ISO 21461:2006

Rubber — Determination of the aromaticity of oil in vulcanized rubber compounds

ISO 21461:2006 provides a method for the selective determination of polyaromaticity of oil in vulcanized rubber compounds. The method is based on nuclear magnetic resonance (NMR) spectrometry.

Caoutchouc — Détermination de l'aromaticité des huiles dans les mélanges vulcanisés

General Information

• Status: Withdrawn
• Publication Date: 23-Mar-2006
• Withdrawal Date: 23-Mar-2006
• ICS: 83.040.10 - Latex and raw rubber
• Technical Committee: ISO/TC 45/SC 3 - Raw materials (including latex) for use in the rubber industry
• Drafting Committee: ISO/TC 45/SC 3 - Raw materials (including latex) for use in the rubber industry
• Current Stage: 9599 - Withdrawal of International Standard
• Completion Date: 24-Feb-2009

Relations

• Revised: ISO 21461:2009 - Rubber — Determination of the aromaticity of oil in vulcanized rubber compounds
• Effective Date: 18-Dec-2008

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 21461
First edition
2006-04-01

Rubber — Determination of the
aromaticity of oil in vulcanized rubber
compounds
Caoutchouc — Détermination de l'aromaticité des huiles dans les
mélanges vulcanisés



Reference number
ISO 21461:2006(E)
©
ISO 2006

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ISO 21461:2006(E)
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©  ISO 2006
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ii © ISO 2006 – All rights reserved

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ISO 21461:2006(E)
Contents Page
Foreword. iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions. 1
4 Reagents and materials . 1
5 Apparatus . 2
6 Procedure . 2
7 Calculation. 4
8 Precision. 5
9 Test report . 5
1
Annex A (informative) H NMR spectra of extracts from compounds containing aromatic oil
(Figures A.1 and A.3) and MES oil (Figures A.2 and A.4) . 6
1
Annex B (informative) H NMR analysis results for typical rubber compounds (those used for the
interlaboratory trial described in Clause 8) . 8

© ISO 2006 – All rights reserved iii

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ISO 21461:2006(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.
Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.
ISO 21461 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee
SC 3, Raw materials (including latex) for use in the rubber industry.

iv © ISO 2006 – All rights reserved

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INTERNATIONAL STANDARD ISO 21461:2006(E)

Rubber — Determination of the aromaticity of oil in vulcanized
rubber compounds
WARNING — Persons using this International Standard should be familiar with normal laboratory
practice. This standard does not purport to address all the safety problems, if any, associated with its
use. It is the responsibility of the user to establish appropriate safety and health practices and to
ensure compliance with any national regulatory conditions.
1 Scope
This International Standard provides a method for the selective determination of polyaromaticity of oil in
vulcanized rubber compounds. The method is based on nuclear magnetic resonance (NMR) spectrometry.
2 Normative references
The following referenced documents are indispensable for the application 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.
ISO 1407, Rubber — Determination of solvent extract
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
polycyclic aromatic hydrocarbon
PAH
organic compound consisting of two or more aromatic rings, certain carbon atoms of which are common to
two or three rings
4 Reagents and materials
All reagents shall be of recognized analytical grade unless otherwise specified.
4.1 Extraction solvent
4.1.1 Acetone.
4.2 Sample preparation reagents
4.2.1 n-Hexane.
4.2.2 Methylene chloride.
4.2.3 Nitrogen, purity > 99,9 %, for protecting the extract from oxidation during drying.
© ISO 2006 – All rights reserved 1

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ISO 21461:2006(E)
4.2.4 CDCl , 99,9 %, NMR grade.
3
4.2.5 Hexamethyldisiloxane (HMDS), 99,5 %, NMR grade, or tetramethylsilane (TMS), 99,5 %, NMR
grade.
5 Apparatus
5.1 Analytical balance, accurate to 0,1 mg.
5.2 Extraction apparatus, as specified in ISO 1407.
5.3 Steam bath.
5.4 Extract purification apparatus, consisting of the items specified in 5.4.1 to 5.4.5:
3 3 3 3
5.4.1 2 cm , 5 cm and 25 cm or 30 cm syringes, with conical end fittings, compatible with solid-phase
extraction (SPE) columns for manual purification operations.
1)
5.4.2 SPE cartridge containing 500 mg of silica gel.
5.4.3 Laboratory glassware.
5.4.4 (Optional) Solid-phase extraction equipment, connected to a vacuum pump, for simultaneous
purification of many extracts.
5.4.5 Disposable needles.
5.5 NMR spectrometer, at least 200 MHz, preferably with the following acquisition parameters:
1
probe: H;
pulse phase: 30°;
spectral width: − 2 ppm to + 12 ppm;
number of scans: 256;
relaxation delay: 2 s.
6 Procedure
6.1 Sample extraction
6.1.1 The laboratory sample shall be of sufficient size to provide at least 350 mg of extracted oil.
6.1.2 Pass the sample between the rolls of a laboratory mill to reduce its thickness to less than 0,7 mm or,
alternatively, cut the sample in pieces smaller than 1 mm × 1 mm × 2 mm.
6.1.3 Wrap the sample in a small filter paper and insert it in the extractor (5.2) or fill the extractor with the
small cut pieces. Fill the flask of the extractor with acetone (4.1.1) and extract for 8 h.

1) VARIAN BOND ELUT JR-SI, 500 mg, part number 12162037B, is an example of a suitable product available
commercially. This information is given for the convenience of users of thi
...