CEN/TS 16011:2013

SLOVENSKI STANDARD
01-maj-2014
Polimerni materiali - Reciklirani polimerni materiali - Priprava vzorcev
Plastics - Recycled plastics - Sample preparation
Kunststoffe - Kunststoff-Rezyklate - Probenvorbereitung
Plastiques - Plastiques recyclés - Préparation des échantillons
Ta slovenski standard je istoveten z: CEN/TS 16011:2013
ICS:
13.030.50 Recikliranje Recycling
83.080.01 Polimerni materiali na Plastics in general
splošno
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

TECHNICAL SPECIFICATION
CEN/TS 16011
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
January 2013
ICS 13.030.50; 83.080.01
English Version
Plastics - Recycled plastics - Sample preparation
Plastiques - Plastiques recyclés - Préparation des Kunststoffe - Kunststoff-Rezyklate - Probenvorbereitung
échantillons
This Technical Specification (CEN/TS) was approved by CEN on 22 October 2012 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

Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2013 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 16011:2013: E
worldwide for CEN national Members.

Contents Page
Foreword .3
Introduction .4
1 Scope .5
2 Normative references .5
3 Terms and definitions .5
4 Symbols and abbreviations .5
5 General requirements .5
6 Sampling .6
7 Methods .6
8 Precision of sample preparation .9
9 Bias in sample preparation .9
10 Packing and marking of samples . 10
Annex A (normative) Principles of sample preparation . 11
Annex B (informative) Sample preparation schemes . 21
Bibliography . 23

Foreword
This document (CEN/TS 16011:2013) has been prepared by Technical Committee CEN/TC 249 “Plastics”, the
secretariat of which is held by NBN.
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 Technical Specification is one part of a series of CEN publications on Plastics Recycling that is structured
as follows:
 EN 15342, Plastics — Recycled Plastics — Characterization of polystyrene (PS) recyclates
 EN 15343, Plastics — Recycled Plastics — Plastics recycling traceability and assessment of conformity
and recycled content
 EN 15344, Plastics — Recycled Plastics — Characterisation of Polyethylene (PE) recyclates
 EN 15345, Plastics — Recycled Plastics — Characterisation of Polypropylene (PP) recyclates
 EN 15346, Plastics — Recycled plastics — Characterisation of poly(vinyl chloride) (PVC) recyclates
 EN 15347, Plastics — Recycled Plastics — Characterisation of plastics wastes
 EN 15348, Plastics — Recycled plastic — Characterization of poly(ethylene terephthalate) (PET)
recyclates
 CEN/TR 15353, Plastics — Recycled Plastics — Guidelines for the development of standards for
recycled plastics
 CEN/TS 16010, Plastics — Recycled plastics — Sampling procedures for testing plastics waste and
recyclates
According to the CEN/CENELEC Internal Regulations, the national standards organisations of the following
countries are bound to announce this Technical Specification: 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
Recycling of plastics waste is one type of material recovery process intended to save resources (virgin raw
materials, water, energy), while minimising harmful emissions into air, water and soil as well as their impacts
on human health. The environmental impact of recycling should be assessed over the whole life cycle of the
recycling system (from the waste generation point to the disposal of final residues). To ensure that recycling
constitutes the best environmental option for treating the available waste, some prerequisites should
preferably be met:
 the recycling scheme being contemplated should generate lower environmental impacts than alternative
recovery options;
 existing or potential market outlets should be identified that will secure a sustainable industrial recycling
operation;
 the collection and sorting schemes should be properly designed to deliver recyclable plastics waste
fractions fitting reasonably well with the available recycling technologies and with the (changing) needs of
the identified market outlets, preferably at minimum costs for society.
This Technical Specification has been produced in accordance with the guidance produced by CEN on
Environmental Aspects and in accordance with CEN/TR 15353, Plastics — Recycled Plastics — Guidelines
for the development of standards for recycled plastics.
NOTE CEN/TR 15353 considers the general environmental aspects which are specific to the recycling process.
The purpose of this Technical Specification is to define the procedures to be followed to prepare samples
taken in accordance with CEN/TS 16010 in readiness for testing various material characteristics as set out in
other relevant standards for recycled plastics (EN 15342 to EN 15348).
It is not the intention of this Technical Specification to develop new sample preparation methods.

1 Scope
This Technical Specification specifies the preparation of samples of recycled plastics prior to testing and takes
account of the specifics of the material.
Sample preparation should avoid any process that causes 'de-mixing' of the sample. Following preparation,
the sample should remain representative.
The behaviour of contaminants should be carefully analysed and observed to ensure this is homogeneous.
This Technical Specification does not address any legal or product safety issues.
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.
CEN/TR 15353:2007, Plastics — Recycled plastics — Guidelines for the development of standards for
recycled plastics
CEN/TS 16010, Plastics — Recycled plastics — Sampling procedures for testing plastics waste and
recyclates
EN ISO 472:2001, Plastics — Vocabulary (ISO 472:1999)
ISO 3085, Iron ores — Experimental methods for checking the precision of sampling, sample preparation and
measurement
ISO 3086, Iron ores — Experimental methods for checking the bias of sampling
ISO 11648-1, Statistical aspects of sampling from bulk materials — Part 1: General principles
ISO 11648-2:2001, Statistical aspects of sampling from bulk materials — Part 2: Sampling of particulate
materials
ISO 13909-7, Hard coal and coke — Mechanical sampling — Part 7: Methods for determining the precision of
sampling, sample preparation and testing
ISO 13909-8, Hard coal and coke — Mechanical sampling — Part 8: Methods of testing for bias
3 Terms and definitions
For the purposes of this document, the terms, definitions and abbreviated terms given in EN ISO 472:2001, in
CEN/TR 15353:2007 apply.
4 Symbols and abbreviations
C coefficient of variation
v
5 General requirements
5.1 Implementation
Successful implementation of this Technical Specification depends on effective communication between the
data user, the sampler and test laboratory. The aim is to close the information chain of the whole processes
around the sampling in combination with the laboratory analysis.
NOTE The data user could be the supplier, purchaser or a third party.
5.2 Instructions
The appropriate instructions for sampling, sample preparation and testing shall be reviewed by all those
involved in the sampling and testing process. If there are no instructions, the test laboratory should contact the
data user.
5.3 Storage
Samples should be collected in appropriate containers for the tests required. The storage conditions shall
ensure that the sample characteristics do not change.
5.4 Documentation
The whole sampling and sub-sampling process shall be documented with all relevant facts recorded. It is also
useful to record the apparatus used and their calibration details.
5.5 Sample preparation rooms
All sample preparations shall be done in rooms or at places which do not influence the samples, or where the
influence is negligible. All these areas shall be free from contamination, be easily decontaminated and be
vented to control dust and remove fumes. It is good laboratory practice to avoid unnecessary flame, heat and
fume.
5.6 Volatiles
If volatiles and non-volatiles are to be determined, then precautions shall be taken to ensure that the volatiles
are not able to escape during the sampling and sample preparation process.
6 Sampling
Take the sample in accordance with CEN/TS 16010.
7 Methods
7.1 General
The general principles of sample preparation are described in Annex A and ISO 11648-2.
7.2 Determination of the minimum laboratory sample
The determination of the minimum laboratory sample is dependent on the characteristics and properties to be
tested. It should be noted that the minimum mass of the laboratory analysis sample increases with the
maximum grain size or mass of the individual particle of the sample.
In Table 1 the relationship is given between the maximum particle size and sample mass to achieve a different
fundamental error with 15 %, 10 % and 5 %. The determination of this minimum value is dependent on the
maximum mass/particle size of the material being analysed, the required measurement tolerance and the
statistical probability value with which the result is correlated. If no information is available, the minimum value
of the laboratory sample should be determined by Table 1. Note the different coefficients of variation C .
v
Samples for the determination of moisture should be a minimum of 1 kg, see 7.5.2.
Table 1 — Minimum value of the laboratory sample
Required minimum Maximum Maximum Maximum Sieve size
mass of the allowable particle allowable particle allowable particle (ISO 565)
a a a
laboratory sample size size size
g cm cm cm
C < 15 % C < 10 % C < 5 %
v v v
0,1 0,05 0,04 0,03 500 µm
1 0,10 0,08 0,06 1,0 mm
2 0,13 0,10 0,08 1,4 mm
5 0,17 0,13 0,10 1,7 mm
10 0,21 0,16 0,13 2,0 mm
30 0,31 0,24 0,19 2,8 mm
50 0,37 0,28 0,22 3,35 mm
100 0,46 0,35 0,28 4,0 mm
a
The particle size is dependent on the maximum linear dimension of the particle. It is the determined effective

.
size or size distribution of particles, mostly done by manual or automatic sieves.

7.3 Homogenisation of samples
Suitable equipment for sample homogenisation and division are the riffle splitter or the sectorial splitter.
7.4 Sample preparation before mechanical testing
The preparation of samples before mechanical testing is dependent on the physical form of the material.
Usually the aim is to produce a moulded part prior to mechanical testing. For flakes and agglomerates then
additional granulation (size reduction) might be required before moulding. If the sample is in the form of a
compound and information is available on the melt filtration used, then additional granulation might be
unnecessary. See Table 2.
Table 2 — Sample preparation before mechanical testing
Powder Flake Agglomerate Compound Moulded part
shredding
granulation granulation granulation granulation
(optional) (optional) (optional) (optional)
moulding moulding moulding moulding moulding
testing testing testing testing testing

7.5 Preparation of samples for the determination of moisture
7.5.1 Sample Type
The sample to be tested shall be either:
a) a sample collected exclusively for the determination of moisture; or
b) a sample on which determinations of moisture and other quality characteristics are required.
7.5.2 Mass
The mass of each moisture sample shall not be less than 1 kg. Recommended masses of samples at various
nominal maximum particle sizes are given in Table 3 (taken from ISO 11648-2:2001). Samples of nominal
maximum particle size greater than 22,4 mm may be subjected to a two-stage drying procedure, as described
in Annex A.4.1 b).
Table 3 — Example of recommended minimum mass
of sample for the determination of moisture
Maximum
Nominal
allowable
Maximum
maximum Accuracy of Minimum
difference
layer
particle size weighing drying time
Minimum mass between
thickness
of material
subsequent
weightings of
dried samples
mm mm kg g g h
63,0 70 110 110 10 16
45,0 50 40 40 4 12
31,5 35 14 14 1 8
22,4 25 5 5 0,5 6
16,0 20 2 2 0,2 4
11,2 13 1 1 0,1 4
7.5.3 Precautions against loss of moisture
One of the main difficulties in determining moisture is that of minimising changes in the moisture content of the
sample when preparing the moisture sample. Take every precaution to minimise changes in moisture content
due to unsuitable containers and by evaporation during handling, particularly if the bulk material is extremely
wet. Keep all moisture samples in sealed containers in a cool place and out of direct sunlight before and after
preparation as well as during any interval between stages of sample preparation.
Take care to minimise changes in moisture content during particle size reduction, by using equipment in which
there is no appreciable heating, and by reducing the amount of air passing through the mill to a minimum.
Take care to minimise changes in moisture content when carrying out sample division; carry out such
operations as quickly as possible. In some circumstances, it might be necessary to carry out moisture
determinations on each increment, to minimise moisture changes (see Annex B).
Where moisture samples are to be retained for any length of time; for example for more than five to seven
days in the case of umpire and shipping samples, place them into moisture-impervious plastic bags which are
sealed so as to minimise free air space. Then store them in an airtight container.
7.5.4 Samples for determination of moisture
Moisture in bulk material may be determined by heating a sample of material at 105 °C in air until constant
mass is achieved.
Preparation of the sample may include preliminary air-drying (see A.3) if the material is visibly wet.
7.6 Preparation of samples for chemical analysis
7.6.1 General
The procedure for preparation of the chemical analysis sample is described in 7.5.2 and shown schematically
in Annex B. The moisture sample may be used as the chemical analysis sample after drying, provided it is
sufficiently representative.
7.6.2 First stage in the preparation
If necessary, the sample may be dried in accordance with A.3. Pass the whole sample through the size
reduction equipment (see A.4), mix it, then divide it (see A.6) to decrease the mass to the value appropriate to
the nominal maximum particle size of the size reduced bulk material (see A.2).
7.6.3 Further stages in the preparation
In the further stages of preparation, reduce the particle size of the portion retained from the first stage to the
required nominal maximum particle size for analysis (see A.4), then divide it to obtain as many samples as
contractually required, each having a recommended mass of no less than 50 g.
Then place the chemical analysis sample in a sealed container and label it with all necessary identification
details.
8 Precision of sample preparation
Check the precision of sample preparation periodically and whenever a new scheme is brought into operation.
Test procedures for the determination of precision in sample preparation are given in ISO 3085 and
ISO 13909-7 and these procedures may be applied to other bulk materials.
9 Bias in sample preparation
9.1 General
Check the bias in sample preparation periodically and whenever a new scheme is brought into operation.
Procedures for checking bias in sample preparation are given in ISO 3086 and ISO 13909-8 and these
procedures may be applied to other bulk materials.
Contamination is often a major source of bias during sample preparation. Contamination might be attributable
to preparation equipment or cross-contamination.
9.2 Cross-contamination
Potential causes of cross-contamination include the following:
a) Dust: Dust settling on open samples can be a possible cause of contamination. Minimise dust settling by
ensuring as much work as possible is carried out using a dust extraction system. If possible, any dust
escaping from size reduction equipment should be extracted downwards and to the rear. Keep all ducting,
machinery and floors clean.
b) Sample: To prevent cross-contamination, clean all equipment used between samples, ensuring that the
sample has been removed first.
10 Packing and marking of samples
The samples for distribution shall be tightly sealed in air-tight containers. The label, and a card placed in the
container, shall contain the following particulars:
a) the type of recycled plastic and the name of the lot (e.g. lot reference number);
b) the mass of the lot;
c) the sample reference number;
d) the place and the date of sampling;
e) the moisture content of the sample (if known);
f) the place and the date of sample preparation;
g) the particle size of the sample;
h) any other consideration (if necessary), for example any special purpose or test for which the sample is
taken.
Annex A
(normative)
Principles of sample preparation
A.1 General
Sample preparation involves several distinct operations, which are sometimes preceded by drying. These are
as follows:
a) reduction, i.e. to decrease the particle size by crushing, grinding, or pulverisation;
b) mixing;
c) division, i.e. to decrease the sample mass by dividing the sample into two or more parts.
These operations are generally considered to constitute one stage of sample preparation.
As a general rule, reduction should always precede division. An exception occurs where high capacity
streams are being sampled mechanically; it is then permissible to divide large primary increments, as
specified in ISO 11648-2:2001, Clause 10.
The stages
...