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1、| | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | BRITISH STANDARD BS ISO 11359-1:1999 ICS 8
2、3.080.01 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAW Plastics Thermomechanical analysis (TMA) Part 1: General principles Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:23 GMT+00:00 2006, Uncontrolled Copy, (c) BSI This British Standard, having been prepared u
3、nder the direction of the Sector Committee for Materials and Chemicals, was published under the authority of the Standards Committee and comes into effect on 15 November 1999 BSI 11-1999 ISBN 0 580 35347 8 BS ISO 11359-1:1999 Amendments issued since publication Amd. No.DateComments National foreword
4、 This British Standard reproduces verbatim ISO 11359-1:1999 and implements it as the UK national standard. The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics, which has the responsibility to: aid enquirers to understand the text; present to the r
5、esponsible international/European committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. A list of organizations represented on this committee can be obtained o
6、n request to its secretary. Cross-references The British Standards which implement international or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled International Standards Correspondence Index, or by using the Find facility of
7、 the BSI Standards Electronic Catalogue. A British Standard does not purport to include all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations.
8、Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, pages ii to iii, a blank page, pages 1 to 7 and a back cover. The BSI copyright notice displayed in this document indicates when the document was last issued. Licensed Copy: sheffieldun sheffieldun, na
9、, Mon Nov 27 08:11:23 GMT+00:00 2006, Uncontrolled Copy, (c) BSI A Reference number ISO 11359-1:1999(E) INTERNATIONAL STANDARD ISO 11359-1 First edition 1999-10-01 Plastics Thermomechanical analysis (TMA) Part 1: General principles Plastiques Analyse thermomcanique (TMA) Partie 1: Principes gnraux L
10、icensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:23 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11359-1:1999(E) ii Contents 1 Scope1 2 Normative references1 3 Terms and definitions .1 4 Principle2 5 Materials .2 6 Apparatus.2 7 Test specimens3 8 Procedure.3 9 Test report4 Annex A (info
11、rmative) ICTA, NIST6 Bibliography7 Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:23 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11359-1:1999(E) iii Foreword ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member b
12、odies). The work of preparing International 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 a
13、nd 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. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives
14、, Part 3. 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 11359-1 was prepared by Technical Co
15、mmittee ISO/TC 61, Plastics, Subcommittee 5, Physical-chemical properties. ISO 11359 consists of the following parts, under the general title Plastics Thermomechanical analysis: Part 1: General principles Part 2: Determination of coefficient of linear thermal expansion and glass transition temperatu
16、re Part 3: Determination of penetration temperature Annex A of this part of ISO 11359 is given for information only. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:23 GMT+00:00 2006, Uncontrolled Copy, (c) BSI Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:23 GMT+00:00 20
17、06, Uncontrolled Copy, (c) BSI INTERNATIONAL STANDARD ISO 11359-1:1999(E) 1 Plastics Thermomechanical analysis (TMA) Part 1: General principles 1 Scope This part of ISO 11359 specifies the general conditions for the thermomechanical analysis of thermoplastics and thermosetting materials, filled or u
18、nfilled, in the form of sheet or moulded parts. Thermomechanical analysis consists of the determination of deformations of a test specimen as a function of temperature and/or time. 2 Normative references The following normative documents contain provisions which, through reference in this text, cons
19、titute provisions of this part of ISO 11359. For dated references, subsequent amendments to, or revisions of, any of these publications do not apply. However, parties to agreements based on this part of ISO 11359 are encouraged to investigate the possibility of applying the most recent editions of t
20、he normative documents indicated below. For undated references, the latest edition of the normative document referred to applies. Members of ISO and IEC maintain registers of currently valid International Standards. ISO 291, Plastics Standard atmospheres for conditioning and testing. ISO 11359-2, Pl
21、astics Thermomechanical analysis (TMA) Part 2: Determination of coefficient of linear thermal expansion and glass transition temperature. ISO 11359-3, Plastics Thermomechanical analysis (TMA) Part 3: Determination of penetration temperature. 3 Terms and definitions For the purposes of this part of I
22、SO 11359, the following terms and definitions apply. 3.1 thermomechanical analysis TMA technique in which the deformation of a test specimen under a non-oscillatory load is recorded as a function of temperature and/or time while the specimen is subjected to a controlled temperature programme 3.2 the
23、rmodilatometry technique in which a dimension (or the volume) of a substance under negligible stress is measured as a function of temperature while the substance is subjected to a controlled temperature programme Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:23 GMT+00:00 2006, Uncontr
24、olled Copy, (c) BSI ISO 11359-1:1999(E) 2 NOTE A distinction is made between linear thermodilatometry (in which a dimension is measured) and volume thermodilatometry (in which the volume is measured). 3.3 TMA curve curve obtained with a TMA apparatus, the curve being a recording of any measured dime
25、nsion of the sample as a function of temperature or time 4 Principle The deformation of a material under non-oscillatory stress is measured as a function of time at a constant temperature or as a function of temperature. 5 Materials 5.1 Pure metallic reference materials, with known melting points, f
26、or temperature calibration purposes. Table 1 Metallic reference materials (purity . 99,99 %) Metal Melting pointa C Indium 156,6 Tin 231,9 Lead 327,5 Zinc 419,6 a Values from NIST reference material catalogue (see annex A). 6 Apparatus The TMA apparatus shall have the following components: 6.1 Tempe
27、rature-programmable furnace, with a test chamber capable of: running tests at constant heating or cooling rates from 1 K/min to 20 K/min or at constant temperature in the recommended range, 123 K (-150 C) to 773 K (500 C); maintaining the temperature of the test within an accuracy of 2 K; regulating
28、 the temperature with a resolution of at least 0,5 K; being swept by a gas flow. 6.2 Displacement transducer, with a detection limit of at least 10-1 mm. 6.3 Measurement probe: a rod made of a material with a low thermal-expansion coefficient (for instance, silica), linked mechanically to the transd
29、ucer, 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 the probe mass, either through calibration or taring. 6.4 Load-application device (compression, penetration, tension or flexure). The magn
30、itude of the load applied to the rod depends on the type of measurement required. It is necessary to determine the force actually applied to the specimen. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:23 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11359-1:1999(E) 3 6.5 Cooling devi
31、ce, using liquid nitrogen, circulating refrigerant, ice or circulating water, and capable of producing a stable and reproducible temperature. 6.6 Inert or oxidizing gas supply device (flow rate about 10 ml/min to 100 ml/min). 6.7 Signal acquisition and/or recording equipment. 6.8 Micrometers or cali
32、pers. 7 Test specimens Cut test specimens from a sheet or moulded article in such a way that any heating will not modify its structure. The test specimen may be of any shape but shall have a thickness of a few millimetres. Refer to the manufacturers instructions regarding specimen size. Ensure that
33、the lower and upper surfaces of the specimen are parallel and smooth, smoothing down if necessary with abrasive paper (e.g. No. 200 grade). If specimens are taken from a moulded article, report the procedure used, i.e. method, type of article and orientation of specimen. Condition the specimen under
34、 one of the sets of conditions specified in ISO 291, if necessary. A visual (naked eye) examination is recommended to make sure that there are no imperfections or defects inside or on the surface, for instance bubbles, holes or scratches. 8 Procedure 8.1 Calibration 8.1.1 Furnace Calibrate the furna
35、ce (6.1) using two or more pure metallic reference materials (5.1) with known melting points (see Table 1) covering the temperature range to be used for the test specimen. The thickness of the metallic pieces made from the reference materials shall be approximately 0,1 mm. Carry out the determinatio
36、ns of the melting point of the reference materials under the same experimental conditions as those which will be used for the test specimen. Measure, under the same load as will be used for the test specimen, the point at which penetration of the reference material by the probe (6.3) occurs due to m
37、elting (see Figure 1). Determine the penetration temperature of the reference material in accordance with ISO 11359-3. 8.1.2 Transducer Calibrate the transducer (6.2) using a micrometer (6.8) or set of standard gauges of precisely known thickness. The precision of the micrometer or gauges shall be t
38、he same as that required for the precision of the displacement transducer. 8.1.3 Load-application device Calibrate the load-application device (6.4) by means of the standard masses provided with each apparatus or using a certified force gauge. For details, refer to the manufacturers instructions. Li
39、censed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:23 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11359-1:1999(E) 4 Figure 1 Determination of the melting point 8.2 Blank run Carry out a blank run, recording the TMA curve under the same conditions as those to be used for the test specimen,
40、 but without the test specimen. The data obtained for the test specimen can then be corrected using the data obtained from the blank run. 8.3 Determination Place the test specimen on the sample holder. Place the temperature sensor as close as possible to the test specimen. Measure the length L0 of t
41、he test specimen at 23 C using the displacement transducer. Select the temperature range, the heating and/or cooling rate and the load to be applied, as given in ISO 11359-2 or ISO 11359-3 or as required in the relevant material standard. Record the TMA curve as a function of temperature or time. On
42、 completion of the run, allow the specimen to cool. The details of the test conditions and procedures for each TMA test are specified in ISO 11359-2 and ISO 11359-3. Compare the blank-run curve with that obtained for the test specimen and make any corrections necessary. 9 Test report The test report
43、 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 sh
44、eet or article it was taken from; Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:23 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11359-1:1999(E) 5 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
45、 probe; g) the materials used for calibration purposes and the values obtained; h) the experimental conditions used for the determination; i) the results of the test, including the TMA curves obtained (if necessary); j) the date(s) of testing. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 0
46、8:11:23 GMT+00:00 2006, Uncontrolled Copy, (c) BSI ISO 11359-1:1999(E) 6 Annex A (informative) ICTA, NIST ICTA is the abreviation for the International Confederation for Thermal Analysis. To obtain the ICTA booklet, contact the thermal analysis society of your country or: Prof. Edward L. Charsley IC
47、TA President Thermal Analysis Consultancy Service Leeds Metropolitan University Calverley Street Leeds LS1 3HE UK NIST is the abbreviation for National Institute of Standards and Technology. NIST, Gaithersburg, MD 20899-0001, USA Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:23 GMT+00
48、:00 2006, Uncontrolled Copy, (c) BSI ISO 11359-1:1999(E) 7 Bibliography 1ISO 472:1999, Plastics Vocabulary. 2ICTA, Nomenclature for Thermal Analysis, 1992 (see also annex A). 3TURI E.A., Thermal Characterization of Polymeric Materials, Academic Press, New York, 1981. 4WUNDERLICH B., Thermal Analysis
49、, Academic Press, New York, 1990. 5ICTA, For Better Thermal Analysis, 3rd edn., 1991. Licensed Copy: sheffieldun sheffieldun, na, Mon Nov 27 08:11:23 GMT+00:00 2006, Uncontrolled Copy, (c) BSI BS ISO 11359-1:1999 BSI 389 Chiswick High Road London W4 4AL | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | | B
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