ISO 15064:2004

Plastics — Aromatic isocyanates for use in the production of polyurethanes — Determination of the isomer ratio in toluenediisocyanate

ISO 15064:2004 specifies methods for the measurement of toluene-2,6-diisocyanate in mixtures of the 2,4- and 2,6-isomers. Two methods based on infrared spectroscopy are required to give accurate results over a broad range of isomer concentrations. Method A is applicable to TDI samples containing 5 % to 95 % of the 2,6-isomer. Method B is applicable to TDI samples containing 0 % to 5 % of the 2,6-isomer. Both methods are based on the quantitative measurement of absorption bands arising from out-of-plane C-H deformation vibrations of the aromatic ring at 810 cm-1 and 782 cm-1.

Plastiques — Isocyanates aromatiques pour utilisation dans la production de polyuréthannes — Détermination du rapport des isomères dans le diisocyanate de toluène

General Information

• Status: Withdrawn
• Publication Date: 08-Aug-2004
• Withdrawal Date: 08-Aug-2004
• ICS: 83.080.10 - Thermosetting materials
• Technical Committee: ISO/TC 61/SC 12 - Thermosetting materials
• Drafting Committee: ISO/TC 61/SC 12 - Thermosetting materials
• Current Stage: 9599 - Withdrawal of International Standard
• Completion Date: 24-Nov-2010

Relations

• Revised: ISO 15064:2010 - Plastics — Aromatic isocyanates for use in the production of polyurethanes — Determination of the isomer ratio in toluenediisocyanate
• Effective Date: 03-Jul-2010

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 15064
First edition
2004-08-15

Plastics — Aromatic isocyanates for use
in the production of polyurethanes —
Determination of the isomer ratio in
toluenediisocyanate
Plastiques — Isocyanates aromatiques pour utilisation dans la
production de polyuréthannes — Détermination du rapport des
isomères dans le diisocyanate de toluène




Reference number
ISO 15064:2004(E)
©
ISO 2004

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ISO 15064:2004(E)
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ii © ISO 2004 – All rights reserved

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ISO 15064:2004(E)
Contents Page
Foreword. iv
Introduction . v
1 Scope. 1
2 Normative references. 1
3 Terms and definitions. 1
4 Sampling. 2
5 Principle. 2
6 Reagents. 2
7 Apparatus. 3
8 Test conditions. 3
9 Method A — Samples containing 5 % to 95 % of 2,6-TDI. 3
10 Method B — Samples containing 0 % to 5 % of 2,6-TDI. 6
Annex A (normative) Calibration curves. 8

© ISO 2004 – All rights reserved iii

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ISO 15064:2004(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 15064 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12, Thermosetting
materials.
iv © ISO 2004 – All rights reserved

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ISO 15064:2004(E)
Introduction
No International Standard for the determination of isomer contents of toluenediisocyanate (TDI) has been
published. This International Standard is based on infrared spectroscopy and consists of two test methods
that can be used to determine the 2,4- and 2,6-isomer contents of commercially important
toluenediisocyanates over a broad range of isomer concentrations. It is important to know the isomer content
of TDI since the isomers have different reaction rates, and the processing and properties of polyurethane
systems, especially flexible polyurethane foams, may be significantly affected. This method is based on work
done in the Bayer Central Analytical Department (Leverkusen) in the early 1960s, and was originally published
as part of ASTM D 1638. It is now designated ASTM D 4660, Standard Test Methods for Polyurethane Raw
Materials: Determination of the Isomer Content of Toluenediisocyanate.

© ISO 2004 – All rights reserved v

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INTERNATIONAL STANDARD ISO 15064:2004(E)

Plastics — Aromatic isocyanates for use in the production
of polyurethanes — Determination of the isomer ratio in
toluenediisocyanate
WARNING — Persons using this International Standard should be familiar with normal laboratory
practice. This standard does not purport to address all of the safety problems, if any, associated with
its use. It is the responsibility of the user of this standard to establish appropriate safety and health
practices and to ensure compliance with any national regulatory conditions prior to use.
1 Scope
This International Standard specifies methods for the measurement of toluene-2,6-diisocyanate in mixtures of
the 2,4- and 2,6-isomers. Two methods based on infrared spectroscopy are required to give accurate results
over a broad range of isomer concentrations. Method A is applicable to TDI samples containing 5 % to 95 %
of the 2,6-isomer. Method B is applicable to TDI samples containing 0 % to 5 % of the 2,6-isomer. Both
methods are based on the quantitative measurement of absorption bands arising from out-of-plane C–H
−1 −1
deformation vibrations of the aromatic ring at 810 cm and 782 cm (12,3 µm and 13,8 µm).
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 648, Laboratory glassware — One-mark pipettes
ISO 4787, Laboratory glassware — Volumetric glassware — Methods for use and testing of capacity
ISO 6353-2, Reagents for chemical analysis — Part 2: Specifications — First series
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.
3.1
isomer
a compound having the same percentage composition and molecular mass as another compound, but
differing in chemical structure and properties
3.2
isomer content
the amount of an isomer expressed as a mass percentage of the total isomer amount
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ISO 15064:2004(E)
3.3
TDI
toluenediisocyanate
3.4
polyurethane
a polymer prepared by the reaction of an organic di- or polyisocyanate with compounds containing two or
more hydroxyl groups
4 Sampling
Since organic isocyanates react with atmospheric moisture, take special precautions in sampling. Usual
sampling methods (for example, sampling an open drum with a thief), even when conducted rapidly, can
cause contamination of the sample with insoluble ureas; therefore, blanket the sample with a dry inert gas
(e.g. nitrogen, argon or dried air) at all times.
WARNING — Organic isocyanates are hazardous when absorbed through the skin, or when the
vapours are breathed in. Provide adequate ventilation and wear protective gloves and eyeglasses.
5 Principle
5.1 Method A
In method A (5 % to 95 % 2,6-isomer), the infrared spectrum of a cyclohexane solution of the sample is
−1 −1 −1
recorded in the 770 cm to 840 cm (12 µm to 13 µm) region. The absorbance ratio of the 810 cm and
−1
782 cm bands is measured and converted to % toluene-2,6-diisocyanate from a previously established
calibration curve.
5.2 Method B
−1
In Method B (0 % to 5 % 2,6-isomer), the absorbance of the 782 cm band is measured from an infrared
spectrum of an undiluted sample and then converted to % 2,6-isomer from a previously established calibration
curve.
6 Reagents
Reagent-grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that the reagents
shall conform to the specifications of ISO 6353-2. Other grades may be used, provided that it is first
determined that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the
determination.
6.1 Cyclohexane, distilled and stored over silica gel to remove traces of moisture.
6.2 Diisocyanate standards.
Pure samples of 2,4-TDI and 2,6-TDI are required for calibration. The following criteria can be used to judge
purity:
20 20
for 2,4-TDI: freezing
...