Materials obtained from end-of-life tyres - Determination of the specific surface area of powders - Method based on krypton adsorption

This document specifies a method for the determination of low specific surface area of powders ELTs rubber by measuring the amount of physically adsorbed krypton gas and applying the theoretical multipoint Brunnauer, Emmett and Teller (BET) method.
This document defines a specific method for powders taking into account that, in order to obtain an accurate value of specific surface area, a representative sample of the material to be tested is taken according to the principle that every particle of the sample that represents the lot have an equal probability of being included in the sample.

Materialien aus Altreifen - Bestimmung der spezifischen Oberfläche von Granulaten und Mehlen - Verfahren basierend auf Kryptonadsorption

Dieses Dokument legt ein Verfahren zur Bestimmung der niedrigen spezifischen Oberfläche von Mehlen aus ELT-Gummi durch Messung der Menge an physikalisch adsorbiertem Kryptongas und Anwendung des theoretischen Brunauer, Emmet und Teller (BET) Multipunkt Verfahrens fest.
Dieses Dokument definiert ein spezifisches Verfahren für Mehle, wobei berücksichtigt wird, dass um einen genauen Wert der spezifischen Oberfläche zu erhalten, eine repräsentative Probe des zu prüfenden Materials nach dem Prinzip entnommen wird, dass jedes Partikel der Probe, die die Charge repräsentiert, mit gleicher Wahrscheinlichkeit in der Probe enthalten ist.

Matériaux produits à partir de pneus usagés non réutilisables - Détermination de la surface spécifique des poudrettes - Méthode fondée sur l'adsorption de krypton

Le présent document spécifie une méthode pour la détermination des faibles surfaces spécifiques des poudrettes à base de caoutchouc issu de PUNR en mesurant la quantité de krypton gazeux physiquement adsorbé et en appliquant la méthode théorique multipoints de Brunauer, Emmett et Teller (BET).
Le présent document définit une méthode spécifique pour les poudrettes en tenant compte du fait que, pour obtenir une valeur exacte de la surface spécifique, un échantillon représentatif du matériau soumis à essai doit être prélevé, conformément au principe selon lequel toutes les particules de l'échantillon du lot ont une probabilité égale d'être incluses dans l'échantillon.

Materiali, pridobljeni iz izrabljenih avtomobilskih gum - Določanje specifične površine prahu - Metoda, ki temelji na adsorpciji kriptona

General Information

Status
Published
Public Enquiry End Date
22-Jul-2020
Publication Date
20-Oct-2020
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
15-Oct-2020
Due Date
20-Dec-2020
Completion Date
21-Oct-2020

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SLOVENSKI STANDARD
SIST-TS CEN/TS 17510:2020
01-december-2020
Materiali, pridobljeni iz izrabljenih avtomobilskih gum - Določanje specifične
površine prahu - Metoda, ki temelji na adsorpciji kriptona

Materials obtained from end-of-life tyres - Determination of the specific surface area of

powders - Method based on krypton adsorption

Materialien aus Altreifen - Bestimmung der spezifischen Oberfläche von Granulaten und

Mehlen - Verfahren basierend auf Kryptonadsorption

Matériaux produits à partir de pneus usagés non réutilisables - Détermination de la

surface spécifique des poudrettes - Méthode fondée sur l'adsorption de krypton
Ta slovenski standard je istoveten z: CEN/TS 17510:2020
ICS:
13.030.50 Recikliranje Recycling
83.160.01 Avtomobilske pnevmatike na Tyres in general
splošno
SIST-TS CEN/TS 17510:2020 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST-TS CEN/TS 17510:2020
---------------------- Page: 2 ----------------------
SIST-TS CEN/TS 17510:2020
CEN/TS 17510
TECHNICAL SPECIFICATION
SPÉCIFICATION TECHNIQUE
October 2020
TECHNISCHE SPEZIFIKATION
ICS 83.160.01; 13.030.50
English Version
Materials obtained from end-of-life tyres - Determination
of the specific surface area of powders - Method based on
krypton adsorption

Matériaux produits à partir de pneus usagés non Materialien aus Altreifen - Bestimmung der

réutilisables - Détermination de la surface spécifique spezifischen Oberfläche von Mehlen - Verfahren

des poudrettes - Méthode fondée sur l'adsorption de basierend auf Kryptonadsorption

krypton

This Technical Specification (CEN/TS) was approved by CEN on 24 August 2020 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, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. CEN/TS 17510:2020 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST-TS CEN/TS 17510:2020
CEN/TS 17510:2020 (E)
Contents Page

European foreword ............................................................................................................................................ 3

Introduction .......................................................................................................................................................... 4

1 Scope .......................................................................................................................................................... 5

2 Normative references .......................................................................................................................... 5

3 Terms and definitions ......................................................................................................................... 5

4 Principle ................................................................................................................................................... 6

5 Apparatus ................................................................................................................................................ 7

5.1 General...................................................................................................................................................... 7

6 Procedure ................................................................................................................................................ 7

6.1 Sample preparation ............................................................................................................................. 7

6.2 Analysis .................................................................................................................................................... 8

6.3 Analysis data ........................................................................................................................................... 8

7 Test report ............................................................................................................................................... 9

Bibliography ....................................................................................................................................................... 10

---------------------- Page: 4 ----------------------
SIST-TS CEN/TS 17510:2020
CEN/TS 17510:2020 (E)
European foreword

This document (CEN/TS 17510:2020) 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.

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.

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, France, Germany, Greece, Hungary, Iceland,

Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of

North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United

Kingdom.
---------------------- Page: 5 ----------------------
SIST-TS CEN/TS 17510:2020
CEN/TS 17510:2020 (E)
Introduction

Specific surface area (A ) is a parameter of great importance when it comes to physical characterization

of materials such as granulates and powders from rubber materials. Like other physical characteristics,

specific surface area could influence the performance of materials in its different applications.

Depending on the type of sample to be characterized, several different methods can be used for the

determination of the specific surface area, generally based on different physical principles. The most

widespread and useful method used in materials characterization is gas adsorption, either through

gravimetric or volumetric methods.

For very low surface area samples the traditional volumetric method of nitrogen adsorption at 77 K or

2 -1

Argon at 87 K shows some important limitations. Alternatively, for absolute areas as low as 0,05 m g

the suitable method for A determination is krypton adsorption at 77 K.
---------------------- Page: 6 ----------------------
SIST-TS CEN/TS 17510:2020
CEN/TS 17510:2020 (E)
1 Scope

This document specifies a method for the determination of low specific surface area of powders ELTs

rubber by measuring the amount of physically adsorbed krypton gas and applying the theoretical

multipoint Brunauer, Emmett and Teller (BET) method.

This document defines a specific method for powders taking into account that, in order to obtain an

accurate value of specific surface area, a representative sample of the material to be tested is taken

according to the principle that every particle of the sample that represents the lot have an equal

probability of being included in the sample.
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
3 Terms and definitions

For the purposes of this document, the terms and definitions given in EN 14243-1:2019 and the following

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 https://www.iso.org/obp
3.1
adsorption

enrichment of the adsorptive gas at the external and accessible internal surfaces of a solid material

[SOURCE: ISO 15901-2:2006]
3.2
adsorbate
adsorbed gas
[SOURCE: 15901-2:2006]
3.3
adsorptive
gas or vapour to be adsorbed
[SOURCE: ISO 15901-2:2006]
3.4
adsorbent
solid material on which adsorption occurs
[SOURCE: ISO 15901-2:2006]
---------------------- Page: 7 ----------------------
SIST-TS CEN/TS 17510:2020
CEN/TS 17510:2020 (E)
3.5
isotherm
relationship between the amount of gas adsorbed and the equi
...

SLOVENSKI STANDARD
kSIST-TS FprCEN/TS 17510:2020
01-julij-2020
Materiali, pridobljeni iz izrabljenih avtomobilskih gum - Določanje specifične
površine prahu - Metoda, ki temelji na adsorpciji kriptona

Materials obtained from End-of-Life Tyres - Determination of the specific surface area of

powders - Method based on krypton adsorption

Materialien aus Altreifen - Bestimmung der spezifischen Oberfläche von Granulaten und

Mehlen - Verfahren basierend auf Kryptonadsorption

Matériaux produits à partir de pneus usagés non réutilisables - Détermination de la

surface spécifique des poudrettes - Méthode fondée sur l'adsorption de krypton
Ta slovenski standard je istoveten z: FprCEN/TS 17510
ICS:
13.030.50 Recikliranje Recycling
kSIST-TS FprCEN/TS 17510:2020 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
kSIST-TS FprCEN/TS 17510:2020
---------------------- Page: 2 ----------------------
kSIST-TS FprCEN/TS 17510:2020
FINAL DRAFT
TECHNICAL SPECIFICATION
FprCEN/TS 17510
SPÉCIFICATION TECHNIQUE
TECHNISCHE SPEZIFIKATION
April 2020
ICS
English Version
Materials obtained from End-of-Life Tyres - Determination
of the specific surface area of powders - Method based on
krypton adsorption

Matériaux produits à partir de pneus usagés non Materialien aus Altreifen - Bestimmung der

réutilisables - Détermination de la surface spécifique spezifischen Oberfläche von Granulaten und Mehlen -

des poudrettes - Méthode fondée sur l'adsorption de Verfahren basierend auf Kryptonadsorption

krypton

This draft Technical Specification is submitted to CEN members for Vote. It has been drawn up by the Technical Committee

CEN/TC 366.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, 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 Technical Specification. It is distributed for review and comments. It is subject to change

without notice and shall not be referred to as a Technical Specification.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2020 CEN All rights of exploitation in any form and by any means reserved Ref. No. FprCEN/TS 17510:2020 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
kSIST-TS FprCEN/TS 17510:2020
FprCEN/TS 17510:2020 (E)
Contents Page

European foreword ............................................................................................................................................ 3

Introduction .......................................................................................................................................................... 4

1 Scope .......................................................................................................................................................... 5

2 Normative references .......................................................................................................................... 5

3 Terms and definitions ......................................................................................................................... 5

4 Principle ................................................................................................................................................... 6

5 Apparatus ................................................................................................................................................ 7

6 Procedure ................................................................................................................................................ 7

7 Test Report .............................................................................................................................................. 9

Bibliography ....................................................................................................................................................... 10

---------------------- Page: 4 ----------------------
kSIST-TS FprCEN/TS 17510:2020
FprCEN/TS 17510:2020 (E)
European foreword

This document (FprCEN/TS 17510:2020) 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 Vote on TS.
---------------------- Page: 5 ----------------------
kSIST-TS FprCEN/TS 17510:2020
FprCEN/TS 17510:2020 (E)
Introduction

Specific surface area (As) is a parameter of great importance when it comes to physical characterization

of materials such as granulates and powders from rubber materials. Like other physical characteristics,

specific surface area could influence the performance of materials in its different applications.

Depending on the type of sample to be characterized, several different methods can be used for the

determination of the specific surface area, generally based on different physical principles. The most

widespread and useful method used in materials characterization is gas adsorption, either through

gravimetric or volumetric methods.

For very low surface area samples the traditional volumetric method of nitrogen adsorption at 77 K or

2 -1

Argon at 87 K shows some important limitations. Alternatively, for absolute areas as low as 0,05 m g

the suitable method for As determination is Krypton adsorption at 77 K.
---------------------- Page: 6 ----------------------
kSIST-TS FprCEN/TS 17510:2020
FprCEN/TS 17510:2020 (E)
1 Scope

This document specifies a method for the determination of low specific surface area of powders ELTs

rubber by measuring the amount of physically adsorbed krypton gas and applying the theoretical

multipoint Brunnauer, Emmett and Teller (BET) method.

This document defines a specific method for powders taking into account that, in order to obtain an

accurate value of specific surface area, a representative sample of the material to be tested is taken

according to the principle that every particle of the sample that represents the lot have an equal

probability of being included in the sample.
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
3 Terms and definitions

For the purposes of this document, the terms and definitions given in EN 14243-1:2019 and the following

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
3.1
adsorption

enrichment of the adsorptive gas at the external and accessible internal surfaces of a solid material

[SOURCE: ISO 15901-2:2006]
3.2
adsorbate
adsorbed gas
[SOURCE: 15901-2:2006]
3.3
adsorptive
gas or vapour to be adsorbed
[SOURCE: ISO 15901-2:2006]
3.4
adsorbent
solid material on which adsorption occurs
[SOURCE: ISO 15901-2:2006]
---------------------- Page: 7 ----------------------
kSIST-TS FprCEN/TS 17510:2020
FprCEN/TS 17510:2020 (E)
3.5
isotherm

relationship between the amount of gas adsorbed and the equilibrium pressure of the gas, at constant

temperature
[SOURCE: ISO 15901-2:2006]
3.6
surface area

extent of available surface area as determined by a given method under stated conditions

[SOURCE: ISO 15901-1:2016]
3.7
specific surface area
absolute surface area of the sample divided by sample mass
3.8
relative pressure

ratio of the equilibrium adsorption pressure, p, to the saturation vapour pressure, p°, at analysis

temperature
[SOURCE: ISO 15901-3:2007]
4 Principle

The determination of the specific surface area undergoes by the determination of the amount of

adsorbate required to cover the external and accessible internal pore surface of the adsorbent with a

complete monolayer of adsorbate. The monolayer capacity is then calculated by using the BET eq

...

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