SIST EN ISO 21268-4:2020

Soil quality - Leaching procedures for subsequent chemical and ecotoxicological testing of soil and soil-like materials - Part 4: Influence of pH on leaching with initial acid/base addition (ISO 21268-4:2019)

This Standard specifies a test to obtain information on the short- and long-term leaching behaviour and characteristic properties of materials. The document has been developed to measure the pH- dependent 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 and ISO 17616. The equilibrium condition, as defined in this document, is established by the addition of predetermined amounts of acid or base to reach desired final pH values. The test method produces eluates, which can subsequently be characterized by physical, chemical and ecotoxicological methods in accordance with existing standard methods. The test is not suitable for substances that are volatile under ambient conditions. For the purposes of ecotoxicological tests, the relevant pH range (see 8.2) will usually be pH 5 to pH 9. This test is mainly aimed at being used for routine and control purposes, and it cannot be used alone to describe all leaching properties of a soil. Additional leaching tests are needed for that extended goal. This document does not address issues related to health and safety. It only determines the leaching properties outlined in Clause 5.

Bodenbeschaffenheit - Elutionsverfahren für die anschließende chemische und ökotoxikologische Untersuchung von Boden und von Bodenmaterialien - Teil 4: Einfluss des pH–Wertes unter vorheriger Säure/Base-Zugabe (ISO 21268-4:2019)

Dieses Dokument legt ein Prüfverfahren fest, um Angaben über das kurzfristige und langfristige Elutionsverhalten und zu den charakteristischen Eigenschaften von Materialien zu erhalten.
Dieses Dokument wurde erstellt, um die pH abhängige Freisetzung anorganischer und organischer Substanzen aus Boden und bodenähnlichem Material zu untersuchen und um Eluate für nachfolgende ökotoxikologische Untersuchungen herzustellen. Hinsichtlich der ökotoxikologischen Prüfung siehe ISO 15799 und ISO 17616. Der Gleichgewichtszustand, wie er in diesem Dokument definiert ist, wird durch Zugabe von vorher bestimmten Mengen an Säure oder Base hergestellt, um die gewünschten endgültigen pH Werte zu erreichen.
ANMERKUNG 1   Zu den flüchtigen organischen Substanzen gehören niedermolekulare Substanzen in Gemischen 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 eher 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 Problemen bei der 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 ökotoxi-kologische Untersuchung auch die genotoxikologische Untersuchung.
Durch das Prüfverfahren werden Eluate hergestellt, die anschließend mit physikalischen, chemischen und ökotoxikologischen Verfahren nach bestehenden Standardverfahren charakterisiert werden können. Die Prüfung ist nicht geeignet für Substanzen, die unter Umgebungsbedingungen flüchtig sind.
Für die Durchführung ökotoxikologischer Untersuchungen liegt der betreffende pH Wert-Bereich (siehe 8.2) üblicherweise zwischen 5 und 9.
Dieses Prüfverfahren ist hauptsächlich darauf ausgerichtet, für Routine  und Kontrollzwecke angewendet zu werden; es ist allein nicht ausreichend, um alle Elutionseigenschaften eines Bodens zu beschreiben. Für diese erweiterte Zielsetzung sind weitere Elutionstests erforderlich. Dieses Dokument befasst sich nicht mit gesundheitlichen und sicherheitstechnischen Belangen. Es dient nur der Bestimmung der in Abschnitt 5 dargestellten Elutionseigenschaften.

Qualité du sol - Modes opératoires de lixiviation en vue d'essais chimiques et écotoxicologiques ultérieurs des sols et matériaux du sol - Partie 4: Essai de dépendance au pH avec ajout initial d'acide/base (ISO 21268-4:2019)

Le présent document spécifie un essai permettant d'obtenir des informations sur le comportement à la lixiviation à court terme et à long terme ainsi que sur les propriétés caractéristiques des matériaux.
Le présent document a été conçu pour étudier le relargage, en fonction du pH, de substances organiques et inorganiques à partir du sol et des matériaux analogues au sol et produire des éluats destinés aux essais écotoxicologiques ultérieurs. Pour en savoir plus sur les essais écotoxicologiques, voir l'ISO 15799 et l'ISO 17616. L'état d'équilibre tel que défini dans le présent document s'obtient en ajoutant des quantités prédéterminées d'acide ou de base afin d'atteindre les valeurs de pH finales désirées.
NOTE 1    Les substances organiques volatiles incluent les substances de 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, et les conditions d'essai optimales peuvent également varier entre différents groupes de substances organiques. Pour les substances organiques, les exigences des essais sont généralement plus contraignantes que pour les substances inorganiques. En général, les conditions d'essai adaptées pour mesurer le relargage des substances organiques seront également applicables 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 substances 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 écotoxicologiques, des éluats représentant le relargage des substances à la fois organiques et inorganiques sont nécessaires. Dans le présent document, les essais écotoxicologiques englobent les essais génotoxicologiques.
Cette méthode d'essai produit des éluats qui peuvent ensuite être caractérisés par des méthodes physiques, chimiques et écotoxicologiques selon des méthodes normalisées existantes. L'essai n'est pas adapté aux substances qui sont volatiles dans des conditions ambiantes.
Pour les besoins des essais écotoxicologiques, la plage de pH applicable (voir 8.2) sera généralement comprise entre 5 et 9.
L'essai est principalement destiné aux fins de contrôle et d'analyse de routine, et il ne peut être utilisé seul pour décrire toutes les propriétés de lixiviation d'un sol. D'autres essais sont nécessaires pour atteindre cet objectif plus large. Le présent document ne traite pas des problèmes liés à la santé et à la sécurité. Il permet uniquement de déterminer les propriétés de lixiviation telles que décrites à l'Article 5.

Kakovost tal - Postopki izluževanja za nadaljnje kemijsko in ekotoksikološko preskušanje tal in tlem podobnih materialov - 4. del: Vpliv pH na izluževanje z začetnim dodatkom kisline ali baze (ISO 21268-4:2019)

Ta standard določa preskus za pridobitev informacij o kratkoročnem in dolgoročnem izluževanju ter značilnih lastnostih materialov. Dokument je bil pripravljen za merjenje od pH odvisnega sproščanja anorganskih in organskih snovi iz prsti in prsti podobnih materialov ter za izdelavo izlužkov za nadaljnje ekotoksikološke preskuse. Za ekotoksikološke preskuse glej ISO 15799 in ISO 17616. Ravnotežno stanje, kot je opredeljeno v tem dokumentu, je določeno z dodajanjem vnaprej določenih količin kisline ali baze, da se dosežejo želene končne vrednosti pH. Preskusna metoda proizvede izlužke, ki jih je nato mogoče določiti s fizikalnimi, kemijskimi in ekotoksikološkimi metodami v skladu z obstoječimi standardnimi metodami. Preskus ni primeren za snovi, ki so hlapne pri okoljskih pogojih. Za namen ekotoksikoloških preskusov bo ustrezni obseg vrednosti pH običajno od pH 5 do pH 9 (glej točko 8.2). Ta preskus se uporablja predvsem za rutinske in kontrolne namene, preskusa pa ni mogoče uporabiti samostojno za opis vseh izluževalnih lastnosti tal. Za ta razširjeni cilj so potrebni dodatni izluževalni preskusi. Ta dokument ne obravnava vprašanj v zvezi z zdravjem in varnostjo, ampak zgolj določa izluževalne lastnosti, opisane v točki 5.

General Information

• Status: Published
• Public Enquiry End Date: 24-Apr-2018
• Publication Date: 11-Dec-2019
• ICS: 13.080.05 - Examination of soils in general
• Technical Committee: KAT - Soil quality
• Current Stage: 6060 - National Implementation/Publication (Adopted Project)
• Start Date: 05-Nov-2019
• Due Date: 10-Jan-2020
• Completion Date: 12-Dec-2019
• Ref Project: EN ISO 21268-4:2019 - Soil quality - Leaching procedures for subsequent chemical and ecotoxicological testing of soil and soil-like materials - Part 4: Influence of pH on leaching with initial acid/base addition (ISO 21268-4:2019)

Relations

• Replaces: SIST-TS CEN ISO/TS 21268-4:2010 - Soil quality - Leaching procedures for subsequent chemical and ecotoxicological testing of soil and soil materials - Part 4: Influence of pH on leaching with initial acid/base addition (ISO/TS 21268-4:2007)
• Effective Date: 01-Jan-2020

Standards Content (Sample)

SLOVENSKI STANDARD
SIST EN ISO 21268-4:2020
01-januar-2020
Nadomešča:
SIST-TS CEN ISO/TS 21268-4:2010
Kakovost tal - Postopki izluževanja za nadaljnje kemijsko in ekotoksikološko
preskušanje tal in tlem podobnih materialov - 4. del: Vpliv pH na izluževanje z
začetnim dodatkom kisline ali baze (ISO 21268-4:2019)
Soil quality - Leaching procedures for subsequent chemical and ecotoxicological testing
of soil and soil-like materials - Part 4: Influence of pH on leaching with initial acid/base
addition (ISO 21268-4:2019)
Bodenbeschaffenheit - Elutionsverfahren für die anschließende chemische und
ökotoxikologische Untersuchung von Boden und von Bodenmaterialien - Teil 4: Einfluss
des pH–Wertes unter vorheriger Säure/Base-Zugabe (ISO 21268-4:2019)
Qualité du sol - Modes opératoires de lixiviation en vue d'essais chimiques et
écotoxicologiques ultérieurs des sols et matériaux du sol - Partie 4: Essai de
dépendance au pH avec ajout initial d'acide/base (ISO 21268-4:2019)
Ta slovenski standard je istoveten z: EN ISO 21268-4:2019
ICS:
13.080.05 Preiskava tal na splošno Examination of soils in
general
SIST EN ISO 21268-4:2020 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 21268-4:2020

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SIST EN ISO 21268-4:2020


EN ISO 21268-4
EUROPEAN STANDARD

NORME EUROPÉENNE

December 2019
EUROPÄISCHE NORM
ICS 13.080.05 Supersedes CEN ISO/TS 21268-4:2009
English Version

Soil quality - Leaching procedures for subsequent chemical
and ecotoxicological testing of soil and soil-like materials -
Part 4: Influence of pH on leaching with initial acid/base
addition (ISO 21268-4:2019)
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 analogues au sol - Partie 4: Essai de Untersuchung von Boden und von Bodenmaterialien -
dépendance au pH avec ajout initial d'acide/de base Teil 4: Einfluss des pH-Wertes unter vorheriger
(ISO 21268-4:2019) Säure/Base-Zugabe (ISO 21268-4:2019)
This European Standard was approved by CEN on 6 October 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 21268-4:2019 E
worldwide for CEN national Members.

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SIST EN ISO 21268-4:2020
EN ISO 21268-4:2019 (E)
Contents Page
European foreword . 3

2

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SIST EN ISO 21268-4:2020
EN ISO 21268-4:2019 (E)
European foreword
This document (EN ISO 21268-4:2019) 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 June 2020, and conflicting national standards shall be
withdrawn at the latest by June 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 21268-4:2009.
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 21268-4:2019 has been approved by CEN as EN ISO 21268-4:2019 without any
modification.


3

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SIST EN ISO 21268-4:2020

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SIST EN ISO 21268-4:2020
INTERNATIONAL ISO
STANDARD 21268-4
First edition
2019-10
Soil quality — Leaching procedures
for subsequent chemical and
ecotoxicological testing of soil and
soil-like materials —
Part 4:
Influence of pH on leaching with initial
acid/base addition
Qualité du sol — Modes opératoires de lixiviation en vue d'essais
chimiques et écotoxicologiques ultérieurs des sols et matériaux
analogues au sol —
Partie 4: Essai de dépendance au pH avec ajout initial d'acide/de base
Reference number
ISO 21268-4:2019(E)
©
ISO 2019

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SIST EN ISO 21268-4:2020
ISO 21268-4:2019(E)

COPYRIGHT PROTECTED DOCUMENT
© 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: [phone]
Fax: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved

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SIST EN ISO 21268-4:2020
ISO 21268-4:2019(E)

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Principle . 3
5 Reagents . 4
6 Apparatus . 4
7 Sample pretreatment . 6
7.1 Preparation of laboratory sample and specification of particle size . 6
7.2 Preparation of test sample . 6
7.3 Determination of the dry matter content and of water content . 6
7.4 Preparation of the test portion . 7
8 Procedure. 7
8.1 Contact time . 7
8.2 pH-range . 7
8.3 Leaching test . 8
8.3.1 General. 8
8.3.2 Preparation of leachants . 8
8.3.3 Leaching step . 9
8.3.4 Liquid/solid separation step .10
8.4 Natural pH .11
8.5 Further preparation of the eluate for analysis.11
8.6 Blank test .11
9 Calculation .12
10 Test report .12
11 Analytical determination .13
11.1 General .13
11.2 Blank test information .13
12 Performance characteristics .13
Annex A (informative) Example of a specific liquid-solid separation procedure for soil samples .14
Annex B (informative) Operation and uses of the test — Influence of pH on the leaching
behaviour .16
Annex C (informative) Preliminary determination of the acid/base consumption .20
Annex D (informative) Repeatability and reproducibility data .24
Annex E (informative) Calculation of centrifugation duration depending on centrifugation
speed and rotor dimensions.28
Bibliography .30
© ISO 2019 – All rights reserved iii

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SIST EN ISO 21268-4:2020
ISO 21268-4:2019(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 21268-4 cancels and replaces ISO/TS 21268-4:2007, 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;
— references in Clause 2 and the Bibliography have been updated;
— Clause 12 “Performance characteristics” has been technically revised;
— a new informative Annex D “Repeatability and reproducibility data” has been added;
— a new informative Annex E "Calculation of centrifugation duration depending on centrifugation
speed and rotor dimensions" has been added.
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

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SIST EN ISO 21268-4:2020
ISO 21268-4:2019(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.
Tests to characterize the behaviour of materials can generally be divided into three categories
addressed in ISO 18772 and EN 12920. The relationships between these tests are summarized below.
“Basic characterization” tests are used to obtain information on the short- and long-term leaching
behaviour and characteristic properties of materials. Liquid/solid ratios (L/S), 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 defined tests.
“Compliance” tests are used to determine whether the material complies with a specific behaviour or
with specific reference values. These tests focus on key variables and leaching behaviour previously
identified by basic characterization tests.
“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.
This document was originally elaborated on the basis of CEN/TS 14429:2005. Especially, modifications
considering requirements on subsequent ecotoxicological testing and analysis of organic substances
[5]
have been included. Validation results have been adopted from US-EPA .
© ISO 2019 – All rights reserved v

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SIST EN ISO 21268-4:2020
INTERNATIONAL STANDARD ISO 21268-4:2019(E)
Soil quality — Leaching procedures for subsequent
chemical and ecotoxicological testing of soil and soil-like
materials —
Part 4:
Influence of pH on leaching with initial acid/base addition
1 Scope
This document specifies a test to obtain information on the short- and long-term leaching behaviour
and characteristic properties of materials.
The document has been developed to measure the pH-dependent 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 and ISO 17616. The equilibrium condition, as defined
in this document, is established by the addition of predetermined amounts of acid or base to reach
desired final pH values.
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 meant to include genotoxicological testing.
The test method produces eluates, which can subsequently be characterized by physical, chemical and
ecotoxicological methods in accordance with existing standard methods. The test is not suitable for
substances that are volatile under ambient conditions.
For the purposes of ecotoxicological tests, the relevant pH range (see 8.2) will usually be pH 5 to pH 9.
This test is mainly aimed at being used for routine and control purposes, and it cannot be used alone
to describe all leaching properties of a soil. Additional leaching tests are needed for that extended goal.
This document does not address issues related to health and safety. It only determines the leaching
properties outlined in Clause 5.
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 2019 – All rights reserved 1

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SIST EN ISO 21268-4:2020
ISO 21268-4:2019(E)

ISO 5667-3, Water quality — Sampling — Part 3: Preservation and handling of water samples
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 purpose of this document, the leachant is specified in 6.1
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 litres per kilogram (l/kg).
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
water content
w
HO
2
ratio, expressed in percent, between the mass of water contained in the material as received and the
corresponding dry residue of the material
Note 1 to entry: The basis for the calculation of the water content is the mass of the dry residue in this document,
as specified in ISO 11465 (for the determination of the water content of soil).
2 © ISO 2019 – All rights reserved

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SIST EN ISO 21268-4:2020
ISO 21268-4:2019(E)

3.7
laboratory sample
sample or subsample(s) sent to or received by the laboratory
3.8
test sample
sample, prepared from the laboratory sample (3.7), from which test portions (3.9) are removed for
testing or analysis
3.9
test portion
quantity of material of appropriate size for measurement of the concentration or other properties of
interest taken from the test sample (3.8)
Note 1 to entry: The test portion can be taken from the laboratory sample (3.7) directly if no pre-treatment of the
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.
3.10
soil-like material
excavated soil, dredged materials, manufactured soils, treated soils and fill materials
4 Principle
The test portions, which originally or after suitable pre-treatment have a particle size less than or equal
to 2 mm, are brought into contact with water containing a low concentration (0,001 mol/l) of calcium
chloride or demineralised water (5.1) under defined conditions. Several separate test portions (up to
eight) are leached at a fixed L/S ratio (L/S = 10 l/kg) with leachants containing different preselected
amounts of acid or base in order to reach stationary pH values at the end of the extraction period (see
8.4). Each leachant is added in three steps in the beginning of the test. In the full test, eight final pH-
values are required, covering the range pH 4 to pH 12 (both included, i.e. the lowest value 4 and the
highest value 12). The amount of acid or base needed to cover the pH range can be derived from the
results of a preliminary titration, from available experimental data on the material to be tested or
from an arbitrary division of the predetermined maximum consumption of acid and base. The tests are
carried out at a fixed contact time at the end of which an equilibrium condition can be assumed to be
reached for most substances in most soil-like materials to be characterized. The equilibrium condition,
as defined in this document, is verified at the end of the extraction period.
The results are expressed in milligrams per litre (mg/l) of substances for each final pH value. For each
+
final pH value, the quantity of acid that is added is also expressed in mol H /kg dry matter and the
+
quantity of base that is added is expressed as negative mol H /kg dry matter.
NOTE 1 This test may also be performed using continuous pH control. The results are generally consistent
(see Annex B).
NOTE 2 Other expressions of results are possible (including mg/kg of dry matter).
From the amount of acid and base used to reach a given end pH, the acid neutralization capacity (ANC)
or base neutralization capacity (BNC) of the soil or soil-like material can also be determined.
NOTE 3 The pH range covered by the test can be restricted to a pH range relevant for the specific material and
the considered problem (see 8.2).
NOTE 4 The leachant is made with 0,001 mol/l CaCl to minimize the mobilization of DOC caused by a too-
2
low ionic strength of the leachant. At the level of 0,001 mol/l CaCl the complexation of metals with chloride is
2
considered to be negligible.
© ISO 2019 – All rights reserved 3

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SIST EN ISO 21268-4:2020
ISO 21268-4:2019(E)

The substances in the eluate(s) are measured using methods developed for water analysis adapted
to meet criteria for analysis of eluates. The eluate may also be applied for subsequent ecotoxicity or
genotoxicity testing.
After the test, the leaching conditions (in terms of pH, electrical conductivity, DOC and, optionally,
turbidity and redox potential dictated by the material) are recorded.
NOTE 5 These parameters often control the leaching behaviour of soil-like materials and are therefore
important for checking the leaching test.
5 Reagents
Reagents used shall be of analytical grade purity.
5.1 Demineralized water or deionized water or water of equivalent purity (5 < pH < 7,5) with
a conductivity of < 0,5 mS/m in accordance with grade 3 specified in ISO 3696 made to 0,001 mol/l CaCl .
2
5.2 Calcium chloride (CaCl · 2 H O), analytical grade.
2 2
5.3 Sodium azide (NaN ), analytical grade.
3
5.4 Nitric acid (pro-analysis) (HNO ), 0,1 mol/l to 5 mol/l, and 0,1 mol/l rinsing solution.
3
5.5 Sodium hydroxide (NaOH) or potassium hydroxide (KOH), 0,1 mol/l to 5 mol/l.
+ +
NOTE The use of KOH instead of NaOH may enhance the leaching of certain cati
...

SLOVENSKI STANDARD
oSIST prEN ISO 21268-4:2018
01-april-2018
.DNRYRVWWDO3RVWRSNLL]OXåHYDQMD]DQDGDOMQMHNHPLMVNRLQHNRWRNVLNRORãNR
SUHVNXãDQMHWDOLQWDOQLK]HPHOMVNLKPDWHULDORYGHO9SOLYS+QDL]OXåHYDQMH]
]DþHWQLPGRGDWNRPNLVOLQHDOLED]H,62',6
Soil quality - Leaching procedures for subsequent chemical and ecotoxicological testing
of soil and soil materials - Part 4: Influence of pH on leaching with initial acid/base
addition (ISO/DIS 21268-4:2018)
Bodenbeschaffenheit - Elutionsverfahren für die anschließende chemische und
ökotoxikologische Untersuchung von Boden und von Bodenmaterialien - Teil 4: Einfluss
des pH–Wertes unter vorheriger Säure/Base-Zugabe (ISO/DIS 21268-4:2018)
Qualité du sol - Modes opératoires de lixiviation en vue d'essais chimiques et
écotoxicologiques ultérieurs des sols et matériaux du sol - Partie 4: Essai de
dépendance au pH avec ajout initial d'acide/base (ISO/DIS 21268-4:2018)
Ta slovenski standard je istoveten z: prEN ISO 21268-4
ICS:
13.080.05 Preiskava tal na splošno Examination of soils in
general
oSIST prEN ISO 21268-4:2018 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
oSIST prEN ISO 21268-4:2018

---------------------- Page: 2 ----------------------
oSIST prEN ISO 21268-4:2018
DRAFT INTERNATIONAL STANDARD
ISO/DIS 21268-4
ISO/TC 190/SC 7 Secretariat: DIN
Voting begins on: Voting terminates on:
2018-02-08 2018-05-03
Soil quality — Leaching procedures for subsequent
chemical and ecotoxicological testing of soil and soil
materials —
Part 4:
Influence of pH on leaching with initial acid/base addition
Qualité du sol — Modes opératoires de lixiviation en vue d'essais chimiques et écotoxicologiques ultérieurs
des sols et matériaux du sol —
Partie 4: Essai de dépendance au pH avec ajout initial d'acide/base
ICS: 13.080.05
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
ISO/CEN PARALLEL PROCESSING
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 21268-4:2018(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
©
PROVIDE SUPPORTING DOCUMENTATION. ISO 2018

---------------------- Page: 3 ----------------------
oSIST prEN ISO 21268-4:2018
ISO/DIS 21268-4:2018(E) ISO/DIS 21268-4:2017(E)

Contents Page
Foreword . v
Introduction . vi
1 Scope .1
2 Normative references .1
3 Terms and definitions .2
4 Symbols and abbreviations .3
5 Principle .4
6 Apparatus .4
7 Reagents .6
8 Sample pretreatment .6
8.1 Sample size .6
8.2 Particle size reduction .6
8.3 Determination of the dry matter content and of water content .7
8.4 Preparation of test portion .7
9 Procedure .8
9.1 Contact time .8
9.2 pH-range .8
9.3 Leaching test .8
9.3.1 General .8
9.3.2 Preparation of leachant .8
9.3.3 Leaching procedure . 10
9.4 Natural pH . 12
10 Eluate treatment, storage and analysis . 12
11 Analytical determination . 12
12 Blank test . 12
13 Calculation. 13
14 Test report . 13
15 Performance characteristics . 13
Annex A (informative) Example of a specific liquid-solid separation procedure for soil
sample . 15
COPYRIGHT PROTECTED DOCUMENT
A.1 Introduction. 15
© ISO 2018
A.2 Apparatus . 15
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
A.3 Procedure . 15
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 Annex B (informative) Operation and uses of the test: influence of pH on the leaching
below or ISO’s member body in the country of the requester.
behaviour. 17
ISO copyright office
B.1 Comparison of the mode of operation of the test with the pH continuous control
CP 401 • Ch. de Blandonnet 8
mode — Influence of pH on the leaching behaviour . 17
CH-1214 Vernier, Geneva, Switzerland
Tel. [phone] B.2 Expression of results . 17
Fax [phone]
B.3 Scope and limits of the application field of the test . 19
[e-mail]
www.iso.org
Published in Switzerland
© ISO 2017 – All rights reserved
iii
ii © ISO 2018 – All rights reserved

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oSIST prEN ISO 21268-4:2018
ISO/DIS 21268-4:2018(E)
Contents Page
Foreword . v
Introduction . vi
1 Scope .1
2 Normative references .1
3 Terms and definitions .2
4 Symbols and abbreviations .3
5 Principle .4
6 Apparatus .4
7 Reagents .6
8 Sample pretreatment .6
8.1 Sample size .6
8.2 Particle size reduction .6
8.3 Determination of the dry matter content and of water content .7
8.4 Preparation of test portion .7
9 Procedure .8
9.1 Contact time .8
9.2 pH-range .8
9.3 Leaching test .8
9.3.1 General .8
9.3.2 Preparation of leachant .8
9.3.3 Leaching procedure . 10
9.4 Natural pH . 12
10 Eluate treatment, storage and analysis . 12
11 Analytical determination . 12
12 Blank test . 12
13 Calculation. 13
14 Test report . 13
15 Performance characteristics . 13
(informative) Example of a specific liquid-solid separation procedure for soil
sample . 15
A.1 Introduction. 15
A.2 Apparatus . 15
A.3 Procedure . 15
(informative) Operation and uses of the test: influence of pH on the leaching
behaviour. 17
B.1 Comparison of the mode of operation of the test with the pH continuous control
mode — Influence of pH on the leaching behaviour . 17
B.2 Expression of results . 17
B.3 Scope and limits of the application field of the test . 19
© ISO 2018 – All rights reserved
iii

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oSIST prEN ISO 21268-4:2018
ISO/DIS 21268-4:2018(E)
B.4 Example: Identification of the sensitivity of leaching to pH over the environmentally
relevant pH range . 19
(informative) Preliminary determination of the acid/base consumption . 21
C.1 General . 21
C.2 Titration procedure to estimate the ANC and the BNC . 21
C.2.1 Reagents . 21
C.2.2 Apparatus . 21
C.2.3 Test portion . 21
C.2.4 Procedure. 21
C.2.5 Expression of results . 23
C.3 Arbitrary division of the maximum acid/base consumption for the extreme pH
values . 23
C.3.1 General . 23
C.3.2 Reagents . 23
C.3.3 Apparatus . 23
C.3.4 Test portion . 23
C.3.5 Procedure. 23
C.3.6 Expression of results . 24
(informative)  Repeatability and reproducibitity data . 26
D.1 Soil sample used in the interlaboratory comparison study . 26
D.2 Interlaboratory comparison results . 26
Bibliography . 1


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iv

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oSIST prEN ISO 21268-4:2018
ISO/DIS 21268-4:2018(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 on 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 the following
URL: www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 190, Soil quality, Subcommittee SC 7, Soil
and site assessment.
This first edition of ISO 21268-4 cancels and replaces ISO/TS 21268-4:2007 which has been technically
revised.
The main changes compared to the previous document are as follows:
 Clause 15 Performance characteristics technically revised;
 Annex D “Repeatability and reproducibility data” has been added.
A list of all parts in the ISO 21268 series can be found on the ISO website.
© ISO 2018 – All rights reserved
v

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oSIST prEN ISO 21268-4:2018
ISO/DIS 21268-4:2018(E)
Introduction
In various countries, tests have been developed to characterize and assess the constituents that can be
released from materials. The release of soluble constituents upon contact with water is regarded as a
main mechanism of release, resulting 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 complexity
of the leaching process makes simplifications necessary.
Not all of the relevant aspects of leaching behaviour can be addressed in one standard.
Tests to characterize the behaviour of materials can generally be divided into three categories (see
References [1], [2] and [4]). 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 defined tests.
b) “Compliance” tests are used to determine whether the material complies with a specific behaviour
or with specific reference values. These tests focus on key variables and leaching behaviour
previously identified by basic characterization 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.
NOTE Up to now, the test procedures described in this part of ISO/TS 21268 have not been validated.
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vi

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oSIST prEN ISO 21268-4:2018
DRAFT INTERNATIONAL STANDARD ISO/DIS 21268-4:2018(E)

Soil quality — Leaching procedures for subsequent chemical
and ecotoxicological testing of soil and soil materials — Part 4:
Influence of pH on leaching with initial acid/base addition
1 Scope
This part of ISO/TS 21268 specifies a test method to obtain information on the short- and long-term
leaching behaviour and characteristic properties of materials.
It applies to the determination of the influence of pH on the leachability of inorganic and organic
constituents from soil and soil material, and the ecotoxicological effects of eluates with respect to
microorganisms, fauna and flora. The test is not suitable for constituents that are volatile under ambient
conditions. The equilibrium condition, as defined in this part of ISO/TS 21268, is established by the
addition of predetermined amounts of acid or base to reach desired final pH values.
The test procedure specified in this part of ISO/TS 21268 produces eluates that are subsequently
characterized by physical, chemical and ecotoxicological standard methods.
For the purposes of ecotoxicological tests, the relevant pH range (see 9.2) will usually be pH 5 to 9.
NOTE 1 Volatile organic constituents include the low molecular weight components in mixtures such as
mineral oil.
NOTE 2 It is not always possible to optimize test conditions simultaneously for inorganic and organic
constituents and optimum test conditions may also vary between different groups of organic constituents. Test
requirements for organic constituents are generally more stringent than those for inorganic constituents. The test
conditions suitable for measuring the release of organic constituents will generally also be applicable to inorganic
constituents.
NOTE 3 For ecotoxicological testing, eluates representing the release of both inorganic and organic
contaminants are needed. In this document, ecotoxicological testing is meant to include genotoxicological testing.
This test cannot be used alone to determine the total leaching behaviour of a soil. More leaching tests
are needed for that extended goal. This part of ISO/TS 21268 does not address issues related to health
and safety. It only determines the leaching properties outlined in Clause 5.
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.
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 5667-3, Water quality — Sampling — Part 3: Guidance on the preservation and handling of water
samples
ISO 7027, Water quality — Determination of turbidity
© ISO 2018 – All rights reserved 1

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oSIST prEN ISO 21268-4:2018
ISO/DIS 21268-4:2018(E)
ISO 10381-1, Soil quality — Sampling — Part 1: Guidance on the design of sampling programmes
ISO 10381-2, Soil quality — Sampling — Part 2: Guidance on sampling techniques
ISO 10381-3, Soil quality — Sampling — Part 3: Guidance on safety
ISO 10381-4, Soil quality — Sampling — Part 4: Guidance on the procedure for investigation of natural,
near-natural and cultivated sites
ISO 10381-5, Soil quality — Sampling — Part 5: Guidance on the procedure for the investigation of urban
and industrial sites with regard to soil contamination
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.
3.1
leaching test
test during which a soil or soil material is put into contact with a leachant under strictly defined
conditions and some constituents of the material are extracted
3.2
leachant
liquid used in a leaching test
3.3
eluate
solution obtained by a laboratory leaching test
3.4
single batch leaching test
leaching test in which a fixed amount of material is leached in one step with a fixed amount of leachant
3.5
liquid to solid ratio
L/S
ratio between the amount of liquid (L) and of solid (S) in the test
Note 1 to entry: L/S is expressed in litres per kilogram (l/kg) of dry matter.
3.6
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
3.7
water content
w
H O
2
ratio, expressed in percent, between the mass of water contained in the material as received and the
corresponding dry residue of the material.
2 © ISO 2018 – All rights reserved

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oSIST prEN ISO 21268-4:2018
ISO/DIS 21268-4:2018(E)
Note 1 to entry: The basis for the calculation of the moisture content is the mass of the dry residue in this part
of ISO/TS 21268, as specified in ISO 11465 (for the determination of the water content of soil).
3.8
laboratory sample
sample or subsample(s) sent to or received by the laboratory
[SOURCE: IUPAC:1997]
3.9
test sample
sample, prepared from the laboratory sample, from which test portions are removed for testing or
analysis
[SOURCE: IUPAC:1997]
3.10
test portion
amount or volume of the test sample taken for analysis, usually of known weight or volume
[SOURCE: IUPAC:1997]
3.11
soil material
soil-like material
excavated soil, dredged materials, manufactured soils, treated soil and fill materials
[SOURCE: ISO 15176:2002, 3.1.4]
4 Symbols and abbreviations
ANC acid neutralization capacity
BNC base neutralization capaci
...