EN ISO 9396:1995

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kunststoffe - Phenolharze - Bestimmung der Gelierzeit mit einem Automaten bei vorgegebener Temperatur (ISO 9396:1989)Plastiques - Résines phénoliques - Détermination de la durée de gélification a une température donnée sur appareils automatiques (ISO 9396:1989)Plastics - Phenolic resins - Determination of the gel time at a given temperature using automatic apparatus (ISO 9396:1989)83.080.10DuromeriThermosetting materialsICS:Ta slovenski standard je istoveten z:EN ISO 9396:1995SIST EN ISO 9396:1999en01-maj-1999SIST EN ISO 9396:1999SLOVENSKI
STANDARD



SIST EN ISO 9396:1999



SIST EN ISO 9396:1999



SIST EN ISO 9396:1999



I NTER NATIONAL STANDARD IS0 First edition 1989-12-1 5 Plastics - Phenolic resins - Determination of the gel time at a given temperature using automatic apparatus Plastiques - Résines phénoligues - Détermination de la durée de gélification à une température donnée sur appareils automatiques Reference number IS0 9396 : 1989 (E) SIST EN ISO 9396:1999



IS0 9396 : 1989 (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, govern- mental 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 approval before their acceptance as International Standards by the IS0 Council. They are approved in accordance with IS0 procedures requiring at least 75 % approval by the member bodies voting. International Standard IS0 9396 was prepared by Technical Committee ISO/TC 61, Plastics. O IS0 1989 All rights reserved. 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 0 CH-121 1 Genève 20 O Switzerland Printed in Switzerland SIST EN ISO 9396:1999



INTERNATIONAL STANDARD IS0 9396 : 1989 (E) Plastics - Phenolic resins - Determination of the gel time at a given temperature using automatic apparatus 1 Scope This International Standard specifies two methods for deter- mining the gel time of phenolic resins at a given temperature, using automatic apparatus under specified conditions. The test temperatures are 100 OC, 130 OC and 150 OC. The two methods specified, which utilize different kinds of automatic apparatus, are : 0 - a) to carry out a rotary (spinning) motion; b) method 6 (clause 41, which employs a plunger driven to carry out a reciprocating vertical motion. method A (clause 31, which employs a glass rod driven These methods apply to the following types of phenolic resin : - liquid resols (methods A and 6); - novolak solutions containing hexamethylenetetramine (HMTA); the boiling point of the solvent must be higher than the test temperature (method A); - solid resols with low melting points (method 6). Powdered resins with a short gel time, such as mixtures of novolak and HMTA, 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 deter- mination. 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 in the presence of a catalyst. The catalyst shall be added in well defined proportions. The type of catalyst used and its treatment shall be stated in the test report. 2 Preparation of test portions 2.1 Test liquid resols as produced (method A or 6). 2.2 Test solid resols as produced (method 6). 2.3 Dissolve powdered resins (such as novolak + HMTA) in the proportions 1 : 1 (rnlrn) in ethylene glycol monoethyl ether at a temperature below 60 OC. If necessary, additional solvent may be added to dissolve the resin completely (method A). NOTE - Ethylene glycol monoethyl ether may plastify the resin and give a longer gel time. 2.4 Test solutions of novolak in high-boiling solvents con- taining HMTA as produced. If the solution does not contain HMTA, add 10 YO of HMTA to the solution, based on the novolak content (method A). 2.5 Dissolve solid novolaks in ethylene glycol monoethyl ether and add HMTA in the following proportions by mass (method A) : 10 parts of novolak; 1 part of HMTA; 11 parts of ethylene glycol monoethyl ether. 3 Method A: Apparatus with rotary stirrer 3.1 Principle In the course of polymerization, phenolic resins pass through a critical point which is manifested by an abrupt increase in the viscosity. The automatic apparatus used measures the time required to reach this point. A glass rod, placed in a test tube containing the substance to be examined, is driven to carry out a rotary movement of limited torque by an electric motor. The gel point is reached when the viscosity of the sample increases abruptly and stops the rotation of the glass rod. This causes the closure of an electric circuit, producing an audible signal. The time indicated by the timer is called the gel time at the particular temperature (method A). 3.2 Reagents 3.2.1 Solvent : Ethylene glycol monoethyl ether. (When measuring at 150 OC, ethyle
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