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

ISO 15064:2010 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
Replaced
Publication Date
23-Nov-2010
Withdrawal Date
23-Nov-2010
Current Stage
6060 - International Standard published
Start Date
18-Nov-2010
Completion Date
24-Nov-2010
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INTERNATIONAL ISO
STANDARD 15064
Second edition
2010-12-01
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 15064:2010(E)
ISO 2010
---------------------- Page: 1 ----------------------
ISO 15064:2010(E)
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© ISO 2010

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ii © ISO 2010 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 15064:2010(E)
Contents Page

Foreword ............................................................................................................................................................iv

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 2010 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 15064:2010(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.

This second edition cancels and replaces the first edition (ISO 15064:2004), of which it constitutes a minor

revision making the following changes:
⎯ the introduction has been deleted;
⎯ the titles of Table 2 and Table 3 have been corrected;
⎯ the repeatability limit given in 9.4.1 has been modified;

⎯ in both the repeatability and the reproducibility statements in 10.4.1, “2,4-TDI” has been replaced by

“2,6-TDI”;
⎯ the clarity of the key to Figure A.2 has been improved;
⎯ the clarity of the title of Figure A.3 has been improved.
iv © ISO 2010 – All rights reserved
---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 15064:2010(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 — Single-volume pipettes

ISO 4787, Laboratory glassware — Volumetric instruments — Methods for testing of capacity and for use

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

compound having the same percentage composition and molecular mass as another compound, but differing

in chemical structure and properties
3.2
isomer content
amount of an isomer expressed as a mass percentage of the total isomer amount
3.3
TDI
toluenediisocyanate
© ISO 2010 – All rights reserved 1
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ISO 15064:2010(E)
3.4
polyurethane

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

782 cm bands is measured and converted to % toluene-2,6-diisocyanate from a previously established

calibration curve.
5.2 Method B

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 point = 22,0 °C; n = 1,567 81; ρ = 1,218 6;
D 4
20 20
for 2,6-TDI: freezing point = 18,2 °C; n = 1,571 11; ρ = 1,227 0.
D 4

The diisocyanates can be prepared by phosgenating the corresponding pure amines and vacuum-distilling the

products. Since these diisocyanates will react with moisture and can discolour in the presence

...

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