Plastics - Phenolic resins - Determination of the gel time at a given temperature using automatic apparatus (ISO 9396:1997)

Migrated from Progress Sheet (TC Comment) (2000-07-10): This document will revised EN ISO 9396:1995 . The reference document is ISO 9396 ++ :1997 glg/1997-08-20 ++ new Tc forecast in BP Bli 991026

Kunststoffe - Phenolharze - Bestimmung der Gelierzeit mit einem Automaten unter spezifischen Bedingungen (ISO 9396:1997)

Diese Internationale Norm beschreibt ein Verfahren zur Bestimmung der Gelierzeit von Phenolharzen bei vorgegebener Temperatur durch Einsatz eines automatischen Gerätes unter spezifischen Bedingungen. Die Prüftemperaturen sind 100°C, 130°C und 150 °C. Bei der Methode wird ein sich vertikal (auf und ab) bewegender Meßstempel verwendet. Dieses Verfahren kann für folgende Phenolharztypen angewendet werden: - flüssige Resole; - feste Resole mit niedrigem Schmelzpunkt. Pulverharze mit kurzer Gelierzeit, wie Mischungen aus Novolak und Hexamethylentetramin, sind für dieses Bestimmungsverfahren nicht geeignet.

Plastiques - Résines phénoliques - Détermination de la durée de gélification à une température donnée sur appareils automatiques (ISO 9396:1997)

La présente Norme internationale prescrit une méthode pour la détermination du temps de gélification à une température donnée, à l'aide d'un appareil automatique, dans des conditions spécifiées. Les températures d'essai sont de 100 °, 130 ° et 150 °. La méthode prescrite utilise un plongeur animé d'un mouvement vertical alternatif.  Cette méthode s'applique aux résines phénoliques:  - liquides du type résol;  - solides du type résol à bas point de fusion.  Les résines en poudre ayant un court temps de gélification (par exemple des mélanges novolaques avec de l'hexaméthylène tétramine) pour lesquelles la réticulation commence dès que la fusion démarre, de sorte que la résine fondue et déjà trop visqueuse pour être apte à réagir de manière satisfaisante dans le tube à essais, ne peuvent pas faire l'objet d'un mesurage. Il y a également des difficultés pour effectuer des mesurages sur des résines contenant une quantité importante de solvants à bas points d'ébullition parce qu'un processus d'ébullition et de distillation se produit en recouvrement avec le processus de durcissement. Il peut être intéressant de déterminer la durée de gélification en présence d'un catalyseur. Celui-ci doit être ajouté dans des proportions bien définies. Le type de catalyseur et son traitement doivent être mentionnés dans le rapport d'essai.

Polimerni materiali - Fenolne smole - Ugotavljanje časa želiranja pri določeni temperaturi z avtomatskim aparatom (ISO 9396:1997)

General Information

Status
Published
Publication Date
19-Sep-2000
Withdrawal Date
30-Mar-2001
Technical Committee
Drafting Committee
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
20-Sep-2000
Completion Date
20-Sep-2000

Relations

Overview

EN ISO 9396:2000 defines a standardized test method for determining the gel time of phenolic resins (resols) at a given temperature using an automatic reciprocating-plunger apparatus. The procedure is intended for liquid resols and low-melting solid resols and specifies controlled test temperatures (100 °C, 130 °C and 150 °C). This method supports quality control (QC), cure monitoring and comparative evaluation of thermosetting materials.

Keywords: EN ISO 9396:2000, gel time, phenolic resins, resols, reciprocating-plunger, automatic apparatus, QC, cure control

Key Topics

  • Scope and applicability: Applies to liquid resols and solid resols with low melting points. Not suitable for powders or resins that boil or distil during cure or those that crosslink immediately on fusion.
  • Apparatus essentials:
    • Automatic reciprocating-plunger apparatus with a plunger cycle typically 10 s (frequency to be reported).
    • Thermostatically controlled bath (max 200 °C) with temperature tolerance ±0.5 °C and suitable bath liquid (e.g., silicone oil).
    • Plunger: metal wire with helix; test tube: specified mass and dimensions; metal ring to hold tube in bath.
  • Test conditions: Typical test temperatures are 100 °C, 130 °C and 150 °C. Test portions are 5 g (±0.1 g) of resin, and tests are performed in duplicate unless otherwise agreed.
  • Principle: The plunger performs a reciprocating vertical motion. Gel time is recorded when the specimen viscosity causes the test tube to move with the plunger and the automatic apparatus stops.
  • Precision:
    • Repeatability: absolute difference expected to lie within about 2–8 % (95 % probability) depending on resin type.
    • Reproducibility: absolute difference expected to lie within about 20 % (95 % probability) across different laboratories.

Applications

  • Routine QC of phenolic resol production and incoming raw materials.
  • Process control for molding, laminating and adhesive cure behavior where gel time at a set temperature is critical.
  • Comparative testing when screening catalysts or evaluating formulation changes (catalyst type and proportion must be reported).
  • Laboratory verification of cure schedules and formulation tuning for thermosetting systems.

Related Standards

  • ISO 9396:1997 (international reference edition cited by EN ISO 9396:2000).
  • Other ISO/CEN methods for thermosetting materials and cure measurement (refer to TC 61 and SC 12 documents for complementary test methods).

Reporting Requirements

The test report shall include a reference to this standard, sample identification, the arithmetic mean gel time (minutes to 0.1 min), test temperature, plunger frequency and any catalyst or special treatment applied.

This content summarizes the practical value and test elements of EN ISO 9396:2000 for engineers and laboratory personnel involved in thermoset testing and quality assurance.

Standard
EN ISO 9396:2001
English language
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Standards Content (Sample)


SLOVENSKI STANDARD
01-junij-2001
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Plastics - Phenolic resins - Determination of the gel time at a given temperature using
automatic apparatus (ISO 9396:1997)
Kunststoffe - Phenolharze - Bestimmung der Gelierzeit mit einem Automaten unter
spezifischen Bedingungen (ISO 9396:1997)
Plastiques - Résines phénoliques - Détermination de la durée de gélification a une
température donnée sur appareils automatiques (ISO 9396:1997)
Ta slovenski standard je istoveten z: EN ISO 9396:2000
ICS:
83.080.10 Duromeri Thermosetting materials
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

INTERNATIONAL IS0
STANDARD 9396
Second edition
1997-07- 15
- Phenolic resins -
Plastics
Determination of the gel time of resols
under specific conditions using automatic
apparatus
P/as tiques - Rksines ph&oliques - Dktermina tion du temps
de ghlification des r&ok dans des conditions spkcifiques sur appareils
automa tiques
Reference number
IS0 9396:1997(E)
IS0 9396: 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 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 IS0 9396 was prepared by Technical Committee
lSO/TC 61, Plastics, Subcommittee SC 12, Thermosetting materials.
This second edition cancels and replaces the first edition
(IS0 9396:1989), in which method A (which used a rotary stirrer) has been
deleted and a precision clause added.
0 IS0 1997
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 l CH-1211 Geneve 20 l Switzerland
Internet central @ isoch
x.400 c=ch; a=400net; p=iso; o=isocs; s=central
Printed in Switzerland
ii
INTERNATIONAL STANDARD @ Iso
IS0 9396: 1997(E)
Plastics - Phenolic resins - Determination of the gel time
of resols under specific conditions using automatic apparatus
l.Scope
This International Standard specifies a method for determining the gel time of
phenolic resins at a given temperature, using automatic apparatus under specified
conditions. The test temperatures are 100 “C, 130 “C and 150 “C.
The method specified employs a plunger driven to carry out a reciprocating vertical
motion. ,
This method applies to the following types of phenolic resin:
- liquid resols
- solid resols with low melting points
Powdered resins with a short gel time, such as mixtures of novolak and
hexamethylenetetramine, do not lend themselves to this type of determination. Such
resins crosslink as soon as fusion starts and become too viscous in the test tube to give
meaningful results. Resins containing large amounts of a solvent with a low boiling point
are especially unsuitable for this type of determination. With such resins, a boiling and
distillation process takes place as the resin hardens.
It might be of interest to determine the time taken for the resin to gel
...

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Frequently Asked Questions

EN ISO 9396:2000 is a standard published by the European Committee for Standardization (CEN). Its full title is "Plastics - Phenolic resins - Determination of the gel time at a given temperature using automatic apparatus (ISO 9396:1997)". This standard covers: Migrated from Progress Sheet (TC Comment) (2000-07-10): This document will revised EN ISO 9396:1995 . The reference document is ISO 9396 ++ :1997 glg/1997-08-20 ++ new Tc forecast in BP Bli 991026

Migrated from Progress Sheet (TC Comment) (2000-07-10): This document will revised EN ISO 9396:1995 . The reference document is ISO 9396 ++ :1997 glg/1997-08-20 ++ new Tc forecast in BP Bli 991026

EN ISO 9396:2000 is classified under the following ICS (International Classification for Standards) categories: 83.080 - Plastics. The ICS classification helps identify the subject area and facilitates finding related standards.

EN ISO 9396:2000 has the following relationships with other standards: It is inter standard links to EN ISO 9396:1995. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.

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