SIST-TS CEN/TS 15413:2007

SLOVENSKI STANDARD
SIST-TS CEN/TS 15413:2007
01-marec-2007
Trdno alternativno gorivo - Metode za pripravo preskusnega vzorca iz
laboratorijskega vzorca
Solid recovered fuels - Methods for the preparation of the test sample from the laboratory
sample
Feste Sekundärbrennstoffe - Verfahren zur Herstellung der Versuchsprobe aus der
Laboratoriumsprobe
Combustibles solides de récupération - Méthodes pour la préparation d'échantillons pour
essais a partir d'échantillons de laboratoire
Ta slovenski standard je istoveten z: CEN/TS 15413:2006
ICS:
75.160.10 Trda goriva Solid fuels
SIST-TS CEN/TS 15413:2007 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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TECHNICAL SPECIFICATION
CEN/TS 15413
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
September 2006
ICS 75.160.10

English Version
Solid recovered fuels - Methods for the preparation of the test
sample from the laboratory sample
Combustibles solides de récupération - Méthodes pour la Feste Sekundärbrennstoffe - Verfahren zur zur Herstellung
préparation d'échantillons pour essais à partir d'échantillons einer Prüfprobe aus einer Laborprobe
de laboratoire
This Technical Specification (CEN/TS) was approved by CEN on 25 March 2006 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, Romania,
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
© 2006 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 15413:2006: E
worldwide for CEN national Members.

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CEN/TS 15413:2006 (E)
Contents Page
Foreword.3
Introduction .4
1 Scope .5
2 Normative references .5
3 Terms and definitions .5
4 Safety remarks .6
5 Principle.6
6 Apparatus .6
7 Interferences and sources of error .6
8 Procedure .7
9 Quality control.10
10 Performance characteristics .10
11 Test report .10
Annex A (normative) Guideline for choosing sample treatment techniques .11
Annex B (informative) Relationship between minimum amount of sample and particle size.20
Annex C (informative) Sample treatment equipment.23
Annex D (normative) Guidelines - Characteristics of the laboratory sample for chemical analysis
of SRF .24
Bibliography .26

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CEN/TS 15413:2006 (E)
Foreword
This document (CEN/TS 15413:2006) has been prepared by Technical Committee CEN/TC 343 “Solid
Recovered Fuels”, the secretariat of which is held by SFS.
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, Romania, Slovakia, Slovenia, Spain, Sweden,
Switzerland and United Kingdom.

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CEN/TS 15413:2006 (E)
Introduction
In laboratory praxis different analytical procedures need to be applied very often to the laboratory sample that
has been taken according to the sampling plan. For this purpose sub-sampling is applied in a way, that the
different test portions are representative for the original laboratory sample with respect to the compounds of
interest and the specific analytical procedures. The representativity of the laboratory sample and of the test
portions is of major importance to guarantee the quality and accuracy of analytical results. The representativity
of the laboratory sample is specified by the sampling plan.
This Technical Specification is largely based on the work already done by CEN/TC 292 "Characterization of
waste", and in particular on latest drafts of just published EN 15002; actually, some experts who developed
EN 15002 actively participated to the preparation of this Technical Specification as well.
EN 15002 was developed for the majority of waste samples, and most of its concepts and specifications are
actually applicable to SRF samples as well, but there would be a number of major problems:
 several points of Annex A (normative) of EN 15002:2006 ("Guideline for choosing sample treatment
techniques") are simply not applicable for SRF samples, due to the very particular nature of these
samples, and in some cases this could be actually misleading.
 the main peculiarity that makes SRF samples significantly different from other kind of waste is that very
often SRFs are solid, but neither "granular" nor monolithic; it often happens that SRF samples are fibrous-
like materials, so the statistical formula for sampling (Annex B normative of EN 15002:2006, that links the
minimum amount of sample depending on the particle size and other parameters), that is one of the
foundations of EN 15002, is not applicable "as it is": one more term in the statistical equation is needed,
namely the "shape factor" (s).
 all examples contained in Annex E of EN 15002:2006 are just not applicable for SRF samples, which may
lead users who need to analyze SRF samples to misunderstandings.
Because of these reasons, a significant revision of just-published EN 15002 would have been necessary in
order to fulfil all requirements for SRF samples, which presumably had better to be carried out jointly by CEN/
TC 292 and TC 343. Moreover, even other CEN/TC 292 standards and TSs on sampling of waste would have
become inconsistent and would have had to be revised in order to include the "shape factor" in the statistical
formula. However, all of this work would probably have caused unacceptable delays for both CEN TCs. So,
CEN TC 343 decided to proceed with the development of a new Technical Specification.
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CEN/TS 15413:2006 (E)
1 Scope
This Technical Specification specifies the correct sequence of operations to ensure the representativity of the
test portions that has been taken according to the sampling plan, prior to physical and/or chemical analysis
(e.g. extractions, digestion and/or analytical determinations) of solid samples.
This Technical Specification specifies the correct sequence of operations and treatments to be applied to the
laboratory sample in order to obtain suitable test portions in compliance with the specific requirements defined
in the corresponding analytical procedures.
2 Normative references
The following referenced documents are indispensable for the application of this Technical Specification. For
dated references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
CEN/TS 15357:2006, Solid recovered fuels — Terminology, definitions and descriptions
prCEN/TS 15443, Solid recovered fuels — Methods for laboratory sample preparation
3 Terms and definitions
For the purposes of this Technical Specification, the terms and definitions given in CEN/TS 15357:2006 and
the following apply.
3.1
drying
process of removing water from a sample
NOTE For the purpose of test portion preparation, it may be useful to remove just the amount of water that could
interfere with other processes involved (e.g. during crushing or milling). In order to minimise the alteration of the sample
during test portion preparation, removing the total amount of water present in the sample is not necessarily needed.
3.2
fraction separation
process of dividing components, particles or layers if homogenisation of the sample is practically not
applicable and/or the analyses of different fractions or phases are appropriate
3.3
homogenisation
process of combining of components, particles or layers into a more homogeneous state of the original
samples (in the case of composite samples) or pre-treated fractions of samples in order to ensure equal
distribution of substances in and properties of the sample
3.4
sub-sampling
process of selecting one or more sub-samples from a sample
3.5
test portion; analytical portion
quantity of material of proper size, for measurement of the concentration or other properties of interest,
removed from the test sample
NOTE The test portion may be taken from the laboratory sample directly if no preparation of sample is required (e.g.
with liquids or samples of proper homogeneity, size and fineness), but usually it is taken from the prepared test sample.
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CEN/TS 15413:2006 (E)
3.6
test sample; analytical sample
sample, prepared from the laboratory sample, from which test portions are removed for testing or analysis
NOTE 1 When the laboratory sample is further prepared (reduced) by subdividing, mixing, grinding, 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 or for analysis.
NOTE 2 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.
NOTE 3 Several laboratory samples may be prepared and sent to different laboratories or to the same laboratory for
different purposes. When sent to the same laboratory, the set is generally considered as a single laboratory sample and is
documented as a single sample.
4 Safety remarks
The safety in handling of potentially hazardous materials is dealt with relevant national and European
regulations, which every laboratory should refer to.
In addition the following information is given:
 the apparatus for grinding, cutting, milling, and homogenisation may result harmful for the users. They
have to be operated by skilled personnel strictly according to the manufacturer instructions;
 all procedures have to be performed in a hood or in closed force-ventilated equipment, due to the
possibility of generation of fine powders.
5 Principle
The laboratory sample is reduced in particle size and mass using different apparatus and procedures
depending on the type of sample and the type of analysis to which the sample will be submitted.
6 Apparatus
For the purpose of preparation of test portions from the laboratory samples appropriate equipment has to be
chosen depending on the procedures selected according to Annex A.
In the selection of the type of treatment techniques, one should keep in mind that each of them has some
potential impact on analytical results, because it can introduce contamination or alter the physical-chemical
properties of the sample.
All glassware and devices that come in contact with the sample shall be made out of a suitable material,
chemically compatible with the sample, selected in order to minimize contamination of samples. Care shall be
taken to ensure a good cleaning, in order to avoid cross-contamination of samples.
An informative list of appropriate equipment for the sample treatment procedures is given in Annex C.
7 Interferences and sources of error
The (sub)-sample shall be re-homogenised after any operation that may have resulted in segregation of
different sized particles.
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CEN/TS 15413:2006 (E)
Care should be taken to avoid loss of material and contamination of the sample via the air, by dust, by the use
of the apparatus (e.g. from the ambient laboratory atmosphere or between samples stored or processed close
to one another).
Three types of contamination could occur from the apparatus:
 abrasion;
 cross-contamination;
 chemical release.
Chemical reaction due to generated heat can also be a source of error and material alteration.
It is recommended to perform treatment of waste material in a separate room used only for this purpose,
especially crushing or sieving.
If the sample has a dust-like consistency or contains (semi)-volatile compounds, part of it may be lost and this
may alter its physical-chemical properties.
8 Procedure
8.1 Sample conservation and pre-treatment
The laboratory samples shall be stored according to guidelines defined in Annex D.
Furthermore any possible source of contamination during the laboratory sample preparation according to
prCEN/TS 15443 (e.g. grinding with metallic apparatus, mainly aluminium or aluminium alloy) shall be avoided
or reduced as much as possible.
The laboratory sample should be stored and delivered in sealed high-density plastic containers.
8.2 Key concepts
Preparation of the test portion can be a complex process, because of a number of factors: sample type and its
physical state, amount of laboratory sample, type and number of determinations to be carried out etc. The
prepared test portions shall satisfy the following requirements at the same time:
 each test portion shall be a representative of the laboratory sample;
 the amount and the physical state (e.g. particle size) of each test portion have to comply with the
requirements of the respective analytical technique;
 for each test portion, no losses of and no contamination with respective analytes of interest should occur.
The preparation of the test portions from the laboratory sample, which has been taken according to the
sampling plan, is related to the requested analytical determinations. This means that, if needed, contact has to
be established among all involved parties such as the sampler, the customer and the analytical laboratory to
achieve the requirements of the standards to be used for the requested determinations.
The preparation of test portions in the laboratory will frequently involve a sequence of operations such as
homogenisation, fraction separation, drying, reducing particle size and sub sampling. Specific forms of these
operations are described in A.1 to A.5, respectively. A number of decisions on the specific order of these
operations for a particular laboratory sample have to be made. In some cases, the sequence of operations to
be applied is rather straightforward, but in more complicated cases (e.g. when several determinations with
different requirements have to be performed) it can be critical to choose the right sequence of such operations.
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CEN/TS 15413:2006 (E)
In order to define the operations to be applied to a laboratory sample to produce one or more representative
test portions, three main steps have to be considered:
 Definition of analytical requirements
First, the requirements of analytical procedures of interest shall be defined:
 what methods shall be used;
 how many test portions are necessary;
 the quantity and the properties of the test portions necessary for each analytical procedure;
 preservation requirements (e.g. time frame, temperature, addition of reagents).
NOTE 1 It is recommended to prepare at least five times the amounts needed as test portions for the test
sample.
 Definition of sequence of operations
Then, the sequence of operations shall be defined according to the flow sheet (Figure 1), based on
the properties of the laboratory sample and the requirements of the analytical procedures: each
single operation of this sequence has to be considered like an independent module; available
modules are:
 fraction separation;
 drying;
 particle size reduction;
 homogenisation;
 sub-sampling.
NOTE 2 For practical reasons it is recommended to group the parameters in a way that test samples with
similar requirements can be prepared for several parameters. The same test sample may be used for different
parameters if it fulfils the necessary requirements.
Frequently, different determinations have to be performed on the laboratory samples. In those cases,
modules have to be combined and/or repeated to obtain sub-samples, finally resulting in different test
portions. In order to define the actual sequence of operations to be applied to a given sample, the
flow sheet (Figure 1) shall be used.
 Choice of appropriate procedures
According to the requirements of the respective analytical techniques and the properties of the
sample the appropriate sample treatment technique has to be chosen within each module by
following the instructions of Annex A. Instructions are given in this annex in which case a particular
operation is appropriate to use.
8.3 Sequence of treatment techniques
The flow sheet in Figure 1 describes the procedure to enable decisions on the specific order of treatment
operations for a particular laboratory sample in order to yield in representative test portions. It shall be applied
on the starting laboratory sample and repeated on all sample fractions or sub-samples subsequently obtained
during the preparation, in an iterative cycle until all analytical requirements are fulfilled.
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CEN/TS 15413:2006 (E)
In the case of mercury determination special care shall be taken in order to avoid losses of these volatile
compounds during homogenisation and/or reduction of the particle size.
NOTE In special cases sub-sampling without a drying step will not lead to representative sub-samples.

Figure 1 — Flow sheet - sequence of operations
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CEN/TS 15413:2006 (E)
9 Quality control
Tests shall be carried out to detect possible contaminations from used apparatus
10 Performance characteristics
Data about performances of the methods will be available after validation in QUOVADIS project.
11 Test report
The test report shall contain at least the following information:
a) name, address and location of any laboratory involved in the preparation of the test portions;
b) description and identification of the laboratory sample;
c) date of receipt of laboratory sample and date(s) of performance of test;
d) a reference to this Technical Specification, i.e. CEN/TS 15413;
e) reference to the analytical standard used for the determination for each element;
f) the analytical results, referring to the relevant clause in the standard specified in e) ;
g) a reference to the sampling report;
h) the whole sequence and operating conditions (procedures and apparatuses) actually applied to the
laboratory sample for preparation of test portions;
i) any details not specified in this Technical Specification or which are optional, and any other factors which
may have affected the results;
j) unique identification of report (such as serial number) and of each page and total number of pages of the
report.
The laboratory should keep a trace of any analytical steps and intermediate results (chromatograms, raw data
and calculation details) that should be kept available in case of specific requirements.
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CEN/TS 15413:2006 (E)
Annex A
(normative)

Guideline for choosing sample treatment techniques
A.1 General
The preparation of test samples from a laboratory sample will frequently involve a sequence of operations
such as homogenisation, phase separation, drying, particle size reduction and sub-sampling. Specific forms of
these operations are described in this annex.
The sample treatment techniques prescribed in the analytical standards have to be fulfilled in any case.
A.2 Homogenisation
A.2.1 General information
Before each operation that implies sub-sampling, a homogenisation step is required, in order to guarantee that
all sub-samples or sample fractions have the same properties and composition. The homogenisation
technique to be used is chosen depending on the properties of the sample.
In many cases before homogenisation particle size reduction may be necessary.
A.2.2 Homogenisation techniques
A.2.2.1 Manual homogenisation
When to use it
 Generally usable;
 in cases when mechanical homogenisation could lead to loss of volatile compounds of interest (mercury).
When not to use it
 For samples that form layers because of the presence of particles of different density;
 for samples with particles of such a large size that homogenisation by manual mixing can not be reached;
 for samples that form layers because of the presence of particles with large differences in particle size.
Procedure
Mix the sample with an appropriate tool (e.g. shovel, pestle and mortar). If there is a risk of losses of volatile
substances the manual homogenisation has to be done very carefully.
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CEN/TS 15413:2006 (E)
A.2.2.2 Mechanical homogenisation
When to use it
 Generally usable especially in cases when manual homogenisation is not suitable;
 in cases of sample of large particle size;
 for solid samples containing particles of nearly the same density (e.g. for materials that don't form "layers"
after shaking).
When not to use it
 For samples that form layers because of the presence of particles of different density; in this case, if
homogenisation is not possible, separate and treat each layer as a different sample;
 when the apparatus may heat the sample and loss of volatile analytes can occur during this process; in
this case, a manual homogenisation shall be performed.
Procedure
Operate according to the manufactures instructions.
NOTE For sample of small particle size it may be also possible to use a ball-mill without balls for homogenisation.
A.2.3 Homogenisation in case of volatile compounds (mercury)
If mercury should be analysed, the sample homogenisation has to be done very carefully and quickly to avoid
losses. If losses cannot be avoided during the homogenisation process it may be a solution to take several
non-homogenised sub-samples for analyses and calculate the statistical mean as an estimate of the total
content. This step should not lead to major alterations of the composition and the representativity of the
remaining sample.
NOTE The sampling plan should consider the presence of volatile compounds.
A.3 Fraction separation
A.3.1 General information
For heterogeneous samples, depending on their nature and on the determinations of interest, one or more
techniques of fraction separation can be applied to obtain two or more different sub-samples that are to be
analysed separately. For samples consisting of different fractions, separation of some fractions may be
necessary. For this reason, the weight of each separated sub-sample shall be directly or indirectly measured
after the separation, in order to allow a final weighed combination of different fractions' analysis results.
The test report shall clearly state the technique(s) used for fraction separation, the weight and analytical
results related to all sub-samples obtained from fraction separation, as well as the “weighted” results.
A.3.2 Separation into different fractions
A.3.2.1 General
In cases of visible heterogeneity of separable fractions the separation of different fractions may be necessary,
especially if this can make subsequent particle size reduction, homogenisation and sub-sampling easier.
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CEN/TS 15413:2006 (E)
A.3.2.2 Manual separation
When to use it
 When several fractions can be distinguished;
 when non-crushable fractions (e.g. copper wire) exist.
When not to use it
 When contamination or losses of analytes of interest may occur.
Procedure
Manually select macroscopic pieces of different nature and store them in separate containers, either by hand
(with protective gloves) or by using appropriate tools (e.g. tweezers, magnet).
A.3.2.3 Sieving
When to use it
 When separation of fractions of different particle size is necessary;
 for checking the particle size of the sample or the particle size distribution.
When not to use it
 When contamination or losses of analytes of interest may occur.
Procedure
Sieve the sample by shaking either by hand or apparatus through sieves with appropriate mesh size and
material.
A.4 Drying
A.4.1 General information
Depending on the nature of the sample and the specific requirements of the test portion, a drying step might
be needed during sample treatment for test portion preparation. For the purpose of this Technical
Specification, drying is just used to remove the amount of water that could interfere with test portion
preparation (e.g. during crushing or milling). For the determination of water content a separate sub-sample
may be necessary.
Drying is very likely to introduce analytical errors for volatile compounds, and should be avoided when not
strictly required. If a sub-sample or test portion for volatile compounds determination is to be dried, the actual
drying technique shall be selected in order to minimise losses of volatile compounds. The test report shall
clearly state the technique(s) used for drying, along with the weight of sub-sample(s) before and after each
drying step.
It is likely that a certain drying technique is not applicable for all requested determinations. In such cases,
different sub-samples shall be dried in different ways, choosing the appropriate sequence of techniques for
each one.
The drying time will depend on the technique chosen, the thickness of the layer of the sample, the nature of
the sample, moisture content of the sample and of the air and the rate of ventilation.
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CEN/TS 15413:2006 (E)
The “grade of dryness” that shall be reached with the drying step depends on the subsequent treatments to be
applied to the sample. Typically, it is not necessary to wait until constant weight: e.g. the sample shall be just
dried enough to make crushing, grinding etc. possible.
A.4.2 Procedures
A.4.2.1 Air drying at room temperature
When to use it
 In every case where drying can be reached in appropriate time without alterations of analytes of interest;
 in case of mercury determination.
When not to use it
 When time is critical, and the properties of the sample do not allow a good drying in a reasonable time at
room temperature, and a higher temperature drying step can be safely applied.
Procedure
Spread the sample on the trays in a thin layer and allow it to get dry enough. Care shall be taken in order to
minimise possible contamination e.g. by dust. The use of a desiccator may accelerate the drying process for
small amounts of (sub-)samples.
A.4.2.2 Oven drying at 40 °C
When to use it
 When time is critical, and the properties of the
...