SIST-TS CEN/TS 14405:2004

SLOVENSKI STANDARD
SIST-TS CEN/TS 14405:2004
01-oktober-2004
.DUDNWHUL]DFLMDRGSDGNRY,]OXåHYDOQLSUHVNXVL3UHVNXVYNRORQLVWRNRPQDY]JRU
SULGRORþHQLKSRJRMLK
Characterization of waste - Leaching behaviour tests - Up-flow percolation test (under
specified conditions)
Charakterisierung von Abfällen - Auslaugungsverhalten - Perkolationsprüfung im
Aufwärtsstrom (unter festgelegten Bedingungen)
Caractérisation des déchets - Essais de comportement a la lixiviation - Essai de
percolation a écoulement ascendant (dans des conditions spécifiées)
Ta slovenski standard je istoveten z: CEN/TS 14405:2004
ICS:
13.030.01 Odpadki na splošno Wastes in general
SIST-TS CEN/TS 14405:2004 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST-TS CEN/TS 14405:2004

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SIST-TS CEN/TS 14405:2004
TECHNICAL SPECIFICATION
CEN/TS 14405
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
June 2004
ICS 13.030.10
English version
Characterization of waste - Leaching behaviour tests - Up-flow
percolation test (under specified conditions)
Caractérisation des déchets - Essais de comportement à la Charakterisierung von Abfällen - Auslaugungsverhalten -
lixiviation - Essai de percolation à écoulement ascendant Perkolationsprüfung im Aufwärtsstrom (unter festgelegten
(dans des conditions spécifiées) Bedingungen)
This Technical Specification (CEN/TS) was approved by CEN on 24 March 2004 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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France,
Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia,
Slovenia, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2004 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 14405:2004: E
worldwide for CEN national Members.

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Contents
page
Foreword.3
Introduction .4
1 Scope.4
2 Normative references.4
3 Terms and definitions .5
4 Principle.6
5 Equipment and reagents.6
5.1 General.6
6 Sample pre-treatment.7
6.1 General.7
6.2 Sample preparation.7
6.3 Test portion .8
6.4 Determination of dry residue.9
7 Procedure.9
7.1 Temperature.9
7.2 Preparation.9
7.3 Packing of the column.9
7.4 Start-up of the test.11
7.5 Collection of additional eluate fractions .12
7.6 Further preparation of the eluates for analysis .13
7.7 Blank test.14
8 Calculations .14
9 Test report.15
10 Test performance.16
Annex A (informative)  Illustration of the column and accompanying equipment.17
Annex B (informative)  Suggestions for packing the column, water saturation and
establishment and checking of equilibrium conditions .18
B.1 General.18
B.2 Guidelines on column filling and packing .18
B.3 Water saturation .18
B.4 Equilibration and checking of equilibrium conditions.19
Annex C (informative)  Background for the choices made in developing this percolation
test.21
C.1 Introduction.21
C.2 Particle size/particle size distribution.22
C.3 Column dimensions .22
C.4 Flow mode (up-flow/down-flow).22
C.5 Flow rate of the leachant .22
C.6 L/S ratio and eluate fractions collected/duration of the test .23
C.7 Nature of the leachant .23
C.8 Temperature .24
D.9 Beneficial use of the test results.24
Bibliography .25
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Foreword
This document (CEN/TS 14405:2004) has been prepared by Technical Committee CEN/TC 292
“Characterisation of waste”, the secretariat of which is held by NEN.
This Technical Specification has been developed primarily to support the requirements for leaching behaviour
testing within EU and EFTA countries.
This Technical Specification was elaborated on the basis of:
NEN 7343:1995
NT ENVIR 002:1995
This Technical Specification specifies an up-flow percolation test to determine the leaching behaviour of
granular waste materials under standardized percolation conditions. Another Technical Specification will be
produced to specify a percolation test for simulating conditions of specific scenarios.
For a more complete characterization of the leaching behaviour of waste under specified conditions the
application of other test methods is required (see ENV 12920). For informative references see the
Bibliography.
The annexes A, B and C are informative.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following
countries are bound to announce this Technical Specification: Austria, Belgium, Cyprus, Czech Republic,
Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Slovakia, Slovenia, Spain, Sweden, Switzerland
and United Kingdom
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Introduction
In various European countries tests have been developed to characterize and assess the constituents that can
be released from waste materials. The release of soluble constituents upon contact with water is regarded as
a main mechanism of release, which results in a potential risk to the environment during the re-use or disposal
of waste materials. These tests are intended to identify the leaching properties of waste materials. The
complexity of the leaching process makes simplifications necessary. Not all of the relevant aspects of leaching
behaviour can be addressed in one standard.
Tests to characterize the behaviour of waste materials can be divided into three categories. The relationships
between these tests are summarized below:
“Basic characterization“ tests are used to obtain information on the short and long term leaching behaviour
and characteristic properties of waste materials. Liquid/solid (L/S) ratios, leachant composition, factors
controlling leachability such as pH, redox potential, complexing capacity, ageing of waste and physical
parameters are addressed in these tests.
“Compliance“ tests are used to determine whether the waste complies with a specific behaviour or with
specific reference values. The tests focus on key variables and leaching behaviour previously identified by
basic characterization tests.
“On-site verification“ tests are used as a rapid check to confirm that the waste is the same as 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 (1): basic characterization tests.
1 Scope
This Technical Specification is applicable to determine the leaching behaviour of inorganic constituents from
granular waste (without or with size reduction (see 6.2)). The waste body is subjected to percolation with water
as a function of liquid to solid ratio under specified percolation conditions. The waste is leached under
hydraulically dynamic conditions. The method is a once-through column leaching test and the test results
establish the distinction between different release patterns, for instance wash-out and release under the
influence of interaction with the matrix, when approaching local equilibrium between waste and leachant.
NOTE 1 The mentioned specified percolation conditions are arbitrary and are not simulating a specific scenario.
-7 -8
NOTE 2 Waste materials that show a saturated hydraulic conductivity between 10 m/s and 10 m/s can be subjected to
this test, but it can be difficult to maintain the imposed flow rate. If a waste shows a saturated hydraulic conductivity below
-8
10 m/s, the test should not be carried out. (See C.5 for a definition of ‘hydraulic conductivity’.)
NOTE 3 This procedure is generally not applicable to biologically degrading materials and materials reacting with the
leachant, leading, for example, to excessive gas emission or excessive heat release.
NOTE 4 This procedure is applicable to materials showing solidification in the column, if the final hydraulic conductivity is
within the specified range (see NOTE 1).
2 Normative references
This Technical Specification incorporates by dated or undated reference, provisions from other publications.
These normative references are cited at the appropriate places in the text, and the publications are listed
hereafter. For dated references, subsequent amendments to or revisions of any of these publications apply to
this Technical Specification only when incorporated in it by amendment or revision. For undated references
the latest edition of the publication referred to applies (including amendments).
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- VI
EN 12506, Characterization of waste – Analysis of eluates – Determination of pH, As, Ba, Cd, Cl , Co, Cr, Cr ,
- 2-
Cu, Mo, Ni, NO , Pb, total S, SO , V and Zn.
2 4
EN 13370, Characterization of waste – Analysis of eluates – Determination of Ammonium, AOX, conductivity,
- -
Hg, phenol index, TOC, easily liberatable CN , F .
prEN 14346:2002, Characterization of waste – Calculation of dry matter by determination of dry residue or
water content.
prEN 14899, Characterisation of Waste - Sampling of waste materials: Framework for the preparation and
application of a Sampling.
EN ISO 5667-3, Water quality – Sampling – Part 3: Guidance on the preservation and handling of samples
(ISO 5667-3:2003).
3 Terms and definitions
For the purposes of this Technical Specification, the following terms and definitions apply.
3.1
dry residue w
dr
remaining mass fraction in percent of a sample after a drying process at 105 °C
[prEN 14346:2002]
3.2
eluate
solution obtained by a laboratory leaching test
3.3
equilibrium condition
condition achieved when the pH deviation during a checking period is below a specified value (see 7.4)
3.4
granular waste
solid waste that is neither monolithic, liquid, gas nor sludge
3.5
laboratory sample
sample or sub sample(s) sent to or received by the laboratory
[IUPAC, 1997]
3.6
leachant
liquid that is brought into contact with the test portion in the leaching procedure
3.7
liquid to solid-ratio
L/S
ratio between the amount of liquid (L) and of solid (S) in the test
NOTE L/S is expressed in l/kg dry matter.
3.8
sample
quantity that is representative of a certain larger quantity
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3.9
test portion
amount or volume of the test sample taken for testing or analysis, usually of known weight or volume
3.10
test sample
sample, prepared from the laboratory sample, from which test portions are removed for testing or analysis
[IUPAC, 1997]
4 Principle
This Technical Specification describes a method to determine the release of constituents from waste, with or
without size reduction, packed in a column with a leachant percolating through it. 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 components are rapidly being washed out and
which components are released under the influence of interaction with the matrix.
The test portion of the waste to be tested is packed in a column in a standardized manner. The leachant is
percolated in up-flow through the column at a specified flow rate up to a fixed L/S ratio. The eluate is collected
in several separate fractions that are characterized physically and chemically according to existing standard
methods. In the test, equilibrium conditions at the outlet of the column are verified after an equilibration period
by measuring a pH deviation.
The results of the test are expressed as a function of L/S ratio, in terms of both mg of the constituents
released per litre of eluate, and mg of the constituents released cumulatively per kg of waste material (dry
matter).
5 Equipment and reagents
5.1 General
The materials and equipment specified in 5.3 to 5.16 shall be checked before use for proper operation and
absence of interfering elements that may affect the result of the test (see 7.7).
The equipment specified in 5.4, 5.5, 5.11 and 5.14 shall also be calibrated.
5.2
Column made of glass or plastics (e.g. PMMA, PTFE) with an internal diameter of 5 cm or 10 cm and a filling
height of about 30 cm ± 5 cm, fitted with filters (see 5.9) in bottom and top section. In the top and bottom
sections of the column a filter plate or a thin layer of fine-grained non-reactive material (e.g. fine quartz sand)
is applied to ensure proper water flow over the width of the column and as a support for the pre-filter.
NOTE An illustration of the column and its accompanying equipment is given in annex A.
5.3
Adjustable volumetric pump (peristaltic or equivalent). For small columns, running at a linear velocity of
15 cm/day, the capacity shall be adjustable between 10 ml/h and 20 ml/h and for wide columns, running at the
same linear velocity, the capacity shall be adjustable between 40 ml/h and 60 ml/h.
5.4
Analytical balance with an accuracy of at least 0,1 g.
5.5
Conductivity meter with an accuracy of at least 0,1 mS/m.
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5.6
Crushing equipment: a jaw crusher or a cutting device.
5.7
Demineralized water with a conductivity of a maximum of 0,1 mS/m.
5.8
Glass or plastics (e.g. HDPE / PP / PTFE / PET) bottles with an appropriate volume, and with screw cap, for
eluate collection and preservation of eluate samples (rinsed in accordance with EN ISO 5667-3).
5.9
Membrane filters for in-line or off-line filtration of the eluates, with a pore size of 0,45 μm.
5.10
Nitric acid (pro analyse), 1 mol/l.
5.11
pH meter with an accuracy of at least 0,05 pH units.
5.12
Plastic hose material.
5.13
Pre-filters for the column with a pore size of 1,5 mm to 8 μm.
NOTE If the eluate is to be used for bio-assays or other specific situations, in which fine particles are important, pre-
filters with a larger pore size should be used.
5.14
Redox potential meter (optional).
5.15
Sample splitter for sub-sampling of laboratory samples (optional).
5.16
Sieving equipment with sieves of 4 mm and 10 mm nominal screen size.
6 Sample pre-treatment
6.1 General
Sampling shall be performed in accordance with WI 00292001 or a standard derived from WI 00292001, in
order to obtain a representative sample. Sample pre-treatment shall consist of sample preparation, taking a
test portion and determining the dry residue of the test sample.
NOTE If it is the intention to determine the leaching behaviour of a waste material, including ageing effects, the test
portion should be representative for the material in the practical situation, also as far as ageing conditions are concerned.
6.2 Sample preparation
A laboratory sample shall be obtained of at least 2,5 kg of the material if a small column (diameter 5 cm) is to
be used and of at least 10 kg, if a wide column (diameter 10 cm) is to be used. The laboratory sample shall be
stored in closed packages and kept under conditions, which prevent any alterations of the waste material.
NOTE 1 Storage at low temperatures (4 °C) may be required, in order to minimise unwanted alterations of the waste
material.
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To investigate whether the material has to be crushed and to investigate which type of column is to be used,
the laboratory sample shall be sieved (see 5.16).
The use of the small or wide column shall depend on the particle size of the material, according to Table 1.
Table 1 - Use of column type, related to particle size of waste
Column to be used (with required size-reduction)
Fraction < 4 mm Fraction ‡ 10 mm
‡ 95 % (m/m) Small column (without size reduction), or
Wide column (without size reduction)
80 % (m/m) to 95 %£ 5 % (m/m) Small column (with size reduction of the fraction ‡ 4 mm), or
(m/m)
Wide column (without size reduction)
Wide column (without size reduction)£ 80 % (m/m)£ 5 % (m/m)
> 5 % (m/m) Wide column (with size reduction of the fraction ‡ 10 mm
Prepare a test sample. Use a sample splitter (see 5.15) or apply coning and quartering to split the laboratory
sample.
The test shall be carried out preferably on a sample in the condition (particle size, moisture content) as it was
delivered to the laboratory.
If oversized material is to be size reduced (in accordance with Table 1), the entire oversized fraction shall be
crushed with a crushing device (see 5.6). On no account shall the material be finely ground. Non-crushable
material (e.g. metallic parts such as nuts, bolts, scrap) in the sample shall be separated and the mass and the
nature of the material shall be recorded.
If the sample cannot be sieved or split or crushed because of its moisture content, it is allowed to dry the
sample, but no further than is required for the sample preparation. The drying temperature shall not exceed
40 °C.
NOTE 2 Depending on the maximum particle size, the splitting can require size reduction of the coarser particles to comply
with the rules of sampling.
NOTE 3 Due to crushing and sieving, contamination of the sample can occur to an extent, which is affecting the release of
some constituents of concern, e.g. Co and W from tungsten carbide crushing equipment or Cr, Ni, Mo and V from stainless
steel equipment.
NOTE 4 Fibrous materials and plastics can often be size-reduced only after cryogenic treatment.
NOTE 5 Drying may lead to oxidation and/or carbonation. If the material is fresh and has to be tested as a non oxidized /
non carbonated material, the drying should be conducted in an inert atmosphere.
6.3 Test portion
At least two test portions shall be taken from the test sample. To fill the column completely, the quantity of one
of the test portions shall be such that its volume after compaction is 0,6 l (in case a column with a diameter of
5 cm is used), or 2,4 l (in case a column with a diameter of 10 cm is used). A sample splitter (see 5.15) shall
be used or coning and quartering shall be applied to split the test sample and prepare the test portion(s).
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6.4 Determination of dry residue
The dry residue of the test sample shall be known and taken into account when calculating the L/S ratio.
Determine the dry residue (w ) at 105 °C ± 5 °C according to prEN 14346, on a separate test portion.
dr
Calculate the dry residue in accordance with equation 1.
w = m · 100 / m [%] (1)
dr d r
where
w dry residue of the waste expressed as percentage [%];
dr
m mass of the undried test portion expressed in grams [g];
r
m dry mass of the test portion expressed in grams [g].
d
7 Procedure
7.1 Temperature
Carry out the up-flow percolation test at a temperature of 20 °C ± 5 °C.
NOTE A constant temperature of 20 °C in the test can be achieved by either controlling the temperature of the lab, or
controlling the temperature of the leachant and insulating the column and accompanying equipment.
7.2 Preparation
Rinse the column, including top and bottom sections and filters (see 5.2) and bottles (see 5.8) with nitric acid
(see 5.10) and water (see 5.11) consecutively. Weigh the dry column, including top and bottom sections, filters
and filter plates or layers of fine-grained material, to an accuracy of 1 g.
7.3 Packing of the column
Fit the bottom section, equipped with a filter plate or a layer of fine-grained chemically inert material (e.g. fine
quartz sand) of approximately 1 cm and a pre-filter (see 5.13) to the column. Fill the column with the test
portion, up to a bed height of 30 cm ± 5 cm, in at least five consecutive layers, as follows:
 Introduce each layer into the column in three sub-layers and level each sub-layer separately.
 Pack each layer using as a rammer a weight of 125 g in case of a column with a diameter of 5 cm, and of
500 g in case of a column with a diameter of 10 cm. Drop the weight three times on each layer falling
down 20 cm along a rod used as a guide. Fix this rod to the centre of a disk, which is placed on the layer
to be packed. Cover the whole surface of the column with the disk (as is shown in Figure 1).
 For the last layer, check the remaining height and adjust the necessary mass in order to get 30 cm ± 5 cm.
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Key
1 Layer of compacted waste
2 Rammer drilled in the centre
3 Column
4 Rod for the manipulation of the rammer
5 Guide
6 Water inlet
Figure 1 – Filling and packing of the column
NOTE 1 In order to determine the proper mass for each layer, a preliminary test may be carried out. In that case, put a
7 cm to 8 cm layer in the column, pack it and calculate the mass necessary to get a layer of approximately 6 cm.
NOTE 2 If the column is not high enough to work according to the above mentioned packing procedure, a heightening
device may be required.
NOTE 3 It is difficult to pack some specific materials in the column in an appropriate way. Annex B gives guidelines on
how to handle in that specific cases.
Fit the top section of the column, equipped with a filter plate or a layer of fine-grained chemically inert material
(e.g. fine quartz sand) of approximately 1 cm and a pre-filter (see 5.13), to prevent entrainment of fine particles
with the eluate. Fit the top section and pre-filter so that the liquid flow cannot bypass the filter and so that no
open space (dead volume) is left above the material.
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NOTE 4 Care should be taken in positioning the pre-filter in place: the filter can tear.
Weigh the column thus filled to an accuracy of 1 g. Determine the dry mass (m ) of the test portion in the
0
column, in accordance with equation 2.
m = (m · w ) / 100 % (2)
0 dr
where
m dry mass of the test portion in the column expressed in kilogram [kg];
0
m  mass of the (moist) test portion in the column expressed in kilogram [kg];
w dry residue expressed as percentage [%].
dr
Fit the outlet-hose to the top section of the column and to the in-line filter (see 5.9), in case an in-line filter is
used.
7.4 Start-up of the test
Saturate the column with water (5.7) either by using the pump (see 5.3) or by hydrostatic pressure (see B.3).
NOTE 1 See annex B for a more detailed description of the methods of saturation.
Stop the pump, or take away the hydrostatic pressure, when the material in the column is all saturated, but the
outlet hose remains empty. Leave the saturated material for a period of three days, in order to equilibrate the
system.
NOTE 2 To facilitate equilibration and the procedure of checking the equilibrium conditions, recirculation of eluate may be
applied. See annex B.
After the equilibration period, start the pump (again) and set the flow rate such that the linear velocity is
15 cm/day ± 2 cm/day through the empty column. Calculate the flow rate in accordance with equation 3.
2
f= v · p · d · 0,0104 (3)
L
where
fleachant flow rate [ml /h];
v linear velocity of the leachant through the empty column [cm/day];
L
d  diameter of the column [cm].
NOTE 3 A linear velocity of 15 cm/day corresponds with a flow rate of 12 ml/h for a column with a diameter of 5 cm and
...