1、BSI Standards PublicationBS ISO 11359-1:2014Plastics Thermomechanicalanalysis (TMA)Part 1: General principlesBS ISO 11359-1:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 11359-1:2014.It supersedes BS ISO 11359-1:1999 which is withdrawn.The UK participati
2、on in its preparation was entrusted to TechnicalCommittee PRI/21, Testing of plastics.A list of organizations represented on this committee can beobtained on request to its secretary.This publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its
3、 correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 77734 9ICS 83.080.01Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and Str
4、ategy Committee on 31 January 2014.Amendments issued since publicationDate Text affectedBS ISO 11359-1:2014 ISO 2014Plastics Thermomechanical analysis (TMA) Part 1: General principlesPlastiques Analyse thermomcanique (TMA) Partie 1: Principes gnrauxINTERNATIONAL STANDARDISO11359-1Second edition2014-
5、01-15Reference numberISO 11359-1:2014(E)BS ISO 11359-1:2014ISO 11359-1:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2014All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electron
6、ic or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester.ISO copyright officeCase postale 56 CH-1211 Geneva 20Tel. + 41 2
7、2 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 11359-1:2014ISO 11359-1:2014(E) ISO 2014 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 15 Apparatus . 16 Test specimens 27 P
8、rocedure. 37.1 Calibration 37.2 Blank run 47.3 Determination . 48 Test report . 4Bibliography 5BS ISO 11359-1:2014ISO 11359-1:2014(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing Inte
9、rnational 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 wi
10、th ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives
11、, Part 1. In particular the different approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).Attention is drawn to the possibility that some of
12、the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations
13、 received (see www.iso.org/patents).Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement.For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISO
14、s adherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 61, Plastics, Subcommittee SC 5, Physical-chemical properties.This second edition cancels and replaces the first
15、 edition (ISO 11359-1:1999), which has been technically revised with the following changes: clarification that deformations shall occur under constant load; inclusion of reference to ISO 472 in Definitions and cancellation of duplicate and trivial definitions; revision of apparatus requirements foll
16、owing guidelines specified in ISO 11357-1 and update of accuracy specifications; revision of specification of temperature calibration; revision of specification of displacement and sample length measurement.ISO 11359 consists of the following parts, under the general title Plastics Thermomechanical
17、analysis (TMA): Part 1: General principles Part 2: Determination of coefficient of linear thermal expansion and glass transition temperature Part 3: Determination of penetration temperatureiv ISO 2014 All rights reservedBS ISO 11359-1:2014INTERNATIONAL STANDARD ISO 11359-1:2014(E)Plastics Thermomech
18、anical analysis (TMA) Part 1: General principles1 ScopeThis part of ISO 11359 specifies the general conditions for the thermomechanical analysis of thermoplastics and thermosetting materials, filled or unfilled, in the form of sheet or moulded parts.Thermomechanical analysis consists of the determin
19、ation of deformations of a test specimen under constant load as a function of temperature and/or time.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition cite
20、d applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 291, Plastics Standard atmospheres for conditioning and testingISO 472, Plastics VocabularyISO 11359-2, Plastics Thermomechanical analysis (TMA) Part 2: Determination of coefficien
21、t of linear thermal expansion and glass transition temperatureISO 11359-3, Plastics Thermomechanical analysis (TMA) Part 3: Determination of penetration temperature3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 472 and the following apply.3.1thermodi
22、latometrytechnique in which one dimension (or the volume) of a substance under negligible constant stress is measured as a function of temperature while the substance is subjected to a controlled temperature programmeNote 1 to entry: A distinction is made between linear thermodilatometry (in which o
23、ne dimension is measured) and volume thermodilatometry (in which the volume is measured).4 PrincipleThe deformation of a material under constant stress is measured as a function of time at a constant temperature or as a function of temperature.5 ApparatusThe components of a basic thermomechanical an
24、alyser consist of the following:5.1 Temperature-programmable furnace, capable of: ISO 2014 All rights reserved 1BS ISO 11359-1:2014ISO 11359-1:2014(E)a) generating constant heating or cooling rates for the intended measurements;b) covering a temperature range in line with the experimental requiremen
25、ts;c) maintaining the temperature variation at a given location to within 1 K over time;d) measuring the temperature with an accuracy of 1 K over time;e) maintaining a controlled purge gas atmosphere.5.2 Displacement transducer, with an accuracy of 0,1 % or better.5.3 Measurement probe, rod made of
26、a material of low thermal-expansion coefficient (e.g. silica, ceramics, quartz glass, etc.), linked mechanically to the displacement transducer, with one end in contact with the test specimen, and with a shape suited to the type of measurement.The apparatus shall include a means of compensating for
27、the probe mass, either through calibration or tarring.5.4 Load application device, shall be suitable for the intended measurement, e.g. compression, penetration, tension, flexure, etc.The magnitude of the load applied to the rod depends on the type of measurement required. It is necessary to determi
28、ne the force actually applied to the specimen.5.5 Cooling device, capable of generating and maintaining controlled and reproducible low temperatures.5.6 Inert or oxidising gas supply, type, purity, and flow rates of purge gas shall be suitable for the intended measurements.5.7 Micrometers or callipe
29、rs, with an accuracy of 2 m or better.6 Test specimensCut test specimens from a sheet or moulded article in such a way that any heating will not modify its structure. The test specimen can be of any shape but shall have a thickness suitable for the intended measurement and specimen holder.Ensure tha
30、t the lower and upper surfaces of the specimen are parallel and smooth, smoothing down if necessary with abrasive paper (e.g. No. 200 grade).NOTE Removal (smoothing) of the surface of specimens moulded or formed from some materials might change the relative amount of oriented skin layers which, in t
31、urn, might affect the mechanical response.If specimens are taken from a moulded article, report the sampling procedure used, i.e. method of extracting the specimen from the article, type of the article, and the location and orientation of specimen.Unless otherwise specified in the appropriate materi
32、al standard, condition the specimen under one of the sets of conditions specified in ISO 291.A visual examination, by eye, shall be done to make sure that there are no imperfections or defects inside or on the surface of the specimen, for instance bubbles, holes, or scratches.2 ISO 2014 All rights r
33、eservedBS ISO 11359-1:2014ISO 11359-1:2014(E)7 Procedure7.1 Calibration7.1.1 FurnaceCalibrate the furnace (5.1) using two or more metallic calibration materials covering the temperature range to be used for the test specimen. Calibration materials shall either be certified or chosen from those liste
34、d in Table 1, provided their purity is 99,99 % or better. The thickness of the specimens prepared from calibration materials shall be approximately 0,1 mm. Carry out the determinations of the melting point of the calibration materials under the same experimental conditions as those which will be use
35、d for the test specimen.Measure, under the same load as will be used for the test specimen, the point at which penetration of the calibration material by the probe (5.3) occurs due to melting (see Figure 1). Determine the penetration temperature of the calibration material in accordance with ISO 113
36、59-3.Table 1 Metallic calibration materialsMetalMelting point5 6 7CGallium 29,76Indium 156,60Tin 231,93Lead 327,46Zinc 419,53Keyl displacementT temperatureTmmelting pointFigure 1 Determination of the melting point ISO 2014 All rights reserved 3BS ISO 11359-1:2014ISO 11359-1:2014(E)7.1.2 Displacement
37、 transducerCalibrate the displacement transducer (5.2) using a certified micrometer (5.7) or set of certified thickness gauges.7.1.3 Load-application deviceCalibrate the load-application device (5.4) by means of certified calibration masses or using a certified force gauge.7.2 Blank runCarry out a b
38、lank run, recording the TMA curve under the same conditions as those to be used for the test specimen, but without the test specimen.The data obtained for the test specimen shall be corrected using the data obtained from the blank run.7.3 DeterminationMeasure the length l0of the test specimen at one
39、 of the standard temperatures specified in ISO 291 using a micrometer or calliper (see 5.7).Place the test specimen on the sample holder.The details of the test conditions and procedures for TMA determinations are specified in ISO 11359-2 and ISO 11359-3. Select the temperature range, the heating an
40、d/or cooling rate, and the load to be applied as given in those International Standards, or as required in the relevant material standard.Record the displacement as a function of temperature and/or time.After completion of the run, cool down the specimen to room temperature.8 Test reportThe test rep
41、ort shall include the following:a) a reference to this part of ISO 11359;b) all details necessary for complete identification of the material or product tested (lot number, etc.);c) the type of test specimen used, its dimensions, the method of preparation, and its orientation with reference to the s
42、heet or article it was taken from;d) details of the conditioning of the test specimen, if applicable;e) the type of TMA equipment used;f) the shape and dimensions of the probe;g) the materials used for calibration purposes and the values obtained;h) the experimental conditions used for the determina
43、tion;i) the results of the test, including the TMA curves obtained (if necessary);j) the date(s) of testing.4 ISO 2014 All rights reservedBS ISO 11359-1:2014ISO 11359-1:2014(E)Bibliography1 ICTA, Nomenclature for Thermal Analysis, 1992 (see also Annex A)2 Turi E.A. Thermal Characterization of Polyme
44、ric Materials. Academic Press, New York, 19813 Wunderlich B. Thermal Analysis. Academic Press, New York, 19904 ICTA. For Better Thermal Analysis. Third Edition, 19915 Cammenga H.K., Eysel W., Gmelin E., Hemminger W., Hhne G.W.H., Sarge S.M. The temperature calibration of scanning calorimeters: Part
45、2: Calibration substances. Thermochim. Acta. 1993, 219 p. 3336 Sarge S.M., Hemminger W., Gmelin E., Hhne G.W.H., Cammenga H.K., Eysel W. Metrologically based procedures for the temperature, heat and heat flow rate calibration of DSC. J. Therm. Anal. 1997, 49 p. 11257 Preston-Thomas H. The Internatio
46、nal temperature scale of 1990 (ITS-90). Metrologia. 1990, 27 pp. 310 ISO 2014 All rights reserved 5BS ISO 11359-1:2014ISO 11359-1:2014(E) ISO 2014 All rights reservedICS 83.080.01Price based on 5 pagesThis page deliberately left blankBSI is the national body responsible for preparing British Standar
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