ISO 21561-2:2024 PDF

Styrene-butadiene rubber (SBR) — Determination of the microstructure of solution-polymerized SBR — Part 2: Fourier transform infrared spectrometry (FTIR) with attenuated total reflection (ATR) method

Название (английский):

ISO 21561-2:2024

Статус документа:: Действующий
Формат:: Электронный (PDF)
Количество страниц:: 15
Дата публикации:: 15 августа 2024 г.
Издание:: ISO IS 21561 edition 2 version 1
ICS:: 83.060

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Описание (английский):

This document specifies procedures for the quantitative determination of the microstructure of the butadiene portion and the content of styrene in solution-polymerized SBR (S-SBR) by Fourier transform infrared spectrometry (FTIR) with attenuated total reflection (ATR) method. The styrene content is expressed in mass fraction relative to the S-SBR. The contents of three microstructure types, i.e. vinyl, trans and cis, are expressed in mol fraction relative to the butadiene portion in the S-SBR. This method is only applicable to raw rubbers. NOTE 1 Precision as shown in Annex A is not always possible to obtain for S-SBRs containing polystyrene block or styrene content more than 45 %. NOTE 2 Only “vinyl”, “trans” and “cis”, are used in this document. However, the expression of vinyl, trans and cis mean as follows in general: vinyl: vinyl unit, vinyl bond, 1,2-unit, 1,2-bond, 1,2-vinyl-unit or 1,2-vinyl-bond; trans: 1,4-trans unit, 1,4-trans bond, trans-1,4 unit or trans1,4 bond; cis: 1,4-cis unit, 1,4-cis bond, cis-1,4 unit or cis-1,4 bond.

Технические детали

Технический комитет: ISO/TC 45/SC 3 - Raw materials (including latex) for use in the rubber industry
SKU: ISO 21561-2:2024

Abstract

Overview

ISO 21561-2:2024 defines a standardized FTIR‑ATR (Fourier transform infrared spectrometry with attenuated total reflection) procedure to quantitatively determine the microstructure of the butadiene portion and the styrene content in solution‑polymerized styrene‑butadiene rubber (S‑SBR). Results report styrene as a mass fraction of the S‑SBR and vinyl / trans / cis microstructures as mol fractions relative to the butadiene portion. The method applies to raw rubbers only and includes calibration, sampling and spectrum‑acquisition requirements.

Key topics and technical requirements

Measurement principle: ATR‑FTIR spectra are used to obtain absorbances characteristic of styrene and each butadiene microstructure; regression formulae convert absorbance ratios into composition.
Instrumentation and settings:
- FTIR detector: DTGS or TGS
- Resolution: 2 cm−1
- Number of scans: 32
- Spectral range: 600–1 800 cm−1
- ATR: single‑bounce diamond crystal, incidence angle 45°, with a pressure clamp to ensure consistent contact
Sampling and sample prep: prepare test piece per ISO 1795; sample surface must be flat and roughly the size of the ATR crystal.
Peak measurement points (examples from the standard):
- Styrene: 695–700 cm−1 (or 720–730 cm−1 when shifted)
- Styrene (secondary): 755–761 cm−1
- Cis: commonly at 726 cm−1 when masked by styrene
- Vinyl: 905–912 cm−1 and 991–996 cm−1
- Trans: 962–967 cm−1
- Baseline reference: 1 200 cm−1
Data processing: baseline correction, calculation of absorbance ratios and second‑order terms, then substitution into the published regression formulae (derived from interlaboratory data) to obtain styrene and microstructure values.
Controls and limitations:
- Maintain consistent sample chamber atmosphere to avoid CO2 interference (peaks at ~668 and 723 cm−1).
- Precision (Annex A) may deteriorate for S‑SBR containing polystyrene blocks or with styrene content >45 %.
Supplementary material: Annex B (regression acquisition), Annex C (NMR alternative) and precision data in Annex A.

Applications

Quality control and batch verification of S‑SBR in rubber and tire manufacturing
Polymer synthesis monitoring and process optimization for solution‑polymerized SBR
Supplier qualification, acceptance testing and material specification compliance
R&D and failure analysis where microstructure affects performance (rolling resistance, wear, etc.)

Who should use this standard

Rubber and tire manufacturers, QC laboratories, polymer chemists, materials characterization labs, and regulatory/standards bodies involved in rubber testing and specification.

Related standards

ISO 1795 - Rubber, raw natural and raw synthetic - Sampling and preparative procedures
ISO 1382 - Rubber - Vocabulary
Other parts of the ISO 21561 series covering complementary methods (e.g., NMR described in Annex C)

Keywords: ISO 21561-2:2024, SBR microstructure, S‑SBR, FTIR ATR method, styrene content, vinyl trans cis, rubber testing, ATR‑FTIR rubber analysis.

Overview

Key topics and technical requirements

Measurement principle: ATR‑FTIR spectra are used to obtain absorbances characteristic of styrene and each butadiene microstructure; regression formulae convert absorbance ratios into composition.
Instrumentation and settings:
- FTIR detector: DTGS or TGS
- Resolution: 2 cm−1
- Number of scans: 32
- Spectral range: 600–1 800 cm−1
- ATR: single‑bounce diamond crystal, incidence angle 45°, with a pressure clamp to ensure consistent contact
Sampling and sample prep: prepare test piece per ISO 1795; sample surface must be flat and roughly the size of the ATR crystal.
Peak measurement points (examples from the standard):
- Styrene: 695–700 cm−1 (or 720–730 cm−1 when shifted)
- Styrene (secondary): 755–761 cm−1
- Cis: commonly at 726 cm−1 when masked by styrene
- Vinyl: 905–912 cm−1 and 991–996 cm−1
- Trans: 962–967 cm−1
- Baseline reference: 1 200 cm−1
Data processing: baseline correction, calculation of absorbance ratios and second‑order terms, then substitution into the published regression formulae (derived from interlaboratory data) to obtain styrene and microstructure values.
Controls and limitations:
- Maintain consistent sample chamber atmosphere to avoid CO2 interference (peaks at ~668 and 723 cm−1).
- Precision (Annex A) may deteriorate for S‑SBR containing polystyrene blocks or with styrene content >45 %.
Supplementary material: Annex B (regression acquisition), Annex C (NMR alternative) and precision data in Annex A.

Applications

Quality control and batch verification of S‑SBR in rubber and tire manufacturing
Polymer synthesis monitoring and process optimization for solution‑polymerized SBR
Supplier qualification, acceptance testing and material specification compliance
R&D and failure analysis where microstructure affects performance (rolling resistance, wear, etc.)

Who should use this standard

Rubber and tire manufacturers, QC laboratories, polymer chemists, materials characterization labs, and regulatory/standards bodies involved in rubber testing and specification.

Related standards

ISO 1795 - Rubber, raw natural and raw synthetic - Sampling and preparative procedures
ISO 1382 - Rubber - Vocabulary
Other parts of the ISO 21561 series covering complementary methods (e.g., NMR described in Annex C)

Keywords: ISO 21561-2:2024, SBR microstructure, S‑SBR, FTIR ATR method, styrene content, vinyl trans cis, rubber testing, ATR‑FTIR rubber analysis.

ISO 21561-2:2024 PDF

Технические детали

Abstract

Overview

Key topics and technical requirements

Applications

Who should use this standard

Related standards

Похожие стандарты

Abstract

Overview

Key topics and technical requirements

Applications

Who should use this standard

Related standards

Похожие стандарты

Rubber, raw natural and raw synthetic — Sampling and further preparative procedures

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