specific properties of the substances in question and the associated potential problems.
NOTE 4 For ecotoxicological testing, eluates representing the release of both inorganic and organic substances
are needed. In this document, ecotoxicological testing is also meant to include genotoxicological testing.
−8
NOTE 5 The test is generally not suitable for soils with hydraulic conductivities below 10 m/s (see also
Annex B). It can be difficult to maintain the designated flow rate already in the range of saturated hydraulic
−7 −8
conductivity between 10 m/s and 10 m/s.
The application of this test method alone is not sufficient for the determination of the leaching
behaviour of a material under specified conditions different to those from the test procedure, since this
generally requires the application of several test methods, behavioural modelling and model validation.
This document does not address issues related to health and safety. It only determines the leaching
properties as outlined in Clause 4.
ISO 21268-3:2019(E)
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements 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.
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 5667-3:2018, Water quality — Sampling — Part 3: Preservation and handling of water samples
ISO 5725-1:1994, Accuracy (trueness and precision) of measurement methods and results — Part 1: General
principles and definitions
ISO 5725-2:1994, Accuracy (trueness and precision) of measurement methods and results — Part 2: Basic
method for the determination of repeatability and reproducibility of a standard measurement method
ISO 7027-1, Water quality — Determination of turbidity — Part 1: Quantitative methods
ISO 10523, Water quality — Determination of pH
ISO 11465, Soil quality — Determination of dry matter and water content on a mass basis —
Gravimetric method
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
3.1
leaching test
test during which a material is put into contact with a leachant (3.2) under strictly defined conditions
and some substances of the material are extracted
3.2
leachant
liquid used in a leaching test (3.1)
Note 1 to entry: For the purposes of this document, the leachant is specified in 5.1.
3.3
eluate
solution recovered from a leaching test (3.1)
Note 1 to entry: Eluate is also referred to as leachate.
3.4
liquid to solid ratio
L/S
ratio between the total volume of liquid (L in litres), which in this extraction is in contact with the soil
sample, and the dry mass of the sample (S in kg of dry matter).
Note 1 to entry: L/S is expressed in l/kg.
2 © ISO 2019 – All rights reserved
ISO 21268-3:2019(E)
3.5
dry matter content
w
dm
ratio expressed in percent between the mass of the dry residue, determined in accordance with
ISO 11465 and the corresponding raw mass.
3.6
laboratory sample
sample or subsample(s) sent to or received by the laboratory
3.7
test sample
sample, prepared from the laboratory sample (3.6), from which test portions (3.8) are removed for
testing or analysis
3.8
test portion
quantity of material of appropriate size for measurement of the concentration or other properties of
interest, taken from the test sample (3.7)
Note 1 to entry: The test portion can be taken from the laboratory sample directly if no pre-treatment of sample
is required, but usually it is taken from the test sample.
Note 2 to entry: A unit or increment of proper homogeneity, size and fineness, needing no further preparation,
can be a test portion.
3.9
soil-like material
excavated soil, dredged materials, manufactured soils, treated soils and fill materials
4 Principle
This document describes a method to determine the release of substances from soil and soil-like
material, packed in a column with leachant percolating through it. A continuous vertical up-flow is
used, which allows a column test under water-saturated conditions. The test conditions, including
the flow rate of the leachant, are chosen such that the substances that are rapidly washed out and the
substances that are released under the influence of interaction with the matrix can be deduced from
the results. It is intended and assumed that conditions approach local equilibrium between the material
and the leachant throughout the test.
The test portion, which originally or after suitable pre-treatment has a particle size less than or equal
to 2 mm, is brought into contact with water containing a low concentration (0,001 mol/l) of calcium
chloride or demineralised water (5.1) under defined conditions. The leachant is percolated in up-flow
direction through the column at a specified flow rate up to a fixed L/S ratio. The eluate is collected in
several separate fractions. The standard method is based on the assumption that equilibrium or near-
equilibrium is achieved between the liquid and solid phases during the test period. The properties
of the eluate are measured using methods developed for water analysis adapted to meet criteria for
analysis of eluates, and the eluate may be subjected to subsequent ecotoxicological testing.
After the test, the leaching conditions, in terms of pH, electrical conductivity, and optionally, turbidity,
dissolved organic carbon (DOC) or redox potential imposed by the material shall be recorded.
NOTE 1 These parameters often control the leaching behaviour of soil materials and are therefore important
for evaluation of the test results. DOC, in particular, is crucial in soil and soil-like materials for many inorganic
and organic substances.
NOTE 2 The leachant is 0,001 mol/l CaCl to minimize the mobilisation of DOC caused by an ionic strength of
the leachant which is too low.
ISO 21268-3:2019(E)
The properties of the eluate are measured using methods developed for water analysis adapted to
meet criteria for analysis of eluates and/or the eluate may be subjected to subsequent ecotoxicological
testing.
The results of the test are expressed as a function of L/S ratio, in terms of both concentration (mg of the
substances released per litre eluate) and release [mg of the substances released cumulatively per kg of
material (dry mass)] of the substances.
The procedure described in this document is based on the more stringent test requirements for
determining the release of organic substances and/or for subsequent ecotoxicological testing. If only
the release of inorganic substances is to be measured, simplifications may be adapted for some steps of
the procedure.
5 Reagents and materials
5.1 Demineralised water or deionised water or water of equivalent purity (5 < pH < 7,5), with a
conductivity <0,5 mS/m in accordance with grade 3 specified in ISO 3696 made to 0,001 mol/l CaCl .
5.2 Calcium chloride (CaCl · 2 H O), analytical grade.
2 2
5.3 Sodium azide (NaN ), analytical grade.
5.4 Nitric acid (HNO ), analytical grade, made to 0.1 mol/l rinsing solution.
5.5 Organic solvent (acetone, analytical grade) for rinsing and cleaning.
6 Apparatus
6.1 Column, made of glass with an internal diameter of 5 cm to 10 cm and a filling height of about
(30 ± 5) cm, fitted with filters (6.3) in the bottom and top sections made of appropriate materials
ensuring minimum interference with the substances of interest. In the top and bottom of the column, a
filter plate or a thin layer of fine-grained non-reactive material (e.g. fine quartz sand) is applied to ensure
proper water flow over the width of the column and as a support for the pre-filter.
NOTE 1 A drawing of the column and accompanying equipment is given in Figure 1.
NOTE 2 Glass of high quality is usually considered adequate for both metal and organic substances,
particularly since the pH range usually covered in soil testing does not reach the conditions (pH > 10 and pH < 3)
where glass itself is attacked. For ecotoxicity testing, eluates with both metal and organic substances are needed,
which emphasises the need to generate integrated eluates.
NOTE 3 When only organic substances are analysed, stainless steel column and fittings can be applied taking
[9]
into account a certain degree of sorption which can be tested in advance . When only inorganic substances are
analysed, column made of plastics can be applied.
NOTE 4 In the case of quartz sand used as filter material, it shall be tested to be free of leachable substances
blank free. As necessary it can be washed with demineralized water to remove fines and gently dried afterwards
not exceeding 25 °C to avoid enhancing the sorption capacity on the surface of quartz grains. The quartz sand can
be treated with acetone first in case of blank values of organic substances under investigation.
NOTE 5 To prevent organic compounds from degradation by light use a dark room, dark colored glassware or
place a layer of aluminium-foil around the leaching equipment.
4 © ISO 2019 – All rights reserved
ISO 21268-3:2019(E)
6.2 Filters, for filtration of the eluates; they shall not adsorb the compounds of interest. This shall be
tested in preliminary experiments.
The filters shall be chosen so as not to adsorb (or release) substances of interest.
NOTE This can be tested in preliminary experiments.
6.3 Pre-filters, for the column with a pore size of 1 µm to 20 µm.
The filters shall be chosen so as not to adsorb (or release) substances of interest.
NOTE This can be tested in preliminary experiments.
6.4 Pump, with an adjustable capacity of between 0 ml/h and 60 ml/h (e.g. peristaltic pump).
6.5 Analytical balance, with an accuracy of at least 0,1 g.
6.6 pH meter, in accordance with ISO 10523 with an accuracy of at least ± 0,05 pH units.
6.7 Electrical conductivity meter, with an accuracy of at least 0,1 mS/m.
6.8 Tubing material, adapted to the analysis to be performed (see ISO 5667-3:2018, Table A.1).
NOTE When both organic and inorganic substances are analysed Perfluoro-Ethylene-Propylene (FEP) can
be used. When only inorganic substances are analysed, PTFE or similar tubing materials can be used.
6.9 High-quality glass bottles of an appropriate volume, and with a screw cap with a PTFE inlay, for
eluate collection and preservation of eluate samples (in accordance with ISO 5667-3).
NOTE If only inorganic substances are analysed, alternative bottle materials can be selected [e.g. high
density polyethylene (HDPE) or PTFE)].
6.10 Crushing equipment, a jaw crusher or a cutting device.
6.11 Sieving equipment, with sieves of 2 mm or 4 mm nominal screen size.
6.12 Sample splitter, for sub-sampling of laboratory samples (optional).
6.13 Redox potential meter (optional).
6.14 Turbidity meter, as specified in ISO 7027-1.
6.15 Centrifuge, refrigerated, operating at 20 000 g to 30 000 g using centrifuge tubes of appropriate
material , which is inert with regard to both inorganic and organic compounds and suitable for high-
[8]
speed centrifugation (e.g. perfluoroalkoxy alkane (PFA), stainless steel .).
Alternatively, if a high-speed centrifuge is not available, a centrifuge operating at 2 000 g to 2 500 g
using glass bottles may be used in combination with increased centrifugation time. Guidance on the
calculation of the rotor-specific duration of centrifugation is given in Annex C in order to ensure a
comparable degree of efficiency of centrifugation at varying rotation speed. Cooling shall be applied to
maintain the desired temperature.
ISO 21268-3:2019(E)
6.16 Rammer to support packing of the column as specified in 8.4
Key
1 leachant storage container 4 sample material
2 pump 5 pre-filter and or filter layer
3 column 6 eluate collection bottle
Figure 1 — Schematic view of up-flow percolation test
7 Sample pre-treatment
7.1 Preparation of laboratory sample and specification of particle size
A representative laboratory sample of at least 2 kg (dry matter) is obtained (e.g. as described in
[10-13] [14]
ISO 18400-101, ISO 18400-104, ISO 18400-105, ISO 18400-202 and ISO 23909 ) and shall be
stored in closed packages and at low temperatures (4 °C), in order to avoid unwanted changes in the
[12]
material (see e.g. ISO 18400-105 ).
The test shall be carried out on soil or soil-like material sieved to <2 mm (e.g. as described in
[9]
ISO 11464 ). Oversized material of natural origin in the sample shall be separated and discarded. The
type and amount of all discarded material shall be reported. If oversized material of anthropogenic
origin is present and assumed to contain substances of interest, this part can be subject to alternative
sample preparation or testing.
If the laboratory sample cannot be homogenised or sieved because of its water content, it is allowed in
[9]
this case only to dry the laboratory sample (e.g. as described in ISO 11464 ). The drying temperature
shall not exceed 30 °C.
NOTE 1 Sieving and drying at more than 30 °C, as well as crushing, can lead to a loss of semi-volatile substances
(inorganic and organic) and can alter the leaching characteristics (refer also to A.3.6).
NOTE 2 Due to sieving, contamination of the sample can occur to an extent that affects the leaching of some
substances of concern, e.g. chromium, nickel and molybdenum from stainless steel equipment or plasticisers
from plastic sieves.
6 © ISO 2019 – All rights reserved
ISO 21268-3:2019(E)
7.2 Preparation of the test sample
Use a sample splitter (6.12) or apply coning and quartering to split the laboratory sample and obtain a test
sample. The size of test sample required depends on the volume of eluate needed for the specific purpose
and the subsequent chemical analysis and/or ecotoxicological tests to be carried out on the eluate.
NOTE 1 If needed for chemical analysis or ecotoxicological testing, larger volumes of eluate can be obtained
by combining eluates from replicate tests after centrifugation (or filtration). Alternatively, larger volumes of
eluate can also be produced in a single test, provided that the ratios in terms of L/S and minimum headspace are
maintained.
NOTE 2 The required amount of the test sample is dependent on the particle size distribution of the soil to be
[14]
analysed (see ISO 23909 ). The specified sample amount will generally be adequate. In specific cases, a smaller
sample amount can be accepted, for instance, if for specific reasons less material is available, provided that the
test can be carried out as specified in 7.2 to 7.4.
7.3 Test portion
Take, from the test sample, a test portion with an appropriate volume (e.g. approximately 0,6 l, if the
column has a diameter of 5 cm, and of 2,4 l, if the column has a diameter of 10 cm). Use a sample splitter
(6.12) or apply coning and quartering to split the test sample.
The inner diameter of the column shall be chosen in such a way that the largest particle size is at least
3 times but preferably 10 times smaller than the diameter of the column.
NOTE 1 If needed for chemical analysis or ecotoxicological testing, larger volumes of eluate can be obtained by
combining eluates from replicate tests after centrifugation (or filtration). Alternatively, larger volumes of eluate
may also be produced by using an appropriate column dimension within the range specified in 6.1.
NOTE 2 The volume of eluate required depends on the specific purpose and the subsequent chemical analysis
and/or ecotoxicological tests to be carried out on the eluate. Analysis for inorganic substances can typically
require from 20 ml to 500 ml of eluate, analysis for organic substances from 250 ml to 2 000 ml, depending
on the number and type of groups of organic substances to be analysed (DOC from 100 ml to 250 ml), and
ecotoxicological testing from 100 ml to 2 000 ml.
7.4 Determination of dry matter content
The whole test sample, complying with the size criterion in 7.1, shall not be further dried. The water
content of the test sample shall be determined on a separate test portion at (105 ± 5) °C. If the soil sample
is air-dried prior to testing, the dry matter content w of the air-dried sample shall be determined as
dm
well. The dry mass of the sample shall be determined at (105 ± 5) °C in accordance with ISO 11465 and
the dry matter content is calculated in Formula (1):
wm=×100 m (1)
dm DW
where
w is the dry matter content, expressed in percent (%);
dm
m is the mass of the dried sample, expressed in kilograms (kg);
D
m is the mass of the undried sample, expressed in kilograms (kg).
W
NOTE If volatile or unstable compounds are present in the soil sample, this gravimetric method cannot be
used for accurate determination of the water content.
If, for reasons expressed in 7.1, the material was (partly) dried before sample splitting, the overall mass
loss shall be taken into account.
ISO 21268-3:2019(E)
8 Procedure
8.1 Temperature
The percolation test shall be carried out at a temperature of (22 ± 3) °C.
NOTE A constant temperature of 22 °C in the test can be achieved by either controlling the temperature
of the laboratory, or controlling the temperature of the leachant and insulating the column and accompanying
equipment.
For material that is very sensitive to biological degradation, performance of the test at reduced
temperature (e.g. 4 °C) and preventing direct exposure to light will limit biological activity significantly.
A reduced temperature may result in slower/lower release of organic substances and hence lower
concentrations of these compounds in the leachates. If the test is modified in this way, this deviation
shall be reported in the test report.
8.2 Preparation of the eluent
Prepare a solution made to 0,001 M CaCl by dissolving 0,147 g CaCl in water and dilute to 1 000 ml.
2 2
In special cases (i.e. measurement of Ca and/or chloride in the eluate are of interest or the sample
exhibits an own salt load), water without addition of CaCl can also be used. The leachant type used
shall be recorded in the test report.
NOTE 1 The application of demineralized water as leachant can induce higher turbidity and lower ionic
strength in the eluate for some types of soils (e.g. high content of organic matter) and can cause increased
concentrations of analytes adsorbed to colloids.
NOTE 2 For eluates that are not to be used for ecotoxicological testing, sodium azide (NaN ) can be added
to a resulting concentration of 0,1 % in order to reduce microbial degradation of organic substances. However,
the addition of NaN is known to only minimize biodegradation if a very high but in turn extremely poisonous
concentration in the eluent is applied. Therefore, other appropriate measures can be considered to prevent/
reduce biodegradation in the sample or collected eluate (e.g. application of γ-radiation to the sample, dark and
air-conditioned room, shorter eluate collection periods, etc). If only inorganic compounds are measured, the
addition of NaN is not appropriate.
8.3 Preparation of the column
Rinse the column, including the top and bottom sections (6.1), pre-filters (6.3), tubing material (6.8)
and bottles (6.9) with nitric acid and/or an organic solvent (5.2) and water (5.1), respectively. Weigh
the dry column, including the top and bottom sections, filters and filter plates or layers of fine-grained
material, to an accuracy of 1 g.
NOTE Alternatively, heat treatment of used glassware at 550 °C can be used to remove traces of analytes.
However, this treatment has been shown to increase adsorption of organic substance from the air substance.
8.4 Packing of the column
Fit the bottom section, equipped with a filter plate or a layer of fine-grained chemically inert material
(e.g. fine quartz sand) of approximately 1 cm and a pre-filter (6.3) to the column. Fill the column with
the test portion, up to a bed height of (30 ± 5) cm in at least five consecutive layers.
Introduce each layer into the column in three sub-layers and level each sub-layer separately.
8 © ISO 2019 – All rights reserved
ISO 21268-3:2019
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.
Loading comments...