EN ISO 9369:1997

SLOVENSKI STANDARD
01-maj-1999
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Plastics - Basic materials for polyurethanes - Pure isocyanates - Analysis of isocyanate
groups (ISO 9369:1997)
Kunststoffe - Ausgangstoffe für Polyurethane - Reine Isocyanate - Analyse der
Isocyanatgruppen (ISO 9369:1997)
Plastiques - Matieres de base pour polyuréthannes - Isocyanates purs - Analyse des
groupes isocyanates (ISO 9369:1997)
Ta slovenski standard je istoveten z: EN ISO 9369:1997
ICS:
83.080.10 Duromeri Thermosetting materials
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

IS0
INTERNATIONAL
STANDARD
First edition
19970Q4- 15
Basic materials for
Plastics -
polyurethanes - Pure isocyanates -
Analysis of isocyanate groups
Plastiques - Matikres de base pour polyur&hannes - lsocyanates
- Analyse des groupes isocyanates
purs
Reference number
IS0 9369: 1997(E)
IS0 9369: 1997(E)
Foreword
IS0 (the International Organization for Standardization) is a worldwide
federation of national standards bodies (IS0 member bodies). The work of
preparing International Standards is normally carried out through IS0
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. IS0
collaborates closely with the International Electrotechnicaj Commission
(IEC) on all matters of electrotechnical standardization.
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.
International Standard IS0 9369 was prepared by Technical Committee
ISOmC 61, Plastics, Subcommittee SC 12, Thermosetting materials.
0 IS0 1997
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or utilized in any form or by any means, electronic or mechanical, including photocopying and
microfilm, without permission in writing from the publisher.
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ii
IS0 9369: 1997(E)
@ IS0
Introduction
The following types of isocyanate are commonly used in the industry as
basic materials for polyurethanes:
- isocyanates purified by rectification and their prepolymers (in particular
pure TDI - a mixture of the 2,4- and 2,6- isomers of tolylene
diisocyanate) to which this International Standard is applicable;
- non-rectified isocyanates such as unrefined MDI [methylene
di-(4-phenylisocyanate], or modified isocyanates such as isocyanates
containing adducts like carbodiimide adducts (e.g. uretonimine) and
phenol adducts for which the method specified will have to be
modified. These modifications will depend on the particular products
concerned and require agreement between purchaser and
manufacturer:
for some isocyanates, such as modified isocyanates, the
temperature of reaction with di-n-butylamine will have to be
chosen to ensure that complete conversion of the isocyanate
groups occurs (the “hot” method);
for unrefined samples, which generally contain acidic materials,
the results must be corrected for any acidic materials present in
the unrefined samples since the method involves an acid-base
titration.
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IS0 9369: 1997(E)
INTERNATIONAL STANDARD @ IS0
- Basic materials for polyurethanes -
Plastics
Pure isocyanates - Analysis of isocyanate groups
WARNING - lsocyanates shall be handled with care. lnhalation shall be avoided. Persons handling these
chemicals shall wear safety glasses and gloves, and the workplace shall be well ventilated.
1 Scope
This International Standard specifies a method for the analysis of the isocyanate groups in pure isocyanates (in
particular pure TDI and pure MDI) and their prepolymers.
2 Normative reference
The following standard contains provisions which, through reference in this text, constitute provisions of this
International Standard. At the time of publication, the edition indicated was valid. All standards are subject to
revision, and parties to agreements based on this International Standard are encouraged to investigate the
possibility of applying the most recent edition of the standard indicated below. Members of IEC and IS0 maintain
registers of currently valid International Standards.
IS0 760:1978, Determination of water - Karl Fischer method (General method).
3 Definitions
For the purposes of this International Standard, the following definitions apply:
3.1 isocyanate concentration: The amount of isocyanate in a product, expressed in one of the following three
ways:
3.1.1 isocyanate equivalent: The number of isocyanate (NCO) groups per kilogram of product (for calculation,
see 8.1).
3.1.2 isocyanate percentage: The percentage by mass of a specific pure isocyanate compound in a product (for
calculation, see 8.2).
3.1.3 isocyanate-group percentage: The percentage by mass of the isocyanate (NCO) groups in a product (for
calculation, see 8.3).
0 IS0
IS0 9369: 1997(E)
4 Principle
The isocyanate groups in a test portion of product are reacted with excess di-n-butylamine at room temperature to
form the corresponding substituted urea:
R-N=C=O -I- (C4H&NH w R - N - C - N(C4H&
I II
H 0
The excess amine is then neutralized by titration with hydrochloric acid:
(C4H&NH + HCI w (C4H& - NH*+ CI-
and the isocyanate concentration calculated.
5 Reagents
5.1 Toluene, reagent grade or equivalent, kept over a 0,4 nm molecular sieve.
Prior to use, activate the molecular sieve by heating at 400 “C for 4 h. The water content of t
...