CEN/TS 16637-3:2016

SLOVENSKI STANDARD
01-marec-2017
*UDGEHQLSURL]YRGL2FHQMHYDQMHVSURãþDQMDQHYDUQLKVQRYLGHO+RUL]RQWDQL
SUHVNXVSUHFHMDQMDYNRORQLVWRNRPQDY]JRU
Construction products - Assessment of release of dangerous substances - Part 3:
Horizontal up-flow percolation test
Bauprodukte - Bewertung der Freisetzung von gefährlichen Stoffen - Teil 3: Horizontale
Perkolationsprüfung im Aufwärtsstrom
Produits de construction - Evaluation de l’émission de substances dangereuses - Partie
3 : Essai horizontal de percolation à l’écoulement ascendant
Ta slovenski standard je istoveten z: CEN/TS 16637-3:2016
ICS:
13.020.99 Drugi standardi v zvezi z Other standards related to
varstvom okolja environmental protection
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.

CEN/TS 16637-3
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
June 2016
TECHNISCHE SPEZIFIKATION
ICS 19.040; 13.040.20; 91.100.01
English Version
Construction products - Assessment of release of
dangerous substances - Part 3: Horizontal up-flow
percolation test
Produits de construction - Evaluation de l'émission de Bauprodukte - Bewertung der Freisetzung von
substances dangereuses - Partie 3 : Essai horizontal de gefährlichen Stoffen - Teil 3: Horizontale
percolation à l'écoulement ascendant Perkolationsprüfung im Aufwärtsstrom
This Technical Specification (CEN/TS) was approved by CEN on 15 March 2016 for provisional application.

The period of validity of this CEN/TS is limited initially to three years. After two years the members of CEN will be requested to
submit their comments, particularly on the question whether the CEN/TS can be converted into a European Standard.

CEN members are required to announce the existence of this CEN/TS in the same way as for an EN and to make the CEN/TS
available promptly at national level in an appropriate form. It is permissible to keep conflicting national standards in force (in
parallel to the CEN/TS) until the final decision about the possible conversion of the CEN/TS into an EN is reached.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION

EUROPÄISCHES KOMITEE FÜR NORMUNG

CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2016 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 16637-3:2016 E
worldwide for CEN national Members.

Contents Page
European foreword . 4
Introduction . 5
1 Scope . 7
2 Normative references . 7
3 Terms and definitions . 8
4 Symbols and abbreviations . 10
4.1 Symbols . 10
4.2 Abbreviations . 11
5 Principle . 11
6 Reagents . 12
7 Equipment . 12
8 Sample preparation . 14
8.1 General . 14
8.2 Preparation of the test sample . 14
8.2.1 Principles . 14
8.2.2 Rules of application . 15
8.3 Test portion . 16
8.4 Drying . 16
8.5 Subsampling . 16
8.6 Sieving of samples into fractions . 16
8.7 Size reduction of particles . 17
9 Test procedure . 17
9.1 Temperature . 17
9.2 Determination of dry residue . 17
9.3 Pre-treatment of the column. 17
9.4 Packing of the column . 18
9.5 Start of the test . 18
9.5.1 Equilibration . 18
9.5.2 Calculation of the flow rate . 18
9.6 Collection of eluates . 18
9.7 Further preparation of the eluates for analysis . 21
9.8 Blank test . 21
10 Evaluation of measurement results . 21
10.1 Expression of results in concentrations. 21
10.2 Expression of results in terms of mass related release . 22
11 Documentation and test report. 22
12 Test performance . 24
13 Indirect methods . 24
13.1 Definition . 24
13.2 Provisions . 24
13.3 Examples of “indirect” methods . 24
Annex A (informative) Examples for sample preparation procedure . 25
A.1 General . 25
A.2 Example 1 . 25
A.3 Example 2 . 26
Annex B (informative) Illustration of the column and accompanying equipment . 28
Annex C (normative) Procedures for packing and saturation of the column . 29
C.1 General . 29
C.2 Column filling and packing . 29
C.3 Procedure for packing . 29
C.4 Water saturation . 30
Annex D (informative) Assessment of release mechanism(s) . 32
D.1 Overview of release mechanisms . 32
D.2 Overview of release mechanisms . 33
D.3 Overview of release mechanisms . 37
D.4 Examples . 38
Bibliography . 54

European foreword
This document (CEN/TS 16637-3:2016) has been prepared by Technical Committee CEN/TC 351
“Construction Products: Assessment of release of dangerous substances”, 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 December 2016 and conflicting national standards
shall be withdrawn at the latest by December 2016.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN [and/or CENELEC] shall not be held responsible for identifying any or all such patent
rights.
This document has been prepared under a mandate given to CEN by the European Commission and the
European Free Trade Association.
This Technical Specification was elaborated on the basis of CEN/TS 14405.
This Technical Specification specifies an up-flow percolation test to determine the leaching behaviour of
granular construction products under standardized percolation conditions.
CEN/TS 16637-1 deals with the determination and use of test methods for leaching of construction
products taking specific situations into account. CEN/TS 16637-2 specifies a dynamic surface leaching
test for determination of surface dependent release of substances from monolithic or plate-like or
sheet-like construction products or granular construction products with low hydraulic conductivity
under standardized conditions.
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 and CEN/TR 16496).
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, Former Yugoslav Republic of Macedonia,
France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta,
Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and the United Kingdom.
Introduction
This introduction describes the interactions and interrelations between the three Technical
Specifications CEN/TS 16637-1, CEN/TS 16637-2 and CEN/TS 16637-3 developed to assess the release
of dangerous substances from construction products into soil, surface water and ground water in the
framework of the Mandate M/366. The horizontal test methods developed under the Mandate M/366
are intended to be used to show compliance with notified regulations. The tests cover the release of
substances from construction products and in particular, those that are regulated in notified regulations
in one or more EU member states.
CEN/TS 16637-1 specifies how the CEN Technical Product Committees and EOTA experts are to
determine the appropriate leaching test for the determination of the release of Regulated Dangerous
Substances from a construction product into soil, surface water and groundwater.
CEN/TS 16637-2 describes a test to assess surface dependent release from monolithic, plate-like or
sheet-like construction products while CEN/TS 16637-3 describes a horizontal test to assess release
from granular construction products. The test methods specified in CEN/TS 16637-2 and
CEN/TS 16637-3 can be used for both steps in the hierarchy (type testing and factory production
control) and are supposed to be used as the reference test for the intended uses and conditions
specified in CEN/TS 16637-1. In this hierarchy of testing conditionally “indirect tests” can be used, but
are not specified. CEN/TS 16637-2 includes a procedure with a modified tank leaching test GLHC for
testing granular products with a low hydraulic conductivity as determined by failure to achieve a
sufficient water flow in the percolation test.
The release of substances upon contact with water results in a potential risk to the environment during
the intended use of construction products. The intent of these tests is to identify the leaching behaviour
of construction products and thereby allow assessments of the release of Regulated Dangerous
Substances from such products to soil, surface water and groundwater under intended use conditions in
relation to CE marking.
Technical Product Committees are expected to apply the test standards developed in CEN/TC 351 for
their products in order to test the potential release of Regulated Dangerous Substances to soil, surface
water and groundwater. CEN/TS 16637-1 is intended to provide clear procedures to determine which
test method is appropriate for a given product. CEN/TS 16637-1 aims to provide the information,
needed in a CEN Technical Product Committee, on how to deal with the relevant test method(s) to
enable the producer to declare a performance in the CE marking as a result of the test. CEN Technical
Product Committees are referred to the informative Annexes A and B of CEN/TS 16637-1 and to
CEN/TR 16098 for background information on the following aspects:
a) identification of the products addressed in the product standards which have relevance with
respect to the release of dangerous substances into soil, surface water and groundwater (products
only applied in the interior of buildings are not subject to testing for these properties);
b) description of the intended use conditions of the construction product (e.g. above ground exposed
to the precipitation, or shielded from direct infiltration, in surface or ground water) in respect to
the release of dangerous substances into soil, surface water and groundwater;
c) identification of main release mechanisms.
Impact assessment is not part of the work of CEN/TC 351.
In addition to existing validation results, in 2011 CEN/TC 351 began an extensive research program on
robustness validation of the existing tank leaching and percolation tests. This was carried out by a
consortium of European experts on 20 construction products to unify differences from the protocols in
different CEN-Member States and to check the influence of testing conditions on the test result (e.g.
temperature, flow rate, renewal scheme, particle size in the percolation test etc., see bibliography. The
results of the research program confirmed the robustness of the horizontal tests known from former
works. Conclusions from the program have been implemented into the Technical Specifications for the
test methods. However, the performance of the leaching test regarding repeatability and reproducibility
is dependent on the tested construction product and on the testing conditions. When these Technical
Specifications of the horizontal leaching tests are adopted by CEN, the leaching tests referred to in these
Technical Specifications will not yet be fully validated. No data will be available on repeatability and
reproducibility for the range of construction products. For other, sometimes comparable, matrices
performance data are available from national as well as EU validation studies.
1 Scope
(1) This Technical Specification specifies an Up-flow Percolation Test (PT) which is applicable to
determine the leaching behaviour of inorganic and non-volatile organic substances from granular
construction products. The test is not suitable for substances that are volatile under ambient conditions.
The construction products 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.
(2) This up-flow percolation test is performed under specified test conditions for construction
products 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 1 Volatile organic substances include the low molecular weight substances in mixtures such as mineral
oil.
NOTE 2 It is not always possible to adjust test conditions simultaneously for inorganic and organic substances
and test conditions may 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.
−8
Construction products that exhibit a saturated hydraulic conductivity of about 10 m/s or higher can
usually be subjected to this test. This procedure is also applicable to materials showing solidification in
the column, if the final hydraulic conductivity is within the specified range. Inert granular material
should not be added to improve permeability in order to enable their testing.
NOTE 4 This procedure is generally not applicable to products that are easily biologically degradable and
products reacting with the leachant, leading, for example, to excessive gas emission or excessive heat release,
impermeable hydraulically bound products or products that swell in contact with water.
2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
EN 933-1, Tests for geometrical properties of aggregates - Part 1: Determination of particle size
distribution - Sieving method
EN 14346, Characterization of waste - Calculation of dry matter by determination of dry residue or water
content
EN 16192, Characterization of waste - Analysis of eluates
CEN/TS 16637-1, Construction products - Assessment of release of dangerous substances - Part 1:
Guidance for the determination of leaching tests and additional testing steps
EN 16687, Construction products - Assessment of release of dangerous substances - Terminology
EN ISO 3696, Water for analytical laboratory use - Specification and test methods (ISO 3696)
EN ISO 5667-3, Water quality - Sampling - Part 3: Preservation and handling of water samples
(ISO 5667-3)
ISO 7027, Water quality - Determination of turbidity
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
dry residue
w
dr
remaining mass fraction of a sample after a drying process at 105 °C
[SOURCE: EN 14346:2006]
3.2
eluate
solution obtained from a leaching test
[SOURCE: EN 16687]
3.3
granular construction product
product composed of solid particles with a particle size smaller than a specified size or grading
Note 1 to entry: Granular products are usually tested by a percolation test.
3.4
laboratory sample
sample or sub-sample(s) sent to or received by the laboratory
[SOURCE: IUPAC 1990, 2.5.5]
Note 1 to entry: When the laboratory sample is further prepared by subdividing, cutting, sawing, coring, mixing,
drying, crushing, and 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 or for the preparation of the test specimen.
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.
3.5
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]
3.6
leaching behaviour
release and change with time in release from a solid product 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]
3.7
liquid to solid-ratio
L/S
ratio between the total volume of liquid (L) percolated through the solid product and of solid product
(S) packed into the column
Note 1 to entry: L/S is expressed in l/kg dry matter.
[SOURCE: EN 16687]
3.8
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
[SOURCE: EN 16687]
3.9
percolation test
PT
column test
release test method to determine the release of substances from a granular construction product
packed in a column with a leachant percolating through it
[SOURCE: EN 16687]
3.10
release
emission
liberation of chemical substances (e.g. non-volatile organic compounds, heavy metals, salts)
from a construction product into soil, surface water or groundwater into the leachant of a test facility
Note 1 to entry: Release to soil, surface and groundwater may be expressed in terms of area related release
(tank leaching test, e.g. mg/m ) or in terms of mass related release (percolation test, e.g. mg/kg).
[SOURCE: EN 16687]
3.11
release mechanism
physico-chemical processes that control the release of substances from a solid construction product
into a leachant
Note 1 to entry: In case of granular products 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]
3.12
sample
portion of material selected from a larger quantity of material
[SOURCE: IUPAC 1990, 2.1.1]
Note 1 to entry: The manner of selection of the sample should be prescribed in a sampling plan (3.13).
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.
3.13
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]
3.14
test portion
amount of the test sample (3.15) taken for testing/analysis purposes, usually of known weight or
volume
[SOURCE: IUPAC 1990, 2.5.7]
3.15
test sample
sample, prepared from the laboratory sample (3.4), from which test portions (3.14) are removed for
testing or for analysis
[SOURCE: IUPAC 1990, 2.5.6]
4 Symbols and abbreviations
4.1 Symbols
For the purposes of this Technical Specification, the following symbols apply.
D sieve diameter 31,5 mm, 45 mm or 63 mm
max
E released quantity of a substance per quantity of sample for analysis in eluate fraction i,
i
expressed in milligrams per kilogram dry matter (mg/kg dry matter)
S sieve diameter for test sample preparation (crushing) to reduce the amount of oversized
cs
product to fit the inner column diameter
U measured cumulative release of a substance for cumulative L/S-ratio n including fraction i = 1
n
to n, expressed in milligrams per kilogram dry matter (mg/kg dry matter)
V volume of the eluate fraction i, expressed in litres (l)
i
V linear velocity of the leachant through the empty column, expressed in millimetres per day
L
(mm/d)
c concentration of the substance concerned in the eluate fraction i
i
d inner diameter of the column, expressed in millimetres (mm)
h packing height of the column, expressed in millimetres (mm)
m dry mass of the test portion, expressed in grams (g)
d
m mass of the undried test portion, expressed in grams (g)
r
t execution time of the test, expressed in days (d)
w dry residue of the construction product, expressed as percentage (%)
dr
Φ leachant flow rate, expressed in millilitres per hour (in ml/h)
4.2 Abbreviations
For the purposes of this Technical Specification, the following abbreviations apply.
DOC dissolved organic carbon
EC electrical conductivity
ETFE ethylene tetrafluoroethylene
FEP fluorinated ethylene propylene
GLHC test method for granular products with low hydraulic conductivity
HDPE high-density polyethylene
PAH polycyclic aromatic hydrocarbon
PCTFE polychlortrifluorehtylene
PTFE polytetrafluorethylene
TPH total petroleum hydrocarbons
5 Principle
(1) The percolation test described in this Technical Specification starts with the representative
laboratory sample. The methodology for the collection of a representative laboratory sample is part of
the respective product standard.
(2) This Technical Specification describes a method to determine the release of substances from a
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
construction product 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.
(3) 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 product or of mg of
substance determined per litre of eluate.
(4) The procedure described in this standard 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, less stringent requirement on equipment (e.g.
column and tubing material, centrifugation) may be adapted for some steps of the procedure.
6 Reagents
Use only reagents of recognized analytical grade, unless otherwise specified.
6.1 Leachant
Demineralized water or deionized water or water of equivalent purity with a conductivity < 0,5 mS/m
according to grade 3 specified in EN ISO 3696.
When the release of biodegradable organic compounds is studied, the leachant might be stabilized with
a preservative in order to avoid biodegradation, e.g. sodium azide (NaN ) at a concentration of 0,1 %.
For ecotoxicological tests, preservatives should not be used. Addition of preservatives may also affect
the release of inorganic substances.
6.2 Rinsing solutions
Nitric acid (pro analyse) c(HNO ) = 0,1 mol/l
6.3 Organic solvent
E.g. acetone, pro analyse.
7 Equipment
7.1 General
(1) The materials and equipment specified in 7.2 to 7.17 shall be checked before use for proper
operation and absence of interfering substances, which can affect the result of the test.
(2) The equipment specified under 7.6, 7.7, 7.8, 7.14 and 7.15 shall be calibrated.
7.2 Column
(1) 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
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.
(2) Filter plates, quartz sand (SiO -content at least 98 % by mass) or glass beads can be washed but
where heated to remove any sorbed 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.
(3) A drawing of the column and accompanying equipment is given in Annex B.
(4) Glass of high quality is usually considered adequate for both metals and organic contaminants,
particularly, since the pH range usually covered in product 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.
(5) 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.
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. PTFE). They shall be of inert material and not 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 9.5.2.
7.6 Analytical balance with an accuracy of at least 0,1 g.
7.7 pH meter with 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 (see EN ISO 5667-3).
NOTE 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.
7.10 Eluate bottles
High quality glass bottles with an appropriate volume and with screw cap with PTFE, ETFE or PTFE
inlay, for eluate collection and preservation of eluate samples (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.
7.11 Crushing equipment
Jaw crusher or a cutting device.
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.
7.16 Centrifuge
(1) Operating at 20 000 g to 30 000 g using centrifuge tubes of FEP (fluorinated ethylene propylene) or
tubes of an alternative material, which is inert with regard to the substances to be measured and
suitable to high speed centrifugation.
(2) Alternatively, if a high speed centrifuge is not available, a centrifuge operating at 2 000 g to 2 500 g
using bottles of an appropriate material 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
(1) 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.
(2) Sampling shall be performed in accordance with the procedures described in the respective product
Standard considering guidance given in CEN/TS 16637-1 in order to obtain a representative laboratory
sample.
NOTE As usual in 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
(1) A laboratory sample shall be received whose minimum amount depends on the maximum particle
size of the granular product, the column diameter chosen and the number of tests to be carried out. The
laboratory sample shall be stored in closed packages and kept under conditions which prevent any
alterations of the construction product.
(2) The laboratory selects the appropriate column and determines the sieve diameter S (7.12) for the
cs
test sample (see Table 1).
(3) Crushing of the product shall be applied no more than absolutely necessary in order to minimize the
effect on the product properties, i.e. crushing is only needed in case of an oversized fraction larger than
S (see Table 1) or to fill a lack of fines less than 4 mm.
cs
(4) For granular construction products at least 45 % by mass of the test sample shall have a particle
size < 4 mm. If the grading of the laboratory sample already contains 100 % by mass particles < S (see
cs
Table 1) and an amount of particles of at least 45 % by mass < 4 mm no further crushing or sieving is
allowed.
(5) The choice of column width depends on the maximum particle size of the product to be tested (S )
cs
and may also depend on equipment available in the laboratory, the mass of the laboratory sample or the
amount of eluate required for chemical analysis or ecotoxicological testing.
(6) No part of the laboratory sample shall be discarded during the sample preparation.
8.2.2 Rules of application
(1) The following stepwise procedure to prepare the test sample shall be applied to fulfill the principles
specified in 8.2.1:
a) If the laboratory sample of the product already contains 100 % by mass of particles < S (see
cs
Table 1) and an amount of particles of least 45 % by mass < 4 mm no further crushing or sieving is
allowed (see Annex A for an example).
b) If the laboratory sample contains an oversized fraction larger than S gently crush this fraction to
cs
obtain a test sample with all particles ≤ S (result: test sample with a maximum particle size to fit
cs
the chosen column size).
Crusher jaws should be adjusted to avoid large amounts of particles < 4 mm.
c) Depending on the number and size of the test portions, the further procedure may be carried out on
a representative subsample (see EN 933-1).
d) Check by sieving on 4 mm-sieve whether test sample contains an amount of particles < 4 mm larger
than 45 % by mass. If this condition is fulfilled the test sample is ready to take test portions for the
percolation test.
e) If the test sample does not contain an amount of at least 45 % by mass passing the 4 mm-sieve after
the step d), gently crush a sufficient and representative portion of 4/ S mm (see Annex A for an
cs
example) to an extent that after crushing the completely prepared (recombined) grading contains
an amount of particles < 4 mm between 45 % by mass and 55 % by mass. If this condition is
fulfilled, the test sample is ready to take test portions for the percolation test.
Table 1 — Column size and corresponding sieve diameter S
cs
Inner column diameter Sieve diameter for test sample preparation (crushing)
to reduce the amount of oversized product to fit the
d
inner column diameter
[mm]
S
cs
[mm]
50 - 100 16
70 - 100 22,4
a
d ≥ 100 and d ≥ 3D D
max max
a
If the sample contains at least 45 % by mass particles < 4 mm, no crushing is allowed. If this condition does not
apply, set S to 22,4 mm.
cs
(2) The particle size distribution of the original granular product should be reported, if available.
Regarding the test sample, the maximum particle size and the percentage of particles < 4 mm shall be
reported.
8.3 Test portion
(1) At least two test portions shall be taken from the test sample (one for determination of the dry
residue, and one for the percolation test itself). The test portions shall be subsampled in line with 8.5.
It is recommended to reserve a test portion to be able to repeat the test in case of failure. It is often
considered good practice to perform the test in duplicate or triplicate (which would require additional
test portions).
(2) The amount of the test portion for the column is depending on the diameter of the column, the
packing height, the density of the granular product and the porosity of the packing.
8.4 Drying
If the sample cannot be sieved or crushed, due to its moisture content, it may be dried, but no further
than is required for the preparation of the test sample. Freeze drying or drying at room temperature is
preferred prior oven drying. The drying temperature shall not exceed 40 °C.
NOTE Drying may alter the properties of the sample (oxidation and/or carbonation) or result in loss of
volatile substances. Drying conducted in an inert atmosphere may prevent alteration of the sample properties.
Guidance on drying of samples is given in EN 15002 and EN 16179.
8.5 Subsampling
A sample splitter (7.13) shall be used or coning and quartering shall be applied to divide the sample and
prepare subsamples.
NOTE Guidance on subsampling is given in EN 15002 and EN 16179.
8.6 Sieving of samples into fractions
Sieving of samples into particle fractions shall be done by dry sieving only, according to EN 933-1.
8.7 Size reduction of particles
If oversized particles are to be size reduced, the entire oversized fraction shall be crushed with a
crushing device (7.11) to grains smaller than the maximum particle size (S ) required for the test
cs
portion. Crushing shall proceed no further than is required for the sample preparation. Heating, loss of
dust or contamination from the equipment shall be minimized. On no account shall the material be
finely ground. Non–crushable material (e.g. metallic particles) shall be separated, weighed and the
nature of the material recorded.
NOTE Plastic or bituminous products may be size-reduced after cryogenic treatment. Guidance on particle
size reduction is given in EN 15002 and EN 16179.
9 T
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