EN ISO 21268-1:2019
(Main)Soil quality - Leaching procedures for subsequent chemical and ecotoxicological testing of soil and soil-like materials - Part 1: Batch test using a liquid to solid ratio of 2 l/kg dry matter (ISO 21268-1:2019)
Soil quality - Leaching procedures for subsequent chemical and ecotoxicological testing of soil and soil-like materials - Part 1: Batch test using a liquid to solid ratio of 2 l/kg dry matter (ISO 21268-1:2019)
This document specifies a test providing information on leaching of soil and soil-like materials under the experimental conditions specified hereafter, and particularly at a liquid to solid ratio of 2 l/kg dry matter.
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].
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 optimise 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.
This 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.
This procedure is not applicable to materials with a dry-matter-content ratio lower than 33 %.
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 as outlined in Clause 4.
Bodenbeschaffenheit - Elutionsverfahren für die anschließende chemische und ökotoxikologische Untersuchung von Boden und von Bodenmaterialien - Teil 1: Schüttelverfahren mit einem Flüssigkeits/Feststoffverhältnis von 2 l/kg Trockenmasse (ISO 21268-1:2019)
Dieses Dokument legt eine Prüfung fest, die Informationen zur Elution von Boden und bodenähnlichen Materialien unter den im Weiteren festgelegten experimentellen Bedingungen und insbesondere bei einem Flüssigkeits /Feststoffverhältnis von 2 l/kg Trockenmasse liefert.
Dieses Dokument wurde erstellt, um die Freisetzung anorganischer und organischer Substanzen aus Boden und bodenähnlichem Material zu untersuchen und um Eluate für nachfolgende ökotoxikologische Unter-suchungen herzustellen. Hinsichtlich der ökotoxikologischen Prüfung siehe ISO 15799 [6] und ISO 17616 [7].
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.
Durch das vorliegende 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.
Dieses Verfahren ist nicht auf Materialien mit einem Trockenmassegehalt von weniger als 33 % anwendbar.
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 Elutionsprüfungen erforderlich. Dieses Dokument befasst sich nicht mit gesundheitlichen und sicherheitstechnischen Belangen. Es dient nur der Bestimmung der in Abschnitt 4 dargestellten Elutionseigenschaften.
Qualité du sol - Modes opératoires de lixiviation en vue d'essais chimiques et écotoxicologiques ultérieurs des sols et matériaux analogues au sol - Partie 1: Essai en bâchée avec un rapport liquide/solide de 2 l/kg de matière sèche (ISO 21268-1:2019)
Le présent document spécifie un essai fournissant des informations sur la lixiviation des sols et des matériaux analogues au sol dans les conditions expérimentales spécifiées ci-après, et notamment pour un rapport liquide/solide égal à 2 l/kg de matière sèche.
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].
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, et les conditions d'essai optimales peuvent également varier entre 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.
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.
Ce mode opératoire ne s'applique pas aux matériaux ayant un taux de matière sèche inférieur à 33 %.
Cet essai est principalement destiné à être utilisé à des fins de vérification de routine et de contrôle, et il ne peut pas, à lui seul, être utilisé pour déterminer 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 questions liées à la santé et à la sécurité. Il permet uniquement de déterminer les propriétés de lixiviation telles que décrites dans l'Article 4.
Kakovost tal - Postopki izluževanja za nadaljnje kemijsko in ekotoksikološko preskušanje tal in tlem podobnih materialov - 1. del: Šaržni preskus z razmerjem tekoče/trdno 2 l/kg suhe snovi (ISO 21268-1:2019)
Ta standard določa preskus, ki zagotavlja informacije o izluževanju prsti in prsti podobnih materialov v eksperimentalnih pogojih, določenih v nadaljevanju, zlasti pri razmerju tekoče/trdno za 2 l/kg suhe snovi. 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 ISO 15799[6] in ISO 17616.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
01-januar-2020
Nadomešča:
SIST-TS CEN ISO/TS 21268-1:2010
Kakovost tal - Postopki izluževanja za nadaljnje kemijsko in ekotoksikološko
preskušanje tal in tlem podobnih materialov - 1. del: Šaržni preskus z razmerjem
tekoče/trdno 2 l/kg suhe snovi (ISO 21268-1:2019)
Soil quality - Leaching procedures for subsequent chemical and ecotoxicological testing
of soil and soil-like materials - Part 1: Batch test using a liquid to solid ratio of 2 l/kg dry
matter (ISO 21268-1:2019)
Bodenbeschaffenheit - Elutionsverfahren für die anschließende chemische und
ökotoxikologische Untersuchung von Boden und von Bodenmaterialien - Teil 1:
Schüttelverfahren mit einem Flüssigkeits/Feststoffverhältnis von 2 l/kg Trockenmasse
(ISO 21268-1:2019)
Qualité du sol - Modes opératoires de lixiviation en vue d'essais chimiques et
écotoxicologiques ultérieurs des sols et matériaux analogues au sol - Partie 1: Essai en
bâchée avec un rapport liquide/solide de 2 l/kg de matière sèche (ISO 21268-1:2019)
Ta slovenski standard je istoveten z: EN ISO 21268-1:2019
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 21268-1
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2019
EUROPÄISCHE NORM
ICS 13.080.05 Supersedes CEN ISO/TS 21268-1:2009
English Version
Soil quality - Leaching procedures for subsequent chemical
and ecotoxicological testing of soil and soil-like materials -
Part 1: Batch test using a liquid to solid ratio of 2 l/kg dry
matter (ISO 21268-1:2019)
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 1: Essai en Untersuchung von Boden und von Bodenmaterialien -
bâchée avec un rapport liquide/solide de 2 l/kg de Teil 1: Schüttelverfahren mit einem
matière sèche (ISO 21268-1:2019) Flüssigkeits/Feststoffverhältnis von 2 l/kg
Trockenmasse (ISO 21268-1:2019)
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 21268-1:2019 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
European foreword
This document (EN ISO 21268-1:2019) 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 21268-1:2009.
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 21268-1:2019 has been approved by CEN as EN ISO 21268-1:2019 without any
modification.
INTERNATIONAL ISO
STANDARD 21268-1
First edition
2019-09
Soil quality — Leaching procedures
for subsequent chemical and
ecotoxicological testing of soil and
soil-like materials —
Part 1:
Batch test using a liquid to solid ratio
of 2 l/kg dry matter
Qualité du sol — Modes opératoires de lixiviation en vue d'essais
chimiques et écotoxicologiques ultérieurs des sols et matériaux
analogues au sol —
Partie 1: Essai en bâchée avec un rapport liquide/solide de 2 l/kg de
matière sèche
Reference number
ISO 21268-1:2019(E)
©
ISO 2019
ISO 21268-1:2019(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
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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 21268-1:2019(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Principle . 3
5 Reagents . 3
6 Apparatus . 4
7 Sample pretreatment . 5
7.1 Preparation of laboratory sample and specification of particle size . 5
7.2 Preparation of test sample . 6
7.3 Determination of dry matter content and water content . 6
7.4 Preparation of the test portion . 7
8 Procedure. 7
8.1 Temperature . 7
8.2 Description of the procedure . 7
8.2.1 Preparation of the eluent . 7
8.2.2 Leaching step . 7
8.2.3 Liquid/Solid separation step . 8
8.3 Further preparation of the eluate for analysis. 9
8.4 Blank test for the application of the leaching procedure . 9
9 Calculation .10
10 Test report .10
11 Analytical determination .11
11.1 General .11
11.2 Blank test information .11
12 Performance characteristics .11
12.1 General .11
12.2 Validation results obtained for DIN 19529 .11
12.2.1 General.11
12.2.2 Results for test material containing inorganic substances .12
12.2.3 Results for test materials containing organic substances .12
Annex A (informative) Information on the influence on the test results of the parameters
that affect leaching .20
Annex B (informative) Example of a specific liquid-solid separation procedure for soil
samples (applying only to the leaching of inorganic substances) .23
Annex C (informative) Calculation of centrifugation duration depending on centrifugation
speed and rotor dimensions.25
Bibliography .27
ISO 21268-1:2019(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 21268-1:2019 cancels and replaces the first edition (ISO/TS 21268-1:2007),
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;
— the demineralized water has been added as possible leachant;
— 7.1 and 7.2 have been renumbered and renamed to read 7.1 "Particle size" and 7.2 "Sample
preparation";
— 12.1 "General" and 12.2 "Validation results obtained for DIN 19529" have been added;
— A.3.6 "Special requirements for tests considering semi-volatile substances" has been added;
— a new informative Annex C "Calculation of centrifugation duration depending on centrifugation
speed and rotor dimensions" has been added;
— references in Clause 2 and the Bibliography have 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 21268-1:2019(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 characterize 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 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.
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 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 b): compliance tests.
[4]
This document was originally elaborated on the basis of EN 12457-1:2004 . Especially, modifications
considering requirements on subsequent ecotoxicological testing and analysis of organic substances
[5]
have been included. Validation results have been adopted from DIN 19529 .
INTERNATIONAL STANDARD ISO 21268-1:2019(E)
Soil quality — Leaching procedures for subsequent
chemical and ecotoxicological testing of soil and soil-like
materials —
Part 1:
Batch test using a liquid to solid ratio of 2 l/kg dry matter
1 Scope
This document specifies a test providing information on leaching of soil and soil-like materials under the
experimental conditions specified hereafter, and particularly at a liquid to solid ratio of 2 l/kg dry matter.
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
[6] [7]
ecotoxicological testing, see ISO 15799 and ISO 17616 .
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 optimise 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.
This 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.
This procedure is not applicable to materials with a dry-matter-content ratio lower than 33 %.
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 as outlined in Clause 4.
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 21268-1:2019(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 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.
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
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
ISO 21268-1:2019(E)
3.7
laboratory sample
sample or sub-sample(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 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 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 solid residue is subsequently separated from the liquid. The separation procedure
may strongly influence the test results and shall be particularly stringent for organic substances. 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 imposed by the material, in terms of pH, electrical conductivity
and, optionally, DOC, redox potential or turbidity, shall be recorded.
NOTE 1 These parameters often control the leaching behaviour of soil and soil-like 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.
The procedure described in this document is based on the more stringent test requirements for
determining the release of organic substances and for subsequent ecotoxicological testing. If only the
release of inorganic substances is to be measured, less stringent requirements may be adopted for some
steps of the procedure.
5 Reagents
5.1 Demineralised water or deionised 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 .
5.2 Calcium chloride (CaCl · 2 H O), analytical grade.
2 2
5.3 Sodium azide (NaN ), analytical grade.
ISO 21268-1:2019(E)
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 Borosilicate glass, of high purity in accordance with ISO 5667-3, with a nominal volume of 1 l,
glass bottles having caps of inert material, for example PTFE (polytetrafluoroethylene). Rinsing is
compulsory, and it should be assured that previously used bottles have no background level of analytes.
NOTE 1 If only inorganic parameters are analysed, alternative materials, such as HDPE/PP bottles, are
appropriate, except for unpreserved samples for mercury analysis.
NOTE 2 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.
If boron analyses are necessary, any plastics bottles can be used, e.g. PTFE (polytetrafluoroethylene).
The volume of 1 l is selected in combination with the mass, m , of 350 g as specified in 7.4 in order
D
to minimize headspace in the bottle at an L/S of 2 l/kg dry matter. In the case of materials with low
density, deviation from this requirement can be necessary while still ensuring minimum headspace.
This deviation shall be reported.
NOTE 3 Glass of high quality is considered adequate for both metals 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 can be partially dissolved. For ecotoxicity testing, eluates with both inorganic and organic substances are
needed, which emphasizes the need to generate integrated eluates.
NOTE 4 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 substances from the air.
6.2 Glass bottle, of high quality (requirements as in 6.1) with a nominal volume of e.g. 5 l, to be used
when samples from replicate tests are recombined after centrifugation for further analysis or testing.
−1 −1 −1
6.3 End-over-end tumbler (5 min to 10 min ) or roller table, rotating at about 10 min . Other
shaking devices may be used provided that they can be shown to provide equivalent results. These
agitation devices are specified because excessive abrasion leading to significant particle size reduction
should be avoided.
6.4 Filtration apparatus, either a vacuum filtration device (between 2,5 kPa and 4,0 kPa) or a
high-pressure filtration apparatus (<0,5 MPa). Rinsing is compulsory. When semi-volatile substances are
to be analysed, vacuum filtration shall not be used.
6.5 0,45 µm membrane filters, pre-rinsed or similarly cleaned [e.g. rinsed with 0,1 mol/l HNO (5.2)
and water (5.1)] (only for analysis of inorganic substances).
The filters shall be chosen so as not to adsorb (or release) substances of interest.
NOTE This can be tested in preliminary experiments.
6.6 Glass fibre filters, with a degree of separation of 0,7 µm
The filters shall be chosen so as not to adsorb (or release) substances of interest.
NOTE This can be tested in preliminary experiments.
6.7 Sieving equipment, with sieves of 2 mm nominal screen size.
4 © ISO 2019 – All rights reserved
ISO 21268-1:2019(E)
NOTE Due to sieving, contamination of the sample can occur to an extent which affects the leaching of some
substances of concern, e.g. chromium, nickel and molybdenum from stainless steel equipment or plasticisers
from plastic sieves.
6.8 Centrifuge, operating at 20 000 g to 30 000 g using centrifuge tubes of PFA (perfluoroalkoxy
alkane), FEP (fluorinated ethylene propylene) or tubes of an alternative material which is inert with
[8]
regard to both inorganic and organic compounds and suitable for high-speed centrifugation .
NOTE Potential sorption of hydrophobic organic substances to the centrifuge tubes can be tested in
preliminary experiments.
Alternatively, if a high-speed centrifuge is not available, a centrifuge operating at 2 000 g to 3 000 g
using glass bottles may be used in combination with increased centrifugation time. Cooling shall be
applied to maintain the desired temperature.
6.9 Device for measuring electrical conductivity.
6.10 pH meter, in accordance with ISO 10523 with an accuracy of at least ±0,05 pH units.
6.11 Thermometer, for air temperature measurement.
6.12 Redox potential meter, (optional).
6.13 Balance, with an accuracy of at least 0,1 g.
6.14 Measuring cylinders, for volume determination with 1 % accuracy.
6.15 Sample splitter, for sub-sampling of laboratory samples (optional).
6.16 Turbidity meter, as specified in ISO 7027-1.
6.17 Crushing equipment, a jaw crusher.
NOTE Due to particle size reduction, contamination of the sample can occur to an extent which affects the
leaching of some substances of concern, e.g. chromium, nickel and molybdenum from stainless steel equipment.
7 Sample pretreatment
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.
ISO 21268-1:2019(E)
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.
7.2 Preparation of test sample
Use a sample splitter (6.15) 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 Determination of dry matter content and water 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
dm
as well. This shall be taken into account when adjusting the L/S. 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
The water content ( w in %) is calculated following Formula (2):
HO
wm=×100 −mm/ (2)
HO ()
2W DD
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.
6 © ISO 2019 – All rights reserved
ISO 21268-1:2019(E)
7.4 Preparation of the test portion
Prepare, from the test sample, a test portion with a total mass m containing (350 ± 5) g [measured with
an accuracy of 0,1 g (6.13)] of dry mass (m ) following Formula (3).
D
mm=×100 /w (3)
Ddm
Use a sample splitter (6.15) or apply coning and quartering to split the sample.
NOTE Sample splitting or coning-and-quartering can lead to loss of semi-volatile substances (inorganic and
organic).
In view of the minimum requirements of eluate volume for analytical purposes, it may be necessary
to use a larger test portion and a correspondingly larger volume of leachant. This deviation from this
document shall be specified in the test report.
If the test is performed on an air-dried sample, use w instead of w to determine the sample mass
dm,AD dm
of the test portion.
8 Procedure
8.1 Temperature
The compliance test for leaching shall be carried out at room temperature: (22 ± 3) °C.
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 Description of the procedure
8.2.1 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.
8.2.2 Leaching step
Place the test portion with the total mass m corresponding to (350 ± 5) g of dry mass m in a bottle (6.1).
D
Depending on the particle size distribution, other test portions may be applied ensuring that a
representative portion is used (see 7.1).
ISO 21268-1:2019(E)
Add an amount of leachant (V ) using a balance (6.13) or measuring cylinder (6.14), to establish a liquid
L
to solid ratio (L/S) of (2 ± 0,04) l/kg during the extraction, following Formula (4). Care shall be taken to
obtain good mixing of solid and liquid.
Vw=−2 / ρ ×100 ×m (4)
()
LH OH OD
where
V is the volume of leachant used (l);
L
m is the dry mass of the test portion (kg);
D
is the density of water (usually taken as 1 kg/l);
ρ
HO
is the water content for the test portion (%).
w
HO
Place the capped bottle in an agitation device (6.3). Agitate for (24 ± 0,5) h.
As an alternative, instead of 24 h, 6 h can be adopted when it can be demonstrated that equilibrium or
semi-equilibrium is reached or a quick turn-around time is required for quality control purposes. In
this case, it shall be recorded that the leaching was carried out for 6 h.
Settling of solids in the bottle during agitation shall be avoided. At the end of the agitation period, the
bottle is removed from the agitation device.
8.2.3 Liquid/Solid separation step
Allow the suspended solids to settle for (15 ± 5) min.
Transfer the supernatant to centrifuge tubes (6.8). The centrifugation containers shall be chosen so as
not to adsorb (or release) analytes.
There are two options for centrifugation:
a) Centrifuge the eluate for 30 min at 20 000 g to 30 000 g using a high-speed centrifuge (6.8, see also
Annex C).
b) Centrifuge the eluate for 5 h at 2 000 g to 3 000 g in glass bottles using a lower-speed centrifuge (6.8).
Cooling shall be applied to maintain the temperature at (22 ± 3) °C (see 8.1).
NOTE 1 Based on Stoke's law, the results of both centrifugation methods are expected to be comparable. Other
alternative combinations of centrifugation acceleration and time can be applied given comparable conditions are
calculated related to the specification of the rotor (see guidance in Annex C).
Gentle braking of the centrifuge shall be applied in order to avoid resuspension. The deceleration time
shall not exceed 20 min.
NOTE 2 In case lightweight substances (e.g. coaly particles) are still floating after centrifugation, a glass fibre
filtration (6.6) can be applied to remove such particles or to reduce the turbidity.
After centrifugation, the eluate shall be transferred immediately to an appropriate container for
measurement of pH and redox potential (see also the next-to-last paragraph of 8.2.2) and stored for
subsequent chemical analysis and/or ecotoxicological testing. In general, this eluate can be used for
both analyses of inorganic and organic substances.
If only inorganic substances are measured, the centrifugation step can be omitted, and the decanted
eluate can be filtered directly using the appropriate membrane filters (6.5) and a vacuum or pressure
filtration device (6.4), (see Annex B for an example). When this filtration as specified is not possible in
less than 1 h with a liquid flow rate of at least 30 ml/cm /h, a liquid-solid separation procedure, specific
8 © ISO 2019 – All rights reserved
ISO 21268-1:2019(E)
for the considered case, shall be applied. Report the details in the test report. This specific procedure
shall not include the use of additives.
NOTE 3 For inorganic substances, it is often preferable to pre-centrifuge the eluate at 2 000 g to 3 000 g for
20 min before filtration using glass bottles with a screw cap and polytetrafluoroethylene inlay (or, if possible,
using the leaching bottle directly) prior to filtration. Higher speed or longer time can also be applied (see
Annex C).
NOTE 4 Such a specific liquid-solid separation procedure can include settling, pre-filtration on a coarser filter,
centrifugation, filtration on a large-size membrane filter, filtration at high pressure, filtration at increasing high
pressure following a first period without pressure, etc.
NOTE 5 An example of a
...
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