EN 17516:2023

SLOVENSKI STANDARD
01-junij-2024
Odpadki - Karakterizacija granuliranih trdnih snovi (granulatov), ki se lahko
uporabljajo kot gradbeni material - Preskus skladnosti izluževanja - Preskus
precejanja v koloni s tokom navzgor
Waste - Characterization of granular solids with potential for use as construction material
- Compliance leaching test - Up-flow percolation test
Abfall - Charakterisierung von granularen Feststoffen mit Verwertungspotential als
Ersatzbaustoff - Übereinstimmungsuntersuchung des Elutionsverhaltens -
Perkolationsprüfung im Aufwärtsstrom
Déchets - Caractérisation des solides granulaires présentant un intérêt potentiel comme
matériaux de construction - Essai de conformité par lixiviation - Essai de percolation à
écoulement ascendant
Ta slovenski standard je istoveten z: EN 17516:2023
ICS:
13.030.10 Trdni odpadki Solid wastes
91.100.01 Gradbeni materiali na Construction materials in
splošno general
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN 17516
EUROPEAN STANDARD
NORME EUROPÉENNE
November 2023
EUROPÄISCHE NORM
ICS 91.100.01
English Version
Waste - Characterization of granular solids with potential
for use as construction material - Compliance leaching test
- Up-flow percolation test
Déchets - Caractérisation des solides granulaires Abfall - Charakterisierung von granularen Feststoffen
présentant un intérêt potentiel comme matériaux de mit Verwertungspotential als Ersatzbaustoff -
construction - Essai de conformité par lixiviation - Übereinstimmungsuntersuchung des
Essai de percolation à écoulement ascendant Elutionsverhaltens - Perkolationsprüfung im
Aufwärtsstrom
This European Standard was approved by CEN on 30 July 2023.

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, Türkiye 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
© 2023 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN 17516:2023 E
worldwide for CEN national Members.

Contents Page
European foreword . 4
Introduction . 5
1 Scope . 6
2 Normative references . 7
3 Terms and definitions . 7
4 Symbols and abbreviations . 10
4.1 Symbols . 10
4.2 Abbreviations . 11
5 Principle . 12
5.1 General principles . 12
5.2 Number of eluates . 12
6 Reagents . 13
7 Equipment . 13
8 Sample preparation . 15
8.1 General. 15
8.2 Preparation of the test sample . 15
8.2.1 Principles . 15
8.2.2 Rules of application . 16
8.3 Test portion . 17
8.4 Drying . 17
8.5 Subsampling . 17
8.6 Sieving of samples into fractions . 17
8.7 Size reduction of particles . 18
9 Test procedure . 18
9.1 Temperature. 18
9.2 Determination of dry residue . 18
9.3 Pre-treatment of the column . 18
9.4 Packing of the column . 19
9.4.1 General. 19
9.4.2 Equilibration. 19
9.4.3 Calculation of the flow rate . 19
9.5 Collection of eluates . 19
9.6 Further preparation of the eluates for analysis . 22
9.7 Blank test . 22
10 Evaluation of measurement results . 23
10.1 Expression of results in concentrations . 23
10.2 Expression of results in terms of mass related release . 23
11 Documentation and test report . 24
12 Test performance . 25
Annex A (informative) A–deviations . 26
Annex B (informative) Examples of sample preparation procedures . 27
B.1 General . 27
B.2 Example 1 . 27
B.3 Example 2 . 27
Annex C (informative) Illustration of the column and accompanying equipment. 30
Annex D (informative) Procedures for packing and saturation of the column . 31
D.1 General . 31
D.2 Column filling and packing . 31
D.3 Procedure for packing . 31
D.4 Water saturation . 32
Annex E (informative) Assessment of release mechanism(s) . 34
E.1 Overview of release mechanisms . 34
E.2 Overview of release mechanisms . 35
E.3 Overview of release mechanisms . 40
E.4 Examples . 41
Annex F (informative) Summary of cumulative results for L/S = 2 and L/S = 10 . 54
F.1 Performance data EN 16637-3 for L/S = 2 and L/S = 10 . 54
F.2 Inorganic substances . 57
F.3 Organic substances . 65
Bibliography . 71

European foreword
This document (EN 17516:2023) has been prepared by Technical Committee CEN/TC 444
“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 May 2024 and conflicting national standards shall be
withdrawn at the latest by May 2024.
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 has been prepared under a standardization request addressed to CEN by the European
Commission. The Standing Committee of the EFTA States subsequently approves these requests for its
Member States.
This document specifies an up-flow percolation test to determine the compliance leaching status of
granular solid waste with potential for beneficial use as construction product under standardized
percolation conditions. The test is equal to the Horizontal up-flow percolation test for construction
products (EN 16637-3), which in turn was elaborated based on the up-flow percolation test for
characterization of waste (CEN/TS 14405:2004). Modifications have been implemented based on
intensive robustness validation work on EN 16637-3 [4], [22]. The reason for implementing this
percolation test is to provide a means to avoid double testing of waste-derived aggregates that could
have a potential as construction products.
NOTE Waste legislation generally prescribes the use of EN 14405 to describe the leaching behaviour of
inorganic and non-volatile organic substances from granular waste materials, whereas construction products
legislation generally prescribes the use of EN 16637-3 to describe the leaching behaviour of inorganic and non-
volatile organic substances from construction products, including waste materials with a potential as construction
products.
Background information on characterization of leaching behaviour of construction products can be
found in Technical Reports provided by CEN/TC 351 (i.e. CEN/TR 16098).
Any feedback and questions on this document should be directed to the users’ national standards body.
A complete listing of these bodies can be found on the CEN website.
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, Türkiye and the United
Kingdom.
Introduction
The implementation of a Circular Economy has a high priority on the agenda of the European
Commission. To fulfil the needs of a Circular Economy granular solid waste should be used as
construction product as much as possible, thus diminishing the amount of landfilling to a minimum and
save natural resources.
The release of dangerous substances upon contact with water results in a potential risk to the
environment during the intended utilization of waste materials as construction products. The intent of
this document together with EN 14405 or the EN 12457 series is to identify the leaching behaviour of
granular solid waste with potential for beneficial use as construction product and thereby allow
assessments of the release of regulated dangerous substances to soil, surface water and groundwater
under intended use conditions in relation to CE marking of construction products derived from waste.
This document describes an up-flow percolation test for granular solid waste with potential for
beneficial use as a construction product. It has been elaborated to avoid double testing, i.e. to assess the
compliance with both waste and construction products regulations in one run. This test addresses
granular solid waste with existing knowledge on long-term leaching behaviour in waste management
scenarios obtained i.e. using basic characterization test EN 14405. The specified methods under
Clauses 5 to 12 (Principle, Reagents, Equipment, Sample preparation, Test procedure, Evaluation of
measurement results, Documentation and Test Report as well as Test Performance) are identical to the
corresponding clauses of EN 16637-3 (Horizontal up-flow percolation test) with the exception that the
term “construction product“ has been changed to terms relevant for this standard such as “granular
solid waste with potential to be reused as construction product” or similar.
In the different European countries, tests have been developed to characterize and assess dangerous
substances which can be leached from solid matrices (e.g. construction products, contaminated soils,
solid waste materials). The intent of these tests is to identify the leaching behaviour of these materials.
The complexity of the leaching process makes simplifications necessary. All relevant aspects of leaching
behaviour cannot be addressed in one single standard. The test hierarchy for waste is e.g. described in
EN 14405, while guidance of appropriate leaching test for determining leaching of dangerous
substances from construction products is specified in EN 16637-1.
The test procedure described in this document constitutes a compliance test used to verify compliance
to regulatory limit values. Column percolation tests according to EN 14405 is applied for basic
characterization of granular solid waste. Column percolation tests according to EN 16637-3 is applied
for basic characterization of construction products.
Basic characterization constitutes a full characterization of the waste by gathering all the necessary
information for a safe management of the waste in the short and long term. Basic characterization may
provide general information on the waste (i.e. type and origin, composition, consistency, leachability,
etc.), information for understanding the behaviour of waste in the considered management scenario,
comparison of waste properties against limit values, and detection of key variables (critical parameters
as liquid/solid (L/S) ratios, leachant composition, factors controlling leachability such as pH, redox
potential, complexing capacity and physical parameters) for compliance testing and options for
simplification of compliance testing. Compliance testing is used to demonstrate that the sample of today
fits the population of samples tested before by basic characterization and through that is used to carry
out compliance with regulatory limit values. The compliance test should therefore always be part of the
basic characterization program. The compliance test focuses on key variables and leaching behaviour
identified by basic characterization tests. Parts of basic characterization tests can also be used for
compliance purposes.
Informative Annex A (A-Deviation) is an integral part of this document.

1 Scope
This document specifies an up-flow percolation test (PT) which is applicable in compliance testing to
determine the leaching behaviour of inorganic and non-volatile organic substances from granular solids
with potential for use as construction material. The test is not suitable for substances that are volatile
under ambient conditions. The granular solids are subjected to percolation with water as a function of
liquid to solid ratio under specified percolation conditions. The method is a once-through column
leaching test.
NOTE 1 Volatile organic substances include the low molecular weight substances in mixtures such as mineral
oil.
This up-flow percolation test is performed under specified test conditions for granular solids with
potential for use as construction material and does not necessarily produce results that mimic specific
intended use conditions. This test method produces eluates, which can subsequently be characterized
by physical, chemical and ecotoxicological methods according to existing standard methods. The results
of eluate analysis are presented as a function of the liquid/solid ratio. The test results enable the
distinction between different leaching behaviour.
NOTE 2 It is not always possible to adjust test conditions simultaneously for inorganic and organic substances.
Test conditions can also vary between different groups of organic substances. Test conditions for organic
substances are generally more stringent than those for inorganic substances. The test conditions are generally
described in a way that they fit testing organic substances and are also applicable to inorganic substances
depending on the set-up.
NOTE 3 For ecotoxicity testing, eluates representing the release of both inorganic and organic substances are
needed. In this document, ecotoxicological testing is meant to include also genotoxicological testing.
NOTE 4 Granular solid waste materials with a low hydraulic conductivity that can cause detrimental pressure
build-up are not supposed to be subjected to this test.
NOTE 5 This procedure is generally not applicable to solids that are easily biologically degradable and solids
reacting with the leachant, leading to, for example, excessive gas emission or excessive heat release, impermeable
hydraulically bound solids or solids that swell in contact with water.
Granular solid waste materials without potential for beneficial use are excluded from the scope.
NOTE 6 Granular solid waste materials without potential for beneficial use can be materials with gas generation
or biodegradation during a potential reuse scenario.
This test is applicable to types of granular solid waste of which the general long-term leaching behaviour
is known based on previous investigations.
In this document the same test conditions as for EN 16637-3 (CEN/TC 351/WG 1) are applied in order
to allow full comparability of testing construction products and waste derived construction products to
avoid double testing. The EN 16637-3 test results are eligible in the context of testing granular solids
with potential for use as construction material as well.
NOTE 7 If a leaching test according to EN 16637-3 has been performed, additional EN 17516 testing does not
need to be carried out.
NOTE 8 The relative standard deviations for inorganic and organic substances are relatively high which is due
to low concentration levels in the eluates (see Annex F).
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.
CEN/TR 15310 (all parts), Characterization of waste — Sampling of waste materials
EN 933-1, Tests for geometrical properties of aggregates — Part 1: Determination of particle size
distribution — Sieving method
EN 14405, Characterization of waste — Leaching behaviour tests — Up-flow percolation test (under
specified conditions)
EN 15002, Characterization of waste — Preparation of test portions from the laboratory sample
EN 15934, Sludge, treated biowaste, soil and waste — Calculation of dry matter fraction after
determination of dry residue or water content
EN 16637-1, Construction products: Assessment of release of dangerous substances — Part 1: Guidance for
the determination of leaching tests and additional testing steps
EN 16637-3, Construction products: Assessment of release of dangerous substances — Part 3: Horizontal
up-flow percolation test
EN ISO 5667-3, Water quality — Sampling — Part 3: Preservation and handling of water samples
(ISO 5667-3)
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— IEC Electropedia: available at https://www.electropedia.org/
— ISO Online browsing platform: available at https://www.iso.org/obp/
3.1
eluate
solution obtained from a leaching test
[SOURCE: EN 16687:2023, 3.3.2.8, modified – Note 1 to entry deleted]
3.2
granular solid waste
waste composed of solid particles with a particle size smaller than a specified size or grading
3.3
laboratory sample
sample or sub-sample(s) sent to or received by the laboratory
Note 1 to entry: When the laboratory sample is further prepared by subdividing, cutting, sawing, coring, drying,
grinding, mixing, curing or by combinations of these operations, the result is the test sample. When no preparation
of the laboratory sample is required, the laboratory sample is the test sample. A test portion is removed from the
test sample for the performance of the test/analysis.
Note 2 to entry: The laboratory sample is the final sample from the point of view of sample collection but it is the
initial sample from the point of view of the laboratory.
[SOURCE: EN 16687:2023, 3.2.2.1]
3.4
leachant
liquid that is brought into contact with the test portion in the leaching procedure
Note 1 to entry: Usually, demineralized water is used as leachant for laboratory leaching tests.
[SOURCE: EN 16687:2023, 3.3.2.7]
3.5
leaching behaviour
release and change with time in release from a granular solid waste in contact with a leachant as a
function of major release controlling factors
Note 1 to entry: Such factors are diffusion, pH, L/S ratio or time.
[SOURCE: EN 16687:2023, 3.3.2.11, modified to refer to granular waste]
3.6
liquid to solid ratio
L/S
ratio between the total volume of liquid (L) percolated through the granular solid waste and of granular
solid waste (S) packed into the column
Note 1 to entry: L/S is expressed in l/kg dry matter.
[SOURCE: EN 16687:2023, 3.3.2.15, modified to refer to granular waste]
3.7
local equilibrium
LE
situation where chemical equilibrium exists between a substance in solution and the same substance in
the solid phase at any point in the column
Note 1 to entry: Even when local equilibrium exists at all points along the column the equilibrium concentrations
may be different at different points.
[SOURCE: EN 16687:2023, 3.3.2.16]
3.8
percolation test
PT
column test
release test method to determine the release of substances from a granular solid waste packed in a
column with a leachant percolating through it
[SOURCE: EN 16687:2023, 3.3.2.5, modified to refer to granular waste]
3.9
release
emission
liberation of chemical substances (e.g. non-volatile organic compounds, heavy metals, salts) from a
granular solid waste into soil, surface water or groundwater into the leachant of a test facility
Note 1 to entry: Release to soil, surface and groundwater is expressed in terms of mass related release (e.g.
mg/kg).
Note 2 to entry: The terms “emission” and “release” have fundamentally the same meaning. However, it is often a
tradition to use the term “emission” when describing liberation of chemical substances or radiation into air and to
use the term “release” when describing the liberation of chemical substances into soil or water.
[SOURCE: EN 16687:2023, 3.3.2.17, modified to refer to granular waste and mass related release]
3.10
release mechanism
physical-chemical processes that control the release of substances from a granular solid waste into a
leachant
Note 1 to entry: In case of granular solid waste the main release mechanisms are washout and solubility control.
Diffusion and additional factors like pH or DOC also have influence on the mechanism of the release.
Note 2 to entry: The release mechanism for every substance can be determined using the results of the release
test (tank leaching test, percolation test). Determination of the release mechanism is relevant for modelling of the
source term and so for determination of the effects on soil and water over a time period.
[SOURCE: EN 16687:2023, 3.3.2.19, modified – Notes edited to refer to percolation only and to refer to
granular waste]
3.11
sample
portion of material selected from a larger quantity of material
Note 1 to entry: The manner of selection of the sample should be prescribed in a sampling plan (3.12).
Note 2 to entry: The term “sample” is often accompanied by a prefix (e.g. laboratory sample, test sample)
specifying the type of sample and/or the specific step in the sampling process to which the obtained material
relates.
[SOURCE: EN 16687:2023, 3.2.1.5]
3.12
sampling plan
predetermined procedure for the selection, withdrawal, on-site pre-treatment, preservation and
transportation of samples to be removed from a population
[SOURCE: EN 16687:2023, 3.2.1.6, modified to remove “if necessary” for waste]
3.13
test portion
analytical portion
amount of the test sample taken for testing/analysis purposes, usually of known weight or volume
[SOURCE: EN 16687:2023, 3.2.2.3, modified to “weight” for waste and examples deleted]
3.14
test sample
sample, prepared from the laboratory sample, from which test portions are removed for testing or for
analysis
[SOURCE: EN 16687:2023, 3.2.2.2]
3.15
limit of quantification
LOQ
lowest value of an analyte (determinant) that can be determined with an acceptable level of accuracy
and precision, generally determined as three times the limit of detection of the method
[SOURCE: EN 16687:2023, 3.3.1.14]
4 Symbols and abbreviations
4.1 Symbols
For the purposes of this document, the following symbols apply.
c concentration of the substance concerned in the eluate fraction i, in µg/l;
i
D sieve diameter, in mm;
max
NOTE Common sizes are 31,5 mm, 45 mm or 63 mm.
d inner diameter of the column, in mm;
i
d
is the density of the solid, expressed in kilograms per cubic metre (kg/m ).
p
E released quantity of a substance per quantity of sample for analysis in eluate fraction i, in
i
mg/kg dry matter;
h is the height or layer thickness of the construction, in m;
k constant that represents the speed of the release of a certain substance;
c
k number of eluates collected in the test;
e
m dry mass of the test portion, in g;
d
m mass of the undried test portion, in g;
r
m mass of the (moist) test portion in the column, in g;
W
S sieve diameter for test sample preparation (crushing) to reduce the amount of oversized
cs
part of the sample to fit the inner column diameter, in mm;
t execution time of the test, in days;
U measured cumulative release of a substance for cumulative L/S ratio n including fraction
n
i = 1 to n, in mg/kg dry matter;
V volume of the eluate fraction i, in l;
i
V linear velocity of the leachant through the empty column, in mm per day;
L
w dry residue of the granular solid waste, in %;
dr
Φ leachant flow rate, in ml per hour.
4.2 Abbreviations
For the purposes of this document, the following abbreviations apply.
DL detection limit;
DOC dissolved organic carbon;
EC electrical conductivity;
EOTA European organization for technical assessment;
ETA European technical assessment;
ETFE ethylene tetrafluoroethylene;
FEP fluorinated ethylene propylene;
FPC factory production control;
GLHC test method for granular products with low hydraulic conductivity;
HDPE high-density polyethylene;
hEN harmonized European Standard;
PAH polycyclic aromatic hydrocarbon;
PCTFE polychlorotrifluoroethylene;
PT percolation test;
PTFE polytetrafluorethylene;
RDS regulated dangerous substances;
TPH total petroleum hydrocarbons.
5 Principle
5.1 General principles
The percolation test described in this document starts with the representative laboratory sample. The
methodology for the collection of a representative laboratory sample is in accordance with the
procedures described in EN 17087 and EN 15002 considering guidance given in EN 16637-1.
This document describes a method to determine the release of substances from a granular solid waste
with potential for beneficial use as construction product, with or without size reduction to a maximum
particle size, packed in a column with a leachant percolating through it. Pre-equilibration is applied to
approach (local) equilibrium at the start. The column size is related to the amount of eluate needed for
subsequent analysis and testing and the size of the largest particles in the test portion. A continuous
vertical up-flow is used, so that the column is water saturated. The test conditions, including the flow
rate of the leachant, enable a conclusion to be drawn from the results as to which substances are rapidly
being washed out and which substances are released under the influence of interaction with the matrix.
The method is a once-through column leaching test. It is assumed that conditions approach local
equilibrium between the granular solid waste and leachant (for inorganic substances) in the test.
NOTE The results obtained under local equilibrium (LE) can be up-scaled and used in the modelling of in-use
conditions for various scenarios.
The eluate is collected in fractions that are characterized physically and chemically and possibly
ecotoxicologically according to existing standards. The results of the test are expressed as a function of
the L/S ratio, in terms of mg of the substances released cumulatively per kg of granular solid waste or
of mg of substance determined per litre of eluate.
The procedure described in this document is based on the more stringent test requirements for
determining the release of organic substances and/or for subsequent ecotoxicological testing. If only the
release of inorganic substances is to be measured, requirements on equipment (e.g. column and tubing
material, centrifugation) are specified in the relevant clauses for some steps of the procedure.
The test procedure described in this document constitutes a compliance test used to verify compliance
to regulatory limit values. The column percolation tests according to EN 14405 shall be applied for basic
characterization of granular solid waste. The column percolation tests according to EN 16637-3 shall be
applied for basic characterization of construction products.
5.2 Number of eluates
By reference the percolation test requires the analysis of seven eluates to determine the release of
dangerous substances for an L/S ratio up to 10. These results are needed for characterization of the
granular solid waste and allow the determination of the release mechanism according to Annex E.
For specific scenarios, other than characterization, it may be beneficial to combine eluates or adopt
other testing schemes based on the one of this document. Examples of such scenarios are:
a) Release at a specific L/S ratio. If it is sufficient to know the cumulative release at a predetermined
L/S ratio, for instance L/S = 2, the test can be stopped after the collection of the fifth eluate fraction.
b) Factory production control. In the case of FPC it is checked whether the product conforms to the
previously determined characteristics (type testing). Different test methods may be used:
— in the case of testing in accordance with the standard it is sufficient to check the release for the
specified L/S ratio and to collect and combine successive eluates in proportion to the volumes,
e.g. L/S (0 to 2) l/kg dry matter or L/S (0 to10) l/kg dry matter;
— following an alternative testing procedure (indirect test method), the release at for instance
L/S (0 to 0,5) l/kg dry matter or L/S (0 to 1) l/kg dry matter, may be extrapolated to predict the
release after L/S (0 to 10) l/kg dry matter or another appropriate L/S ratio. Also, other leaching
tests may be used.
As long as the adapted test scheme is based on the one of this document and the test is performed
according to this document, the cumulative release at a specified L/S ratio is equal to the cumulative
release based on the reference test performance. The release mechanisms specified in Annex E of this
document cannot be determined if less than seven eluates are analysed.
6 Reagents
6.1 General
Use only reagents of recognized analytical grade, unless otherwise specified.
6.2 Leachant
Use as a leachant demineralized water or deionized water or water of equivalent purity with a
conductivity < 0,5 mS/m or better.
When the release of biodegradable organic compounds is studied, the eluate might be stabilized with a
preservative in order to avoid biodegradation.
For ecotoxicological tests, preservatives are not allowed.
6.3 Rinsing solutions
Use as rinsing solution nitric acid, c(HNO ) = 0,1 mol/l and an organic solvent (e.g. acetone). Make sure
that the quality grade of the nitric acid is appropriate for analysis of trace elements.
7 Equipment
7.1 General
Check the materials and equipment specified in 7.2 to 7.17 before use for proper operation and absence
of interfering substances that may affect the result of the test.
The equipment specified under 7.6, 7.7, 7.8, 7.14 and 7.15 shall be calibrated.
7.2 Column
Column made of plastics or glass for inorganic substances and glass or stainless steel for organic
substances with an inner diameter d larger than 50 mm and a length that can accommodate a filling
i
height of 300 mm ± 50 mm. In top and bottom of the column a filter plate, glass beads or a thin layer of
quartz sand with a particle size range of 1,0 mm to 2,5 mm is applied to ensure proper water flow over
the total width of the column.
Filter plates, quartz sand (SiO -content at least 98 % by mass) or glass beads can be washed but where
heated to remove any adsorbed organic contaminants they shall not be heated to red-heat. They shall
also be low in substances (i.e. determinants) which could lead to increased levels in procedural blanks.
NOTE 1 In some cases, it is useful to place a pre-filter at least in the bottom section to prevent the material from
leaving the column through the water inlet duct.
A drawing of the column and accompanying equipment is given in Annex C.
Glass of high quality is usually considered adequate for both metals and organic contaminants,
particularly, since the pH range usually covered in granular solid waste testing does not reach the
conditions where glass itself is attacked. For ecotoxicity testing, eluates with both metals and organic
contaminants are needed, which emphasizes the need to generate integrated eluates.
NOTE 2 Usually borosilicate glass is appropriate, unless boron has to be analysed. Sodium glass can change the
pH of the eluate.
In case of organic substances to be analysed, it shall be checked that the material does not interfere
significantly with the substances to be measured.
7.3 Packing equipment, Rammer with a weight of 125 g in the case of a column with a diameter of
50 mm up to 500 g for a column with a diameter of ≥ 100 mm. Intermediate weights to be linearly
interpolated by surface area.
NOTE The limited contact of the rammer is considered not to affect the test results.
7.4 Membrane for off-line filtration of eluates to be analysed for inorganic substances, with a pore
size of 0,45 µm (e.g. cellulose acetate, PTFE).
Membranes shall be of inert material and not absorb or adsorb compounds of interest. Filters shall not
be used for eluates to be analysed for organic substances.
7.5 Volumetric pump, with an adjustable capacity to be suitable to allow for the flow rate specified
according to 9.4.3.
7.6 Analytical balance, with an accuracy of at least 0,1 g.
7.7 pH meter, with an accuracy of at least 0,05 pH units.
7.8 Electrical conductivity meter, with an accuracy of at least 0,1 mS/m.
7.9 Tubing material, inert and adapted to the substances to be analysed. In case organic substances
are to be analysed, stainless steel or glass and FEP can be used in contact with the eluate. In case
inorganic substances are analysed PE, PP, PTFE, ETFE, FEP or similar tubing materials can be used.
NOTE Examples of appropriate tubing material are given in EN ISO 5667-3.
7.10 Eluate bottles
For eluate collection and preservation of eluate samples, use high quality glass bottles with an
appropriate volume and with screw cap with PTFE, ETFE or PTFE inlay (in accordance with
EN ISO 5667-3). If only inorganic contaminants are to be analysed, alternative bottle materials can be
selected, e.g. PE or PP.
NOTE Usually borosilicate glass is appropriate, unless boron has to be analysed. Sodium glass can change the
pH of the eluate.
7.11 Crushing equipment
Jaw crusher or a cutting device. The crushing device shall be cleaned thoroughly to avoid cross
contamination from previous use.
NOTE Due to crushing, contamination of the sample can occur to an extent which affects the leaching of some
constituents of concern e.g. cobalt and tungsten from tungsten carbide equipment or chromium, nickel and
molybdenum from stainless steel equipment.
7.12 Sieving equipment (dry sieving), e.g. with sieves 4 mm, 11,2 mm and 22,4 mm nominal screen
size.
7.13 Sample splitting equipment
For sub-sampling of laboratory samples, e.g. riffle divider or dividing cross for coning and quartering
(optional).
7.14 Redox potential meter (optional)
7.15 Turbidity meter, as specified in ISO 7027-1 [28].
7.16 Centrifuge
Use a centrifuge operating at 20 000 g to 30 000 g using centrifuge tubes of FEP or tubes of an
alternative material, which is inert with regard to both inorganic and organic substances and suitable to
high-speed centrifugation.
Alternatively, if a high-speed centrifuge is not available, a centrifuge operating at 2 000 g to 2 500 g
using glass bottles may be used in combination with increased centrifugation time. Cooling shall be
applied to maintain the desired temperature.
7.17 Filtration
Vacuum filtration device 30 kPa to 70 kPa or pressure filtration device (≤0,5 MPa).
8 Sample preparation
8.1 General
Sample preparation shall consist of preparation of the test sample from the laboratory sample,
preparing a test portion and determining the dry residue of the test sample.
Sampling shall be performed in accordance with the procedures described in the CEN/TR 15310 series
and EN 15002, considering guidance given in EN 16637-1 in order to obtain a representative laboratory
sample.
NOTE As usual in an accreditation procedure, the testing laboratory reports on sampling only when it
performs sampling itself to produce laboratory sample.
8.2 Preparation of the test sample
8.2.1 Principles
A laboratory sample shall be received whose minimum amount depends on the maximum particle size
of the granular solid waste, the column diameter chosen and the number of t
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