EN ISO 3001:1999

Plastics - Epoxy compounds - Determination of epoxy equivalent (ISO 3001:1999)

This International Standard specifies a method for the determination of the epoxy equivalent and is applicable to all epoxy compounds. In the case of epoxyamines, it is necessary to apply the modification specified in annex A.

Kunststoffe - Epoxid-Verbindungen - Bestimmung des Epoxid-Äquivalents (ISO 3001:1999)

Diese Internationale Norm beschreibt ein Verfahren zur Bestimmung des Epoxid- Äquivalents und ist anwendbar auf alle Epoxid-Verbindungen; Bei Epoxidaminen ist es erforderlich, die im Anhang beschriebenen Änderungen zu berücksichtigen.

Plastiques - Compositions époxydiques - Détermination de l'équivalent époxy (ISO 3001:1999)

Polimerni materiali - Epoksidne spojine - Določanje epoksidnega ekvivalenta (ISO 3001:1999)

General Information

• Status: Published
• Publication Date: 14-Feb-1999
• Withdrawal Date: 30-Aug-1999
• ICS: 83.080.01 - Plastics in general
• Technical Committee: CEN/TC 249 - Plastics
• Drafting Committee: CEN/TC 249/SC 1/WG 13 - Thermosets
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 15-Feb-1999
• Completion Date: 15-Feb-1999
• Ref Project: SIST EN ISO 3001:2000 - Plastics - Epoxy compounds - Determination of epoxy equivalent (ISO 3001:1999)

Standards Content (Sample)

SLOVENSKI STANDARD
01-maj-2000
3ROLPHUQLPDWHULDOL(SRNVLGQHVSRMLQH'RORþDQMHHSRNVLGQHJDHNYLYDOHQWD,62

Plastics - Epoxy compounds - Determination of epoxy equivalent (ISO 3001:1999)
Kunststoffe - Epoxid-Verbindungen - Bestimmung des Epoxid-Äquivalents (ISO
3001:1999)
Plastiques - Compositions époxydiques - Détermination de l'équivalent époxy (ISO
3001:1999)
Ta slovenski standard je istoveten z: EN ISO 3001:1999
ICS:
83.080.10 Duromeri Thermosetting materials
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

INTERNATIONAL ISO
STANDARD 3001
Fourth edition
1999-02-15
Plastics — Epoxy compounds —
Determination of epoxy equivalent
Plastiques — Compositions époxydiques — Détermination de l'équivalent
époxy
A
Reference number
ISO 3001:1999(E)
ISO 3001:1999(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.
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 ISO 3001 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 12,
Thermosetting materials.
This fourth edition cancels and replaces the third edition (ISO 3001:1997), which has been technically revised.
Annex A forms an integral part of this International Standard.
© ISO 1999
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means, electronic
or mechanical, including photocopying and microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case postale 56 • CH-1211 Genève 20 • Switzerland
Internet [e-mail]
Printed in Switzerland
ii
INTERNATIONAL STANDARD  © ISO ISO 3001:1999(E)
Plastics — Epoxy compounds — Determination of epoxy
equivalent
1 Scope
This International Standard specifies a method for the determination of the epoxy equivalent and is applicable to all
epoxy compounds. In the case of epoxyamines, it is necessary to apply the modification specified in annex A.
2 Definitions
For the purposes of this International Standard, the following definitions apply.
2.1
epoxy equivalent
the mass of resin, in grams, which contains one mole of epoxy groups
2.2
epoxy index
the number of moles of epoxy groups contained in 1 kg of resin
3 Principle
The epoxy groups in a test portion are reacted with nascent hydrogen bromide produced by the action of 0,1 mol/l
standard volumetric perchloric acid solution on tetraethylammonium bromide. The end-point is determined either
using crystal violet as indicator or by a potentiometric method.
4 Reagents
During the analysis, use only reagents of recognized analytical grade.
4.1  Glacial acetic acid.
4.2  Acetic anhydride, purity > 96 %.
4.3  Chloroform.
4.4  Potassium hydrogen phthalate.
4.5  Crystal violet, indicator solution.
Dissolve 100 mg of crystal violet in 100 ml of glacial acetic acid (4.1).
4.6  Perchloric acid, 0,1 mol/l standard volumetric solution.
© ISO
ISO 3001:1999(E)
4.6.1  Preparation
Add 8,5 ml of a 70 % (m/m) aqueous solution of perchloric acid to a solution consisting of a mixture of 500 ml of
glacial acetic acid (4.1) and 30 ml of acetic anhydride (4.2). Make up to 1 000 ml with glacial acetic acid and mix
thoroughly.
4.6.2  Standardization
WARNING — The use of safety goggles and a safety screen is recommended.
Standardize this solution by titrating it against 200 mg of potassium hydrogen phthalate (4.4) — previously dried, if
necessary, for 2 h at 120 °C — dissolved in 20 ml of glacial acetic acid (4.1) and 10 ml of chloroform (4.3), using
crystal violet indicator solution (4.5) or a potentiometric titration apparatus (5.1).
Carry out the end-point determination using 4 to 6 drops of crystal violet solution, titrating until a stable green colour
is obtained, or carry out this procedure using a potentiometric titration apparatus. If a potentiometric method is used
to determine the epoxy equivalent, it is necessary to use the same method for the standardization of the perchloric
acid. Note the temperature t of the standard volumetric solution.
s
4.6.3  Calculation of the concentration
Calculate the concentration c of the perchloric acid solution (4.6.1), in moles per litre, by the following equation,
rounding to four places of decimals:
m
c=
()VV−× 0,20422
where
m is the mass, in grams, of potassium hydrogen phthalate used;
V is the volume, in millilitres, of perchloric acid solution (4.6.1) used in the blank test;
V is the volume, in millilitres, of perchloric acid solution (4.6.1) used in the determination.
4.7  Tetraethylammonium bromide, reagent solution.
Dissolve 100 g of tetraethylammonium bromide in 400 ml of glacial acetic acid (4.1). Add a few drops of crystal
violet solution (4.5). If it changes colour, bring it back to the original (blue-green) colour with standard volumetric
perchloric acid solution (4.6).
For some epoxy compounds of low reactivity, the use of tetrabutylammonium iodide is advised, either as the solid or
as a 10 % solution in chloroform. In this case, light shall be excluded as much as possible. Solutions of
tetrabutylammonium iodide in chloroform are unstable and shall be freshly prepared for each titration.
5 Apparatus
5.1  Potentiometric titration apparatus, equipped with a silver el
...