SIST EN 14243-2:2019
(Main)Materials obtained from end of life tyres - Part 2: Granulates and powders - Methods for determining their dimension(s) and impurities, including free steel and free textile content
Materials obtained from end of life tyres - Part 2: Granulates and powders - Methods for determining their dimension(s) and impurities, including free steel and free textile content
This European Standard provides test methods for the determination of the dimension(s) of granulates and powders, produced from all categories of end-of-life tires at all steps of the treatment processes as well as for the determination of impurities (including free steel and free textile content).
The methods described in this Standard include sample collection and the preparation of a representative sample based on a sampling plan for the purpose of determining dimensions and impurities.
This Standard does not cover the operational performance or fitness for use of the materials which is deemed to be a function of the agreement between manufacturer and customer.
This Standard does not purport to address all of the safety concerns, if any, associated with its use. This standard does not establish appropriate safety and health practices and does not determine the applicability of regulatory limitations prior to use.
Materialien aus Altreifen - Teil 2: Granulate und Pulver - Methode zur Bestimmung der Abmessungen und Verunreinigungen einschließlich freier Stahl, freie Textilien und andere Verunreinigungen
Diese Europäische Norm enthält Prüfverfahren zur Bestimmung der Abmessung(en) von Granulaten und Gummimehlen, die aus allen Kategorien von Altreifen in allen Stufen der Behandlungsprozesse hergestellt werden sowie zur Bestimmung von Verunreinigungen (einschließlich freiem Stahl und Anteil an freiem Textil).
Die in dieser Norm beschriebenen Verfahren enthalten die Probesammlung und die Vorbereitung einer repräsentativen Probe auf Basis eines Probenahmeplans, um die Abmessungen und Verunreinigungen zu bestimmen.
Diese Norm gilt nicht für die Betriebsleistung oder Gebrauchstauglichkeit der Materialien, die als eine Funktion von Vereinbarungen zwischen dem Hersteller und dem Kunden gelten.
Diese Norm enthält nicht die Absicht, alle mit ihrer Verwendung verbundenen Sicherheitsbedenken zu berücksichtigen. Diese Norm legt keine angemessenen Sicherheits- und Gesundheitspraktiken fest und bestimmt nicht die Anwendbarkeit von behördlichen Einschränkungen vor der Verwendung.
Matériaux produits à partir de pneus usagés non réutilisables (PUNR) - Partie 2 : Granulats et poudrettes - Méthodes de détermination de leur(s) dimension(s) et impuretés, y compris la teneur en fils métalliques et en fibres textiles libres
La présente Norme européenne fournit des méthodes d’essai pour la détermination de la (des) dimension(s) des granulats et poudrettes produits à partir de toutes les catégories de pneus usagés non réutilisables (PUNR) à toutes les étapes des procédés de traitement ainsi que pour la détermination d’impuretés (y compris le taux d’acier libre et le taux de textile libre).
Les méthodes décrites dans la présente norme comprennent la collecte de l’échantillon et la préparation d’un échantillon représentatif sur la base d’un plan d’échantillonnage afin de déterminer des dimensions et des impuretés.
La présente norme ne couvre pas les performances opérationnelles ou l’aptitude à l’emploi des matériaux, considérées dans le cadre de l’accord passé entre le fabricant et le client.
La présente norme ne traite pas de tous les problèmes de sécurité, s’ils existent, associés à son utilisation. La présente norme n’établit pas de bonnes pratiques en matière de sécurité et d’hygiène et ne détermine pas l’applicabilité des limitations réglementaires avant utilisation.
Snovi iz izrabljenih avtomobilskih gum - 2. del: Granulati in praški - Metode za ugotavljanje njihovih mer in nečistoč, vključno z jeklenimi in tekstilnimi delci
Ta evropski standard določa preskusne metode za določanje mer granulatov in praškov, proizvedenih iz vseh kategorij izrabljenih avtomobilskih gum v vseh korakih procesov obdelave ter tudi za določanje nečistoč (vključno z jeklenimi in tekstilnimi delci).
Metode, opisane v tem standardu, zajemajo jemanje vzorcev in pripravo reprezentativnega vzorca na podlagi načrta vzorčenja za namene določanja mer ter nečistoč.
Ta standard ne zajema operativnega delovanja ali primernosti za uporabo materialov, za katere se šteje, da so predmet dogovora med proizvajalcem in stranko.
Ta standard ne obravnava vseh morebitnih varnostnih težav, ki se nanašajo na njegovo uporabo. Ta standard ne vzpostavlja ustreznih varnostnih in zdravstvenih praks ter ne določa uporabnosti regulativnih omejitev pred uporabo.
General Information
Relations
Standards Content (Sample)
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Materialien aus Altreifen - Teil 2: Granulate und Pulver - Methode zur Bestimmung der Abmessungen und Verunreinigungen einschließlich freier Stahl, freie Textilien und andere VerunreinigungenMatériaux produits à partir de pneus usagés non réutilisables (PUNR) - Partie 2 : Granulats et poudrettes - Méthodes de détermination de leur(s) dimension(s) et impuretés, y compris la teneur en fils métalliques et en fibres textiles libresMaterials obtained from end of life tyres - Part 2: Granulates and powders - Methods for determining their dimension(s) and impurities, including free steel and free textile content83.160.01Avtomobilske pnevmatike na splošnoTyres in general13.030.50RecikliranjeRecyclingICS:Ta slovenski standard je istoveten z:EN 14243-2:2019SIST EN 14243-2:2019en,fr,de01-april-2019SIST EN 14243-2:2019SLOVENSKI
STANDARDSIST-TS CEN/TS 14243:20101DGRPHãþD
SIST EN 14243-2:2019
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN 14243-2
February
t r s { English Version
Materials obtained from end of life tyres æ Part
tã Granulates and powders æ Methods for determining the particle size distribution and impuritiesá including free steel and free textile content Matériaux produits à partir de pneus usagés non æ Méthodes de détermination de la distribution granulométrique et des impuretésá y compris la teneur en fils métalliques et en fibres textiles libres
This European Standard was approved by CEN on
s { November
t r s zä
egulations which stipulate the conditions for giving this European Standard the status of a national standard without any alterationä Upætoædate lists and bibliographical references concerning such national standards may be obtained on application to the CENæCENELEC Management Centre or to any CEN memberä
translation under the responsibility of a CEN member into its own language and notified to the CENæCENELEC Management Centre has the same status as the official versionsä
CEN members are the national standards bodies of Austriaá Belgiumá Bulgariaá Croatiaá Cyprusá Czech Republicá Denmarká Estoniaá Finlandá Former Yugoslav Republic of Macedoniaá Franceá Germanyá Greeceá Hungaryá Icelandá Irelandá Italyá Latviaá Lithuaniaá Luxembourgá Maltaá Netherlandsá Norwayá Polandá Portugalá Romaniaá Serbiaá Slovakiaá Sloveniaá Spainá Swedená Switzerlandá Turkey and United Kingdomä
EUROPEAN COMMITTEE FOR STANDARDIZATION COMITÉ EUROPÉEN DE NORMALISATION EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre:
Rue de la Science 23,
B-1040 Brussels
9
t r s { CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Membersä Refä Noä EN
s v t v uæ tã t r s { ESIST EN 14243-2:2019
EN 14243-2:2019 (E) 2
Contents Page European foreword . 4 Introduction . 5 1 Scope . 6 2 Normative references . 6 3 Terms and definitions . 6 4 Categories of products obtained from end-of-life tyres based mainly on their dimensions and particle size distribution . 6 5 Determination of particle size distribution for granulates and powders . 7 Annex A (normative)
Determination of free steel content for granulates and powders by the method of magnetic separation . 17 A.1 General. 17 A.2 Principle of determination . 17 A.3 Sampling . 17 A.4 Equipment . 17 A.5 Procedure . 18 A.6 Calculation . 19 A.7 Metrological characteristics . 19 A.8 Test report . 19 Annex B (normative)
Determination of free textile content for granulates and powders by the method of the "small ball" agglomeration . 20 B.1 General. 20 B.2 Principle of the determination . 20 B.3 Sampling . 20 B.4 Equipment . 20 B.5 Procedure . 20 B.6 Calculations . 21 B.7 Metrological characteristics . 21 B.8 Test report . 21 Annex C (normative)
Determination of other impurities for granulates and powders by the method of a saline solution . 22 C.1 General. 22 C.2 Principle of the determination . 22 C.3 Sampling . 22 SIST EN 14243-2:2019
EN 14243-2:2019 (E) 3
C.4 Equipment and Reagents . 22 C.5 Procedure . 23 C.6 Calculations . 24 C.7 Metrological characteristics . 25 C.8 Test report . 25 Annex D (informative)
Example of separatory funnel . 26 Annex E (informative)
Sieving . 27 Annex F (informative)
Recommended sieve list. 28 Bibliography . 29
SIST EN 14243-2:2019
EN 14243-2:2019 (E) 4
European foreword This document (EN 14243-2:2019) has been prepared by Technical Committee CEN/TC 366 “Materials obtained from End-of-Life Tyres (ELT)”, the secretariat of which is held by UNI. 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 August 2019, and conflicting national standards shall be withdrawn at the latest by August 2019. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN shall not be held responsible for identifying any or all such patent rights. This document together with EN 14243-1 and EN 14243-3 supersede CEN/TS 14243:2010. EN 14243, Materials obtained from End-of-Life Tyres (ELTs), consists of the following parts: — Part 1: General definitions related to the methods for determining their dimension(s) and impurities — Part 2: Granulates and powders – Methods for determining the particle size distribution and impurities including free steel and free textile content — Part 3: Shreds cuts and chips – Methods for determining their dimension(s) including protruding filaments dimensions According to the CEN-CENELEC Internal Regulations, the national standards organisations 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, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom. SIST EN 14243-2:2019
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Introduction This standard is used in conjunction with the other parts of EN 14243 series. Such series is intended to cover the testing programs needed to characterize each product category as shown on the figure below.
Figure 1 — Typical scheme for a testing programme concerning several characteristics with testing steps in the field and in the laboratory End-of-life tyres consist mainly of passenger and commercial vehicle tyres, truck, earthmover and agricultural tyres manufactured for distribution in the European market that are no longer suitable for their original purpose. Products from end-of-life tyres are used as a secondary raw material finding a wide range of applications. The principal categories of materials from end-of-life tyres are defined on the basis of their dimension(s) according to EN 14243-1. SIST EN 14243-2:2019
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1 Scope This standard provides test methods for the determination of the particle size distribution of granulates and powders, produced from all categories of end-of-life tyres at all steps of the treatment processes as well as for the determination of impurities (including free steel and free textile content). The methods described in this standard include sample collection and the preparation of a representative sample based on a sampling plan for the purpose of determining particle size distribution and impurities. 2 Normative references The following documents are referred to in the text in such a way that some or all of their content constitutes requirements of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. EN 14243-1:2019, Materials obtained from end of life tyres — Part 1: General definitions related to the methods for determining their dimension(s) and impurities EN 933-1, Tests for geometrical properties of aggregates — Part 1: Determination of particle size distribution — Sieving method EN 933-2, Tests for geometrical properties of aggregates — Part 2: Determination of particle size distribution — Test sieves, nominal size of apertures CEN/TS 17188, Materials obtained from end of life tyres — Sampling method for granulates and powders stored in big-bags ISO 565, Test sieves — Metal wire cloth, perforated metal plate and electroformed sheet — Nominal sizes of openings ISO 3310-1:2016, Test sieves — Technical requirements and testing — Part 1: Test sieves of metal wire cloth ISO 3310-2:2013, Test sieves — Technical requirements and testing — Part 2: Test sieves of perforated metal plate 3 Terms and definitions For the purposes of this document, the terms and definitions given in EN 14243-1:2019 apply. ISO and IEC maintain terminological databases for use in standardization at the following addresses:
IEC Electropedia: available at http://www.electropedia.org/
ISO Online browsing platform: available at http://www.iso.org/obp 4 Categories of products obtained from end-of-life tyres based mainly on their dimensions and particle size distribution For categories and testing program, refer to EN 14243-1:2019, Clause 4. SIST EN 14243-2:2019
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5 Determination of particle size distribution for granulates and powders 5.1 General Particle size and related parameters are key measurements for product classification of size-reduced materials such as granulates and powders. Particle size analysis is the first measurement of consistency and forms the basis for material grading. Before being able to obtain an accurate particle size distribution, a representative sample of the material to be tested shall be taken. Depending on the agreed testing program between the producer and the customer, or on the producer's own will, the determination of particle size distribution specified in this clause for granulates and powders may be followed by the additional determination(s) of the free steel content and/or the free textile content and/or the other impurities as specified in Annexes A, B and C. 5.2
Sampling plan 5.2.1 Principles of sampling The main principle of sampling is to obtain a representative sample(s) from a lot of material from which a characteristic is to be determined. If the lot is to be represented by a sample, then every particle in the lot shall have an equal probability of being included in the sample (i.e. probabilistic sampling). When these principles cannot be applied in practice, the sampler shall define a procedure as close as possible to probabilistic sampling in his judgement (i.e. judgemental sampling) and note the limitations in the sampling plan and sampling report. Obtaining samples that are truly representative of the material produced is easier when the material is moving (for example on a conveyor belt). Therefore, sampling from moving material is to be preferred wherever possible. For granulates and powders stored in big-bags a sampling method is described in CEN/TS 17188. NOTE The determination of properties other than particle size distribution may result in different sampling requirements. This is the case for the determination of physical properties (such as bulk density) or chemical composition. 5.2.2 Preparation of the sampling plan A sampling plan shall be prepared before samples are taken through a specific definition of the lot size and the size and number of increments to be taken. 5.2.3 Definition of lot size The lot size shall be defined by the producer in accordance with requested specifications and is a fixed quantity for which a characteristic is to be determined. The lot size mlot may be defined by the producer as:
a fixed quantity produced between changes in the process settings that could affect the product specifications
a fixed quantity in a production day/shift
a fixed quantity minimum of 100 t (10 t for powders). The lot size is based on production quality management decisions or specific customer requirements. SIST EN 14243-2:2019
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5.2.4 Sampling point and apparatus Based on health and safety assessments and producer equipment, a fixed sampling point for the collection of sample increments shall be chosen for each material fraction to be monitored. Sampling shall be carried out using a sample box or other suitable equipment. The sampling box is passed through the stream of falling material so that it uniformly cuts the full flow of falling material. The box shall be large enough so that it does not become overloaded. Automatic systems fulfilling these criteria may also be used. 5.2.5 Size of a sample increment The sampling box shall have a capacity of not less than: Vmin = 0,5 dm3 for d < 10 Vmin = 0,05 × d
for
s r
¶ d
¶
t r where Vmin is the minimum capacity of the sampling box (in cubic decimetres); d is the nominal top size in millimetres;
The sampling operator shall record the approximate capacity of the sampling device Vincrement (in cubic decimetres). 5.2.6 Number of increments The minimum number of increments to be taken from a lot depends on the nominal top size of the material to be sampled. The material shall be assigned by the sampler to one of two groups in Table 1. Table 1 — Classification of material according to size Group 1 Group 2 nominal top size < 10 mm nominal top size between 10 mm and 20 mm For sampling from moving material: Group 1: n = 3 + 0,025 × mlot (size of granulates from 0,8 mm to 10 mm and powders under 0,8 mm) Group 2: n = 5 + 0,040 × mlot (size of granulates from 10 mm to 20 mm) where n is the minimum permitted number of increments rounded off to the higher nearest whole number mlot is the mass of the lot in tonnes.
Sample collection is carried out according to the sample plan and the increments are collected manually using the sampling box. Increments shall be taken at regular intervals during the production of the lot in accordance with the sampling plan. The time of increment collection is recorded in the sampling plan. Each increment taken from the lot is placed in the sampling container and at the end of the process, it constitutes the combined sample which is sent to a laboratory as laboratory sample. In case more than one laboratory sample is required, they shall be prepared in the plant in accordance with the principles of sample division of 5.4.2. SIST EN 14243-2:2019
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5.2.7 Visual assessment The increments shall be assessed visually and observations on the quality should be noted as additional information and recorded according to quality management, best practice policies or specific customer requirements. 5.2.8 Sampling certificate The sampling certificate shall include at least the following information: a) the name of the producer; b) kind of material: powder or granulate; c) a unique identification number of the sample; d) the name of the sampler; e) the location(s), date and time of sampling; f) Collection point of the material: 1) production with the additional information: — nominal top size — definition and mass of the lot size — a unique identification number of the lot — sampling point — number, time and volume of increments — V increment 2) big bag (sampling according to CEN/TS 17188); g) weight of the combined sample sent to laboratory; h) reference to this standard; i) any deviation from this standard. 5.3 Storage and transport of laboratory sample(s) Samples are to be stored in such a way that material will not be lost during transportation. The samples are to be stored dry and in a sealed sample box. The sampling certificate shall be attached. SIST EN 14243-2:2019
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5.4 Preparation of the laboratory sample(s) and test portion(s) 5.4.1 Principles of correct sample preparation and sample division The main purpose of sample preparation is that the laboratory sample collected from the whole lot are reduced to one or more test samples based on sample division. The aim of sample division is therefore to homogenize and reduce the mass of the laboratory sample to make several duplicate test samples. Each test sample shall be representative of the original sample based on the principle that the composition of the sample as taken on site shall not be changed during the steps of sample preparation for testing. 5.4.2 Test sample and test portion preparation The increments that have been collected are mixed together in a container of suitable size to form a combined sample. In this case the combined sample is the laboratory sample. The laboratory sample may need to be reduced to a test sample before a test portion is produced. The test sample(s) or directly the laboratory sample shall be reduced to a suitable size in order to obtain test portion(s) in such a way that sufficient material is still provided for all the tests to be performed. In particular, the calculation shall take into account the need for duplicate test portions, for extra material in case dubious results are obtained and the need for sampling with replacement. The sampling plan shall take into account such requirements. The test sample(s) (or directly the laboratory sample) shall be reduced using the principles of sample division using either: — a riffle splitter; — a rotary sample divider, or — other equivalent device. 5.4.3 Apparatus for sample division The most relevant sample division methods are based on the following apparatus: a) Riffle splitter: a sample splitter shall have at least 12 slots and an even number with adjacent slots directing material into two different sub-samples. The width of the slots shall be at least three times the nominal top size of the material to be riffled to prevent sample bridging. SIST EN 14243-2:2019
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Figure 2 — Example of a riffle box b) Rotary sample divider: a rotary sample divider shall be used according to its manufacturer's manual. The inner dimensions of the equipment where the sample is fed shall be at least three times as wide as the nominal top size to be processed. 5.4.4 Procedure The combined sample is mixed with a scoop and sent through the sample divider until the sample reduction is complete. A final mass quantity is prepared for the purposes of particle size analysis depending on the size of the sieving system in order to fulfil the non-overloading criteria given in 5.5.6. 5.5 Particle size analysis 5.5.1 General principles A sample is subjected to mechanical sieving through a set of oscillating sieves, sorting the particles in decreasing size classes by mechanical means. All apparatus shall conform to the general requirements of EN 933-1, EN 933-2, ISO 565, ISO 3310-1 and ISO 3310-2. The sample shall be completely dry before particle size analysis. 5.5.2 Sieves For the sieve analysis, an appropriate number of sieves is required and shall be chosen according to the size specification of the sample to be tested. The geometry of the apertures shall be either circular or square, the thickness of the sieves, the distances of the holes and the diameter of the holes shall be in accordance with ISO 3310-1 and/or ISO 3310-2. The frame of the sieves shall have a height that enables the sieves to contain the samples and allow for the free movement of the sample during the sieving process. The number of sieves that are used may vary according to the particle size distribution that is to be determined. When choosing sieves for performing the analysis the supplementary row R 20 from ISO 3310-1:2016 and/or ISO 3310-2:2013 shall be preferred. It is not permitted to jump between principal and supplementary rows within a series. Annex F reports a list of square apertures commonly used for dimensional determination of granulates and powders. SIST EN 14243-2:2019
EN 14243-2:2019 (E) 12
5.5.3 Flat brush A flat brush is required for cleaning the sieves. 5.5.4 Mechanical vibrating equipment A mechanical device that applies a 3-dimentional vibrating movement is to be used. The equipment shall have a timer and amplitude settings. The amplitude shall be set at 1,5 mm. 5.5.5 Scales Scales capable of measuring the mass of the sample to be sieved to the nearest 0,1 g. 5.5.6 Procedure Assemble and operate the mechanical shaking device with the appropriate sieve sizes with decreasing aperture size ending with the collecting pan. The quantity of sample to be used depends primarily on the maximum particle size, the number of sieves in the sieve stack and their openings. The sieves shall not be overloaded. Criteria for not overloading are given in Annex E. The initial sieve should be loaded with a quantity of material as close as possible to 0,3 g/cm2 for powders and 0,5 g/cm2 for granulates. Therefore, for the purpose of this standard, 200 mm sieves are recommended with a sample mass as close as possible to 100 g for powders and 150 g for granulates. If 315 mm sieves are used, the sample mass is as close as possible to 250 g for powders and 350 g for granulates. NOTE 1 For powders having a nominal dimension smaller than 250 µm it is advised to split the test portion in sub-portions to be sieved separately. Fractions retained on each sieve are gathered and weighted. Then they are expressed as percentage of the total test portion. In case of moist samples, drying shall be performed by placing the sample inside an oven of circulating air at a temperature of (60 ± 2) °C until constant weight is reached. Wait until room temperature is reached. The particle size analysis shall not be performed before 30 min after the extraction of the sample from the oven. Before sieving starts, the mass of all individual sieves shall be measured on the scales used for determination of sieving fractions. The mass of each sieve i shall be recorded as msi. Weigh the sample to the nearest 0,1 g. For the following calculations the mass of the sample will be defined m0. Spread the test sample in an even layer on the top sieve. Using a brush, remove all traces from the sample box. Secure the cover plate (lid) and begin the sieving operation. The duration of the sieving operation for granulates and powders is fixed at: — 12 min ± 15 s; Weigh each sieve together with the retained net material and the material in the collecting pan with an accuracy of 0,1 g and record the masses as expressed in 5.5.7. NOTE 2 It is advised to avoid the loss of particles from the screens. If a particle sticks in a sieving hole, it is suggested to remove it and add it to the fraction which remained on the sieve (as it did not pass the hole). SIST EN 14243-2:2019
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5.5.7 Calculation Weigh each sieve and record the various masses on a test data sheet alongside the corresponding sieve size. The mass of the empty sieve i plus the material retained on it is mssi. The mass mi of the material retained on each sieve i shall be calculated according to the following formula: mi=mssi-msi After calculating all the masses from each sieve, calculate the total mass collected (mt): mt ± Ãmi Calculate the difference between m0 and mt in terms of percentage according to following formula: Total deviation (%) = 100-|(mt/m0) x 100| If there is more than a 1 % difference between the total mass of the test sample m0 and the sum of the masses mi of all the fractions mt then the test shall be repeated. Calculate the cumulative percentage of mi passing each sieve, to the nearest decimal point, by adding in each step the mass in percentage of the corresponding sieve. The percentage on each sieve is calculated according to formula: mi(%)=(mi/m0) x 100 5.5.8 Graphical representation After calculation a graphical representation of the results shall be made. Both the percentage of the mass retained on each sieve and the percentage of the mass passing through it shall be plotted as a function of the aperture size of the sieve, expressed in millimetres (mm) for sizes of 1 mm and above and in microns
From the plot of the mass passing through each sieve, it is possible to determine by linear interpolation at which aperture size the passing percentage is 90 % and take this as the upper limit of the dimension of the granulate or powder under analysis. Likewise, for granulates it is possible to determine the aperture size at which the passing percentage is 10 % and take this as the lower limit. The two limits are a typical measure of the particle size distribution of the material. A granulate is characterised by its nominal dimensions (agreed between producer and customer). In a compliance testing of the particle size distribution of a sample, the nominal upper dimension shall be not smaller than the upper limit, and the nominal lower dimension shall not be higher than the lower limit. For a powder only the upper values shall be considered. Hereafter an example of graphical representation is given. It relates to the results of a particle size analysis made on a granulate sample, obtained from a production lot having nominal dimensions 1,4 – 4,0 mm. For the test eight sieves have been used. For each sieve aperture, the material retained on it and that passing through it are reported in percentage in the following table: SIST EN 14243-2:2019
EN 14243-2:2019 (E) 14
Table 2 — Material retained on the sieve and passing through the sieve I II R C bottom 1 0,5 % 0,5 %
...
SLOVENSKI STANDARD
oSIST prEN 14243-2:2018
01-februar-2018
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Materials obtained from end of life tyres - Part 2: Granulates and powders - Methods for
determining their dimension(s) and impurities, including free steel and free textile content
Materialien aus Altreifen - Teil 2: Granulate und Pulver - Methode zur Bestimmung der
Abmessungen und Verunreinigungen einschließlich freier Stahl, freie Textilien und
andere Verunreinigungen
Matériaux produits à partir de pneus usagés non réutilisables (PUNR) - Partie 2 :
Granulats et poudrettes - Méthodes de détermination de leur(s) dimension(s) et
impuretés, y compris la teneur en fils métalliques et en fibres textiles libres
Ta slovenski standard je istoveten z: prEN 14243-2
ICS:
13.030.50 Recikliranje Recycling
83.160.01 Avtomobilske pnevmatike na Tyres in general
splošno
oSIST prEN 14243-2:2018 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN 14243-2:2018
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oSIST prEN 14243-2:2018
DRAFT
EUROPEAN STANDARD
prEN 14243-2
NORME EUROPÉENNE
EUROPÄISCHE NORM
November 2017
ICS 83.160.01 Will supersede CEN/TS 14243:2010
English Version
Materials obtained from end of life tyres - Part 2:
Granulates and powders - Methods for determining their
dimension(s) and impurities, including free steel and free
textile content
Matériaux produits à partir de pneus usagés non Materialien aus Altreifen - Teil 2: Granulate und Pulver
réutilisables (PUNR) - Partie 2 : Granulats et - Methode zur Bestimmung der Abmessungen und
poudrettes - Méthodes de détermination de leur(s) Verunreinigungen einschließlich freier Stahl, freie
dimension(s) et impuretés, y compris la teneur en fils Textilien und andere Verunreinigungen
métalliques et en fibres textiles libres
This draft European Standard is submitted to CEN members for enquiry. It has been drawn up by the Technical Committee
CEN/TC 366.
If this draft becomes a European Standard, CEN members are bound to comply with the CEN/CENELEC Internal Regulations
which stipulate the conditions for giving this European Standard the status of a national standard without any alteration.
This draft European Standard was established by CEN in three official versions (English, French, German). A version in any other
language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC
Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania,
Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland,
Turkey and United Kingdom.
Recipients of this draft are invited to submit, with their comments, notification of any relevant patent rights of which they are
aware and to provide supporting documentation.
Warning : This document is not a European Standard. It is distributed for review and comments. It is subject to change without
notice and shall not be referred to as a European Standard.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Avenue Marnix 17, B-1000 Brussels
© 2017 CEN All rights of exploitation in any form and by any means reserved Ref. No. prEN 14243-2:2017 E
worldwide for CEN national Members.
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Contents Page
European foreword . 4
Introduction . 5
1 Scope . 6
2 Normative references . 6
3 Terms and definitions . 6
4 Categories of products obtained from end-of-life tyres based mainly on their
dimensions . 7
5 Determination of dimensions for granulates and powders . 7
5.1 General. 7
5.2 Sampling plan . 7
5.2.1 Principles of sampling . 7
5.2.2 Preparation of the sampling plan . 7
5.2.3 Definition of lot size . 7
5.2.4 Sampling point and apparatus . 8
5.2.5 Size of a sample increment . 8
5.2.6 Number of increments . 8
5.2.7 Visual assessment . 9
5.2.8 Sampling certificate . 9
5.3 Storage and transport of laboratory sample(s) . 9
5.4 Preparation of the laboratory sample(s) and test portion(s) . 9
5.4.1 Principles of correct sample preparation and sample division . 9
5.4.2 Test sample and test portion preparation . 10
5.4.3 Apparatus for sample division . 10
5.4.4 Procedure . 11
5.5 Particle size analysis . 11
5.5.1 General principles . 11
5.5.2 Sieves . 11
5.5.3 Flat brush . 11
5.5.4 Mechanical vibrating equipment . 11
5.5.5 Scales . 11
5.5.6 Procedure . 11
5.5.7 Calculation . 12
5.5.8 Graphical representation . 12
5.6 Test Report . 13
Annex A (normative) Determination of free steel content for granulates and powders by the
method of magnetic separation . 15
A.1 General. 15
A.2 Principle of the determination . 15
A.3 Sampling . 15
A.4 Equipment . 15
A.5 Procedure . 16
A.6 Calculation . 17
A.7 Metrological characteristics . 17
A.8 Test report . 17
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Annex B (normative) Determination of free textile content for granulates and powders by
the method of the “small ball” agglomeration . 18
B.1 General . 18
B.2 Principle of the determination . 18
B.3 Sampling . 18
B.4 Equipment . 18
B.5 Procedure . 18
B.6 Calculations . 19
B.7 Metrological characteristics . 19
B.8 Test report . 19
Annex C (normative) Determination of other impurities for granulates and powders by the
method of a saline solution . 20
C.1 General . 20
C.2 Principle of the determination . 20
C.3 Sampling . 20
C.4 Equipment . 20
C.5 Procedure . 21
C.5.1 Sample cleaning . 21
C.5.2 Saline solution procedure . 21
C.6 Calculations . 22
C.7 Metrological characteristics . 22
C.8 Test report . 22
Annex D (informative) Example of separatory funnel . 24
Annex E (informative) Sieving . 25
Annex F (informative) Recommended sieve list . 27
Bibliography . 29
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European foreword
This document (prEN 14243-2:2017) has been prepared by Technical Committee CEN/TC 366
“Materials obtained from End-of-Life Tyres (ELT)”, the secretariat of which is held by UNI.
This document is currently submitted to the CEN Enquiry.
This document will supersede CEN/TS 14243:2010.
prEN 14243, Materials obtained from end of life tyres, consists of the following parts:
— Part 1: General definitions related to the methods for determining their dimension(s) and impurities;
— Part 2: Granulates and powders — Methods for determining their dimension(s) and impurities,
including free steel and free textile content;
— Part 3: Shreds, cuts and chips — Methods for determining their dimension(s) including protruding
filaments dimensions;
— Part 4: Steel wires and textile fibres — Methods for their characterization.
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Introduction
This Standard will be used in conjunction with the other parts of the prEN 14243 series. Such series is
intended to cover the testing programs needed to characterize each product category as shown on the
figure below.
Figure 1 — Typical scheme for a testing programme concerning several characteristics with
testing steps in the field and in the laboratory
End-of-life tyres consist mainly of passenger and commercial vehicle tyres, truck, earthmover and
agricultural tyres manufactured for distribution in the European market that are no longer suitable for
their original purpose. Products from end-of-life tyres are used as a secondary raw material finding a
wide range of applications. The principal categories of materials from end-of-life tyres are defined on
the basis of their dimension(s) according to prEN 14243-1.
European Standards are needed for the production, trade and use of the materials from end-of-life
tyres. They are also useful for buyers, regulators, controllers and laboratories.
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1 Scope
This European Standard provides test methods for the determination of the dimension(s) of granulates
and powders, produced from all categories of end-of-life tires at all steps of the treatment processes as
well as for the determination of impurities (including free steel and free textile content).
The methods described in this Standard include sample collection and the preparation of a
representative sample based on a sampling plan for the purpose of determining dimensions and
impurities.
This Standard does not cover the operational performance or fitness for use of the materials which is
deemed to be a function of the agreement between manufacturer and customer.
This Standard does not purport to address all of the safety concerns, if any, associated with its use. This
standard does not establish appropriate safety and health practices and does not determine the
applicability of regulatory limitations prior to use.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content
constitutes requirements of this document. For dated references, only the edition cited applies. For
undated references, the latest edition of the referenced document (including any amendments) applies.
EN 933-1, Tests for geometrical properties of aggregates — Part 1: Determination of particle size
distribution— Sieving method
EN 933-2, Tests for geometrical properties of aggregates — Part 2: Determination of particle size
distribution — Test sieves, nominal size of apertures
prEN 14243-1:2017, Materials obtained from end of life tyres — Part 1: General definitions related to the
methods for determining their dimension(s) and impurities
FprCEN/TS 17188, Materials obtained from end of life tyres — Sampling method for granulates and
powders stored in big-bags
ISO 565:1990, Test sieves — Metal wire cloth, perforated metal plate and electroformed sheet — Nominal
sizes of openings
ISO 3310-1:2000, Test sieves — Technical requirements and testing — Part 1: Test sieves of metal wire
cloth
ISO 3310-2:1999, Test sieves — Technical requirements and testing — Part 2: Test sieves of perforated
metal plate
3 Terms and definitions
For the purposes of this document, the terms and definitions given in prEN 14243-1 apply.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
• IEC Electropedia: available at http://www.electropedia.org/
• ISO Online browsing platform: available at http://www.iso.org/obp
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4 Categories of products obtained from end-of-life tyres based mainly on their
dimensions
For categories and testing program refer to prEN 14243-1:2017, Clause 4.
5 Determination of dimensions for granulates and powders
5.1 General
Particle size and related parameters are key measurements for product classification of size-reduced
materials such as granulates and powders. Particle size analysis is the first measurement of consistency
and forms the basis for material grading. Before being able to obtain an accurate particle size
distribution, a representative sample of the material to be tested shall be taken.
Depending on the agreed testing program between the producer and the customer, or on the producer's
own will, the determination of dimensions specified in this clause for granulates and powders may be
followed by the additional determination(s) of the free steel content and/or the free textile content
and/or the other impurities as specified in Annexes A, B and C.
5.2 Sampling plan
5.2.1 Principles of sampling
The main principle of sampling is to obtain a representative sample(s) from a lot of material from which
a characteristic is to be determined. If the lot is to be represented by a sample then every particle in the
lot shall have an equal probability of being included in the sample (i.e. probabilistic sampling). When
these principles cannot be applied in practice, the sampler shall define a procedure as close as possible
to probabilistic sampling in his judgement (i.e. judgemental sampling) and note the limitations in the
sampling plan and sampling report.
Obtaining samples that are truly representative of the material produced is easier when the material is
moving (for example on a conveyor belt). Therefore, sampling from moving material shall be preferred
wherever possible. For granulates and powders stored in big-bags a sampling method is described in
FprCEN/TS 17188.
NOTE The determination of properties other than dimension may result in different sampling requirements.
This is the case for the determination of physical properties (such as bulk density) or chemical composition.
5.2.2 Preparation of the sampling plan
A sampling plan shall be prepared before samples are taken through a specific definition of the lot size
and the size and number of increments to be taken.
5.2.3 Definition of lot size
The lot size shall be defined by the producer in accordance with requested specifications and is a fixed
quantity for which a characteristic is to be determined. The lot size m may be defined by the producer
lot
as:
• a fixed quantity produced between machine settings
• a fixed quantity in a production day/shift
• a fixed quantity minimum of 100 t (10 t for powders).
The lot size is based on production quality management decisions or specific customer requirements.
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5.2.4 Sampling point and apparatus
Based on health and safety assessments and producer equipment, a fixed sampling point for the
collection of sample increments shall be chosen for each material fraction to be monitored. Sampling
shall be carried out using a sample box or other suitable equipment. The sampling box is passed
through the stream of falling material so that it uniformly cuts the full flow of falling material. The box
shall be large enough so that it does not become overloaded. Automatic systems fulfilling these criteria
may also be used.
5.2.5 Size of a sample increment
The sampling box shall have a capacity of not less than:
V = 0,5 for d < 10
min
V = 0,05 × d for 10 ≤ d ≤ 20
min
3
V = 5 dm (chips considered as very large granulates)
min
where
V is the minimum capacity of the sampling box (in cubic decimetres);
min
d is the nominal top size in millimetres;
The sampling operator shall record the approximate capacity of the sampling device V (in cubic
increment
decimetres).
5.2.6 Number of increments
The minimum number of increments to be taken from a lot depends on the nominal top size of the
granulate to be sampled. The granulate shall be assigned by the sampler to one of two groups in Table 1.
Table 1 — Classification of material according to size
Group 1 Group 2
nominal top size < 10 mm nominal top size between 10 mm and 20 mm
For sampling from moving material:
Group 1: n = 3 + 0,025 × t m size of granulates from 0,8 mm to 10 mm and powders under
lot
0,8 mm
Group 2: n = 5 + 0,040 × m size of granulates from 10 mm to 20 mm
lot
where
n is the minimum permitted number of increments rounded off to the higher nearest whole
number
m is the mass of the lot in tonnes.
lot
Sample collection is carried out according to the sample plan and the increments are collected manually
using the sampling box. Each increment is placed in a separate container. Increments shall be taken at
regular intervals during the discharge of the lot in accordance with the sampling plan. The time of
increment collection is recorded in the sampling plan. At the end of this process, all the increments
corresponding to the lot are placed in a single container and constitute the combined sample(s) which
is sent to a laboratory as laboratory sample(s). In case more than one laboratory sample is required,
they shall be prepared in the plant in accordance with the principles of sample division of 5.4.2.
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5.2.7 Visual assessment
The increments shall be assessed visually and observations on the quality should be noted as additional
information and recorded according to quality management, best practice policies or specific customer
requirements.
5.2.8 Sampling certificate
The sampling certificate shall include at least the following information:
a) the name of the producer;
b) kind of material: powder or granulate;
c) a unique identification number of the sample;
d) the name of the sampler;
e) the location(s), date and time of sampling;
f) collection point of the material:
1) production with the additional information:
i) nominal top size;
ii) definition and mass of the lot size;
iii) a unique identification number of the lot;
iv) sampling point;
v) number, time and volume of increments;
2) big bag (sampling according to FprCEN/TS 17188);
g) weight of the combined sample sent to laboratory;
h) reference to this Standard;
i) any deviation from this Standard.
5.3 Storage and transport of laboratory sample(s)
Samples shall be stored in such a way that material will not be lost during transportation. The samples
shall be stored dry and in a sealed sample box. The sampling certificate shall be attached.
5.4 Preparation of the laboratory sample(s) and test portion(s)
5.4.1 Principles of correct sample preparation and sample division
The main purpose of sample preparation is that the laboratory sample collected from the whole lot are
reduced to one or more test samples based on sample division. The aim of sample division is therefore
to homogenize and reduce the mass of the laboratory sample to make several duplicate test samples.
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Each test sample shall be representative of the original sample based on the principle that the
composition of the sample as taken on site shall not be changed during the steps of sample preparation
for testing.
5.4.2 Test sample and test portion preparation
The increments that have been collected are mixed together in a container of suitable size to form a
combined sample. In this case the combined sample is the laboratory sample.
The laboratory sample may need to be reduced to a test sample before a test portion is produced. The
test sample(s) or directly the laboratory sample shall be reduced to a suitable size in order to obtain
test portion(s) in such a way that sufficient material is still provided for all the tests to be performed. In
particular the calculation shall take into account the need for duplicate test portions, for extra material
in case dubious results are obtained and the need for sampling with replacement. The sampling plan
shall take into account such requirements. The test sample(s) (or directly the laboratory sample) shall
be reduced using the principles of sample division using either:
— a riffle splitter;
— a rotary sample divider, or
— other equivalent device.
5.4.3 Apparatus for sample division
The most relevant sample division methods are based on the following apparatus:
a) Riffle splitter: a sample splitter shall have at least 12 slots and an even number with adjacent slots
directing material into two different sub-samples. The width of the slots shall be at least three times
the nominal top size of the material to be riffled to prevent sample bridging.
Figure 2 — Example of a riffle box
b) Rotary sample divider: a rotary sample divider shall be used according to its manufacturer's
manual. The inner dimensions of the equipment where the sample is fed shall be at least three
times as wide as the nominal top size to be processed.
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5.4.4 Procedure
The combined sample is mixed with a scoop and sent through the sample divider until the sample
reduction is complete. A final mass quantity of at least 150 g is used for the purposes of the particle size
analysis depending on the size of the sieving system in order to fulfil the non-overloading criteria given
in 5.5.6.
5.5 Particle size analysis
5.5.1 General principles
A sample is subjected to mechanical sieving through a set of oscillating sieves, sorting the particles in
decreasing size classes by mechanical means. All apparatus shall conform to the general requi
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