EN ISO 11409:1998

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kunststoffe - Phenolharze - Bestimmung der Reaktionswärmen und -temperaturen durch dynamische Differenzkalorimetrie (ISO 11409:1993)Plastiques - Résines phénoliques - Détermination des chaleurs et températures de réaction par calorimétrie différentielle a balayage (ISO 11409:1993)Plastics - Phenolic resins - Determination of heats and temperatures of reaction by differential scanning calorimetry (ISO 11409:1993)83.080.10DuromeriThermosetting materialsICS:Ta slovenski standard je istoveten z:EN ISO 11409:1998SIST EN ISO 11409:2000en01-maj-2000SIST EN ISO 11409:2000SLOVENSKI
STANDARD
INTERNATIONAL STANDARD ISO 11409 First edition 1993-12-01 Plastics - Phenolic resins - Determination of heats and temperatures of reaction by differential scanning calorimetry Plas tiques - R&ines phenoliques - Determination des chaleurs et temp&a tures de r6action par calorime trie diffken tielle 2 balayage Reference number ISO 11409:1993(E) SIST EN ISO 11409:2000

ISO 11409:1993(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. 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 organizetions, governmental and non-governmental, in liaison with ISO, also take patt in the work. ISO collaborates closely with the International Electrotechnical Commission (1 EC) 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 11409 was prepared by Technical Committee ISO/TC 61, Plastics, Sub-Committee SC 12, Thermosetting materials. Later, this International Standard will become concerning differential scanning calorimetry. part of a general Standard Annex A of this International Standard is for information only. 63 ISO 1993 All rights reserved. No part of this publication may be reproduced or utilized in any ferm 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 Cl-l-1 2’1% Gen&ve 20 0 Switzerland Printed in Switzerland ii SIST EN ISO 11409:2000

INTERNATIONAL STANDARD ISO 11409:1993(E) Plastics - Phenolic resins - Determination of heats and temperatures of reaction by differential scanning calorimetry 1 Scope 1.1 This International Standard specifies a method for the determination of heats and temperatures of reaction of phenolic resins by differential scanning calorimetry. 1.2 The method is applicable to phenolic resins with exothermit behaviour, such as resols or mixtures of novolaks with hexamethylenetetramine or other cur- ing agents. :he characterization o 1.3 The method is useful for t products and for research. 2 Normative references The following Standards contain provisions which, through reference in this text, constitute provisions 0% this International Standard. At the time of publi- cation, the editions indicated were 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 re- cent editions of the Standards indicated below. Members of IEC and ISO maintain registers of cur- rently valid International Standards. ISO 47211988, Plastics - Vocabulary. ISO 5725:1986, Precision of test methods - Deter- mination of repeatability and reproducibility for a Standard test method by inter-laboratory tests. ISO 10082:1991, Plastics - Phenolic resins - Defi- nitions and test methods. 3 Definitions For the purposes of this International Standard, the following definitions apply. 3.1 differential scanning calorimetry (DSC): A technique whereby the differente in energy absorbed or released by a polymer and by a reference material is measured as a function of temperature and/or time while the polymer and the reference are subjected to the same temperature schedule. 3.2 phenolic resin: Generally, a class of resins made by polycondensation of Phenol, its homologues and/or derivatives, with aldehydes or ketones. [ISO 4721 3.3 novoiaks: Non-self-curing, soluble, fusible phenolic resins that remain stable when stored, the Phenol nuclei of which are linked primarily by methylene bridges. Novolaks tan be made to react further and crosslink by the addition of hardeners; heating is also usually necessary. [ISO 100821 See also novolak in ISO 472. 3.4 resob: Soluble, fusible phenolic resins which, in contrast to novolaks, contain methylol groups and methylene-ether and sometimes also methylene- amine bridges. Resols are self-curing; they crosslink into insoluble products when heated and/or mixed with catalysts, without addition of further reaction components. Resols are perishable and tan be stored for a limited time only. [ISO 100821 See also resol in ISO 472. NOTE 1 In this document, the term “heat” and “heat of reaction” used throughout the text are equivalent to the terms “enthalpy” and “enthalpy of reaction”. 4 Test method 4.1 Principle The heat flux (power) supplied to a test Sample is measured as a function of time or temperature, while 1 SIST EN ISO 11409:2000

ISO 11409:1993(E) the test Sample is subjected to a temperature sched- ule under a specified atmosphere. In practice, what is measured is the differente be- tween the heat flux supplied to a Sample holder con- taining the test Sample and the heat flux supplied to a reference holder. A reaction is marked by the release of energy from the Sample, resulting in an exothermit peak in the heating curve. Integration of the recorded peak area as a function of time gives a measure of the energy of the reaction. Observing the Position of the reaction on the temperature axis provides the necessary tem- perature information. 4.2 Materials 4.2.1 Indium, for calibration of the apparatus (sec 4.5.1). 4.3 Apparatus 4.3.1 Differential scanning calorimeter, having the following characteristics: a) heating or cooling rate of up to 10 “C/min; b) automatic recording of differential heat flow be- tween the Sample and reference material; c) sensitivity for measurement of heat flux or energy differente such that a precision of & 1 % is en- sured; d) time-base precision of &- 1 % over the time-base range from 0,l min/cm to 2,0 min/cm (10,O cm/min to 0,5 cm/min) on the Chart; e) temperature sensitivity such that the Sample tem- perature is readable to at least + 0,l “C; f) operating range preferably from 20 “C to 300 “C. 4.3.2 Area-measurement device, with an accuracy of + 0,l %. - 4.3.3 Pressure-tight Sample holders, inert to the test material, of high thermal conductivity, for exam- ple steel capsules, pressure-tight to at least 2 MPal) (see recommended design in figure 1). NOTE 2 If a differential scanning calorim
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