EN ISO 11401:1998

SLOVENSKI STANDARD
01-maj-2000
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Plastics - Phenolic resins - Separation by liquid chromatography (ISO 11401:1993)
Kunststoffe - Phenolharze - Trennung durch Flüssigchromatographie (ISO 11401:1993)
Plastiques - Résines phénoliques - Séparation par chromatographie en phase liquide
(ISO 11401:1993)
Ta slovenski standard je istoveten z: EN ISO 11401:1998
ICS:
83.080.10 Duromeri Thermosetting materials
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

ISO
STANDARD 11401
First edition
1993-12-01
- Phenolic resins - Separation
Plastics
by liquid chromatography
- R&ines phbnoliques - Separation par Chromatographie en
Plas tiques
Phase liquide
Reference number
ISO 11401:1993(E)
Foreword
ISO (the Wernational 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. Esch 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 11401 was prepared by Technical Committee
lSO/TC 61, Plastics, Sub-Committee SC 12, Thermosetting materials.
Later, this International Standard will become part of a general Standard
concerning liquid chromatography.
0 ISO 1993
All rights reserved. No part of this publication may be reproduced or utilized in any form or
by any means, electronie or mechanical, including photocopying and microfilm, without per-
mission in writing from the publisher.
International Organization for Standardization
Case Postale 56 0 CH-121 ‘1 GenGve 20 0 Switzerland
Printed in Switzerland
ii
ISO 1~401:1993(E)
INTERNATIONAL STANDARD
- Phenolic resins - Separation by liquid
Plastics
chromatography
2 Normative references
1 Scope
The following Standards contain provisions which,
1.1 This International Standard specifies chromato-
through reference in this text, constitute provisions
graphic methods for the Separation of phenolic resins
of this International Standard. At the time of publi-
into their component compounds. Separation takes
cation, the editions indicated were valid. All Standards
place according to molecular weight and/or polarity.
are subject to revision, and Parties to agreements
based on this International Standard are encouraged
There are various liquid chromatographic methods:
to investigate the possibility of applying the most re-
cent editions of the Standards indicated below.
A: Gel-permeation chromatography
Members of IEC and ISO maintain registers of cur-
rently valid International Standards.
liquid chromatography on
B: High-performance
polar columns
ISO 472:1988, Plastics - Vocabulary.
liquid chromatography on
Ce l-ligh-performance
ISO 10082:199”1, Plastics - Phenolic resins - Defi-
non-polar columns
nitions and test methods.
lt is possible to separate a phenolic resin into its
components according to molecular size using
3 Definitions
method A (gel-permeation chromatography). Whereas
free Phenol and the sum of the dihydro-
For the purposes of this International Standard, the
xydiphenylmethanes (in novolaks) and various
following definitions apply.
methylolphenols (in resols) are quantitatively separ-
ated in this procedure, high-molecular-weight compo-
3.1 phenolic resin: Generally, a class of resins
nents of the resins are only incompletely separated
made by the polycondensation of Phenol, its
due to the multitude of isomers.
homologues and/or derivatives, with aldehydes or ke-
tones. [ISO 4721
Methods B and C (high-performance liquid chroma-
tography) separate the compounds in the resin ac-
3.2 novolaks: Non-self-curing, soluble, fusible
cording to molecular weig ht and polarity.
phenolic resins that remain stable when stored, the
Molecular-weight effects predominate on polar sta-
Phenol nuclei of which are Iinked primarily by
tionary phases (method B), and the effect of polarity
methylene bridges. Novolaks tan be made to react
on non-polar stationary phases (method C). These
further and crosslink by the addition of hardeners;
methods also allow quantitative determination of in-
heating is also usually necessary. [ISO 10082]
dividual low-molecular-weight resin components. Be-
cause of the different resin solubilities, method B is
See also novolak in ISO 472.
more suitable for novolaks and method C for resols.
3.3 resols: Soluble, fusible phenolic resins which, in
contrast to novolaks, contain methylol groups and
1.2 The methods are applicable to phenolic resins
methylene-ether and sometimes also methylene-
that are soluble in the solvents and solvent blends
amine bridges. Resols are self-curing; they crosslink
used.
into insoluble products when heated and/or mixed
with catalysts, without addition of further reaction
1.3 This test is useful for characterization of pro-
components. Resols are perishable and tan be stored
ducts and for research.
for a limited time only. [ISO 100821
ISO 11401:1993(E)
4.1.5 Test conditions
See also resol in ISO 472.
Temperature: room temperature
4 Test methods
Carrier: tetrahydrofuran
4.1 Method A - Gel-permeation
Flow rate: 1 ml/min
chromatography
Injection volume: 20 pl
NOTE 1 The reagents, apparatus and test conditions
given are examples. Others may be used if similar or better
Detector: UV detector at 254 nm or 280 nm, or
results are obtained.
refractometer
4.1.1 Principle
4.1.6 Evaluation of results
A test Sample of the phenolic resin is dissolved in a
Exact calibration for determination of the molecular-
suitable solvent and the molecular-weight distribution
weight distribution is difficult since the phenolic
is determined by Separation on columns with polymer
hydroxyl groups add to tetrahydrofuran, although this
gels having different pore diameters.
addition is incomplete in long-chain molecules due to
steric hindrance.
4.1.2 Reagents
Qualitative evaluation may be carried ou
...