ISO/TS 21396:2017

TECHNICAL ISO/TS
SPECIFICATION 21396
First edition
2017-12
Rubber — Determination of mass
concentration of tire and road
wear particles (TRWP) in soil and
sediments — Pyrolysis-GC/MS method
Caoutchouc — Détermination de la concentration massique en
particules de pneus et d'usure de la route (TWRP) dans le sol et les
sédiments — Méthode par pyrolyse-GC/MS
Reference number
©
ISO 2017
© ISO 2017, Published in Switzerland
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ii © ISO 2017 – All rights reserved

Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 2
5 Reagents . 2
6 Apparatus . 3
7 Specimen preparation laboratory . 5
8 Measuring range . 5
9 Limit of detection . 5
10 Procedure. 6
10.1 General . 6
10.2 Sample collection . 6
10.3 Deuterated internal standard preparation . 6
10.4 Calibration curve preparation . 7
10.4.1 Stock solutions . 7
10.4.2 Calibration curves . 7
10.5 Sample preparation . 8
10.5.1 Oven drying . 8
10.5.2 Sieving and homogenization . 8
10.6 Sample measurement . 8
10.6.1 Sample mass . 8
10.6.2 Internal standard addition . 9
10.6.3 Pyrolysis-gas chromatograph/mass spectrometer measurement . 9
11 Analysis . 9
11.1 TRWP detection limit . 9
11.2 Quantity of tyre polymer in the sample . 9
11.3 Mass concentration of TRWP.10
12 Performance characteristics .10
12.1 General .10
12.2 Specific performance characteristics .10
12.3 Method detection limit .10
13 Test report .10
Annex A (informative) Recipe for calibration curves and stock solutions .12
Annex B (informative) Curie-point pyrolyser .14
Annex C (informative) Representative calibration curves and pyrograms .15
Annex D (normative) Calculation of TRWP detection limits .20
Annex E (normative) Calculation of results using dimer markers .21
Bibliography .23
Foreword
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electrotechnical standardization.
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described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
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URL: www.iso.org/iso/foreword.html.
This document was prepared by Technical Committee ISO/TC 45, Rubber and Rubber Products.
iv © ISO 2017 – All rights reserved

Introduction
Tyre and road wear particles (TRWP) are formed as a result of tread abrasion from the road surface,
and subsequent particle release to the environment. TRWP consist of tyre tread particles which include
[1]
incorporated material from the road surface (Kreider et al. 2010 ). The elastomeric fraction in TRWP
contained in soil or sediment materials is quantified in this document by direct pyrolysis-GC/MS
analysis. Mass concentration can be expressed on the basis of the rubber polymer, tyre tread, or TRWP.
This method has been used to measure the TRWP concentration in soil and sediment samples from three
[2] [3]
geographically separated regions (Unice et al. 2012 ; Unice et al. 2013 ). The airborne concentration
[4]
of TRWP in the PM fraction has also been characterized by a similar method (Panko et al. 2013 ).
Specific chemical markers are generated from intact TRWP by pyrolysis of sample specimens. The
chemical markers consist of characteristic and specific pyrolysis dimeric fragments of passenger
and truck tyre tread polymers including butadiene rubber, styrene-butadiene rubber, and isoprene
rubber. The polymer fragments generated by sample pyrolysis are subsequently separated by gas
chromatography, and identified by mass spectroscopy. The TRWP mass concentration is calculated
based on market average polymer use rates in tread, and prior characterization of the mineral content
of TRWP. Rubber polymer specificity is achieved by quantification of dimeric polymer fragments
[5] [6]
consisting of two monomer units (Kitamura et al. 2007 ; Harada et al. 2009 ). Repeatability is
achieved by the use of a deuterated internal standard of similar polymeric structure to the tyre tread
polymers. The internal standard corrects for variable analyte recovery caused by sample size, matrix
effects, and temporal variation in instrument response. The method is suitable for monitoring changes
in soil or sediment TRWP concentrations over time.
TECHNICAL SPECIFICATION ISO/TS 21396:2017(E)
Rubber — Determination of mass concentration of tire
and road wear particles (TRWP) in soil and sediments —
Pyrolysis-GC/MS method
WARNING 1 — Persons using this document should be familiar with normal laboratory practice.
This document does not purport to address all of the safety problems, if any, associated with its
use. It is the responsibility of the user to establish appropriate safety and health practices.
WARNING 2 — Certain procedures specified in this document may involve the use or generation
of substances, or the generation of waste, that could constitute a local environmental hazard.
Reference should be made to appropriate documentation on safe handling and disposal after use.
1 Scope
This document specifies a method for the determination of the soil or sediment mass concentration
(μg/g) of tyre and road wear particles (TRWP) in environmental samples.
This document establishes principles for soil or sediment sample collection, the generation of pyrolysis
fragments from the sample, and the quantification of the generated polymer fragments. The quantified
polymer mass is used to calculate the concentration of TRWP in soil or sediment. These quantities are
expressed on a TRWP basis, which includes the mass of tyre tread and mass of road wear encrustations,
and can also be expressed on a tyre rubber polymer or tyre tread basis.
NOTE Tyre and road wear particles are a discrete mass of elongated particles generated at the frictional
interface between the tyre and roadway surface during the service life of a tyre. The particles consist o
...