BS EN ISO 3146-2000 Plastics - Determination of melting behaviour (melting temperature or melting range) of semi-crystalline polymers by capillary tube and polarizing-microscope me.pdf

1、BRITISH STANDARD BS EN ISO 3146:2000 Incorporating Corrigenda Nos. 1 and 2 Plastics Determination of melting behaviour (melting temperature or melting range) of semi-crystalline polymers by capillary tube and polarizing-microscope methods The European Standard EN ISO 3146:2000 has the status of a Br

2、itish Standard ICS 83.080.01 BS EN ISO 3146:2000 This British Standard, having been prepared under 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 September 2000 BSI 21 March 2003 ISBN 0 580 3

3、4852 0 National foreword This British Standard is the official English language version of EN ISO 3146:2000, including Corrigendum December 2002. It is identical with ISO 3146:2000, including Technical Corrigendum October 2002. It supersedes BS EN ISO 3146:1997 which is withdrawn. The UK participati

4、on in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement international or European

5、 publications referred to in this document may be found in the BSI Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all t

6、he necessary provisions of a contract. Users are responsible for its correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European committee any enquiries on t

7、he interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the EN ISO title page, the EN ISO foreword page, the I

8、SO title page, pages ii to v, a blank page, pages 1 to 7, the Annex ZA page, an inside back cover and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date Comments 13828 Corrigendum No. 1 3 Apri

9、l 2002 Revised EN ISO foreword and Annex ZA pages 14301 Corrigendum No. 2 21 March 2003 Change to Table 1EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 3146 June 2000 ICS 83.080.10 Supersedes EN ISO 3146:1997 English version Plastics - Determination of melting behaviour (melting temperatur

10、e or melting range) of semi-crystalline polymers by capillary tube and polarizing-microscope methods (ISO 3146:2000) Plastiques - Dtermination du comportement la fusion (temprature de fusion ou plage de tempratures de fusion) des polymres semi-cristallins par mthodes du tube capillaire et du microsc

11、ope polarisant (ISO 3146:2000) Kunststoffe - Bestimmung des Schmelzverhaltens (Schmelztemperatur oder Schmelzbereich) von teilkristallinen Polymeren im Kapillarrohr- und Polarisationsmikroskop- Verfahren (ISO 3146:2000) This European Standard was approved by CEN on 9 April 2000. CEN members are boun

12、d to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the Ce

13、ntral Secretariat or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the Central Secretariat has the same status a

14、s the official versions. CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZA

15、TION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Central Secretariat: rue de Stassart, 36 B-1050 Brussels 2000 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 3146:2000 E Incorporates corrigendum December 2002

16、CORRECTED 2002-03-13 Foreword This document (ISO 3146:2000) has been prepared by Technical Committee ISO/TC 61 “Plastics“ in collaboration with Technical Committee CEN/TC 249 “Plastics“, the secretariat of which is held by IBN. This European Standard shall be given the status of a national standard,

17、 either by publication of an identical text or by endorsement, at the latest by December 2000, and conflicting national standards shall be withdrawn at the latest by December 2000. This document supersedes EN ISO 3146:1997. According to the CEN/CENELEC Internal Regulations, the national standards or

18、ganizations of the following countries are bound to implement this European Standard: Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice

19、 The text of the International Standard ISO 3146:2000 has been approved by CEN as a European Standard without any modifications. NOTE Normative references to International Standards are listed in annex ZA (normative). EN ISO 3146:2000INTERNATIONAL STANDARD ISO 3146 Third edition 2000-06-01 Reference

20、 number ISO 3146:2000(E) Plastics Determination of melting behaviour (melting temperature or melting range) of semi-crystalline polymers by capillary tube and polarizing-microscope methods Plastiques Dtermination du comportement la fusion (temprature de fusion ou plage de tempratures de fusion) des

21、polymres semi-cristallins par mthodes du tube capillaire et du microscope polarisant EN ISO 3146:2000ii EN ISO 3146:2000iii Contents Page 1 Scope . 1 2 Normative reference . 1 3 Terms and definitions 1 4 Method A Capillary tube 2 5 Method B Polarizing microscope 5 EN ISO 3146:2000iv Foreword ISO (th

22、e 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 com- mittees. Each member body interested in a subject for which a technical commi

23、ttee has been established has the right to be represented on that committee. International organizations, governmental and non-governmental, in liai- son with ISO, also take part in the work. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrot

24、echnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 3. Draft International Standards adopted by the technical committees are circulated to the member bodies for voting. Publication as an International Standard requires appr

25、oval by at least 75 % of the member bodies casting a vote. Attention is drawn to the possibility that some of the elements of this International Standard may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. International Standard ISO 3

26、146 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-chemical properties. This third edition cancels and replaces the second edition (ISO 3146:1985), which has been technically revised. EN ISO 3146:2000v Introduction The melting behaviour of a crystalline or semi-

27、crystalline polymer is a structure-sensitive property. In polymers, a sharp melting point, such as is observed for low molecular mass substances, usually does not occur; instead a melting temperature range is observed on heating, from the first change of shape of the solid particles to the transform

28、ation into a highly viscous or viscoelastic liquid, with accompanying disappearance of the crystalline phase. The melting range depends upon a number of parameters, such as molecular mass, molecular mass distribu- tion, per cent crystallinity, and thermodynamic properties. It may also depend on the

29、previous thermal history of the specimens. The lower or upper limit of the melting range, or its average value, is sometimes conventionally referred to as the “melting temperature”. EN ISO 3146:2000EN ISO 3146:20001 Plastics Determination of melting behaviour (melting temperature or melting range) o

30、f semi-crystalline polymers by capillary tube and polarizing-microscope methods 1 Scope This International Standard specifies two methods for evaluating the melting behaviour of semi-crystalline polymers. Melting temperatures determined by the different methods usually differ by several kelvins for

31、the reasons explained in the introduction. Method A: Capillary tube This method is based on the changes in shape of the polymer. It is applicable to all semi-crystalline polymers and their compounds. NOTE 1 Method A may also be useful for the evaluation of the softening of non-crystalline solids. Me

32、thod B: Polarizing microscope This method is based on changes in the optical properties of the polymer. It is applicable to polymers containing a birefringent crystalline phase. It may not be suitable for plastics compounds containing pigments and/or other addi- tives which could interfere with the

33、birefringence of the polymeric crystalline zone. NOTE 2 Another method applicable to semi-crystalline polymers is described in ISO 11357-3:1999, Plastics Differential scan- ning calorimetry (DSC) Part 3: Determination of temperature and enthalpy of melting and crystallization. 2 Normative reference

34、The following normative document contains provisions which, through reference in this text, constitute provisions of this International Standard. For dated references, subsequent amendments to, or revisions of, any of these publica- tions do not apply. However, parties to agreements based on this In

35、ternational Standard are encouraged to investi- gate the possibility of applying the most recent edition of the normative document 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 I

36、nternational Standards. ISO 291, Plastics Standard atmospheres for conditioning and testing. 3 Terms and definitions For the purposes of this International Standard, the following terms and definitions apply. 3.1 semi-crystalline polymer polymer containing both crystalline and amorphous phases which

37、 may be present in varying proportions EN ISO 3146:20002 3.2 melting range the temperature range over which crystalline or semi-crystalline polymers lose their crystalline characteristics or par- ticulate shape when heated NOTE The “melting temperatures” determined by methods A and B are defined in

38、4.1 and 5.1. 4 Method A Capillary tube 4.1 Principle A test sample is heated at a controlled rate, and the temperature of the sample measured at the first visible change in shape and again at the disappearance of the last remnants of the crystalline phase. The first temperature is taken as the melti

39、ng temperature of the sample, while the range between the two tempera- tures describes its melting range. NOTE This method may be used for non-crystalline materials where required by the relevant specifications or by agreement be- tween the interested parties. 4.2 Apparatus (see Figure 1) 4.2.1 Melt

40、ing apparatus, consisting of the following items: a) Cylindrical metal block, the upper part of which is hollow and forms a chamber. b) Metal plug, with two or more holes, allowing a thermometer and one or more capillary tubes to be mounted in the metal block. c) Heating system for the metal block,

41、for example an electrical resistance enclosed in the block. d) Rheostat for regulation of the power input, if electrical heating is used. e) Four windows of heat-resistant glass on the lateral walls of the chamber, diametrically disposed at right angles to each other. In front of one of these window

42、s an eyepiece is mounted for observing the capillary tube. The other three windows are used for illuminating the inside of the enclosure by means of lamps. NOTE Other suitable types of melting apparatus may be used, provided that they give the same results. 4.2.2 Capillary tube,ofh ea t-re si sta nt

43、g la ss ,cl os eda to n ee n d. NOTE The maximum external diameter should preferably be . 4.2.3 Calibrated thermometer, graduated in divisions of . The thermometer bulb shall be positioned in such a way that heat dispersion in the apparatus is not impeded. NOTE Other suitable temperature-measuring d

44、evices may be used. 4.3 Test samples 4.3.1 General The test samples used shall be representative of the material to be tested. 1,5 mm 0,1 C EN ISO 3146:20003 4.3.2 Characteristics Powder of particle size up to or cut pieces of film of thickness to should preferably be used. Comparison tests shall be

45、 carried out on test samples of the same or similar particle size, or of similar thickness in theca seofl a y er so rfil ms . 4.3.3 Conditioning If not otherwise specified or agreed between the interested parties, the test sample shall be conditioned at and a relative humidity of for in accordance w

46、ith ISO 291 prior to the measurement. 4.4 Procedure 4.4.1 Calibration Periodically calibrate the thermometer with reagent grade or certified chemicals over the temperature range used for the test. Chemicals recommended for calibration purposes are listed in Table 1. Key 1 Metal heating block 2L a m

47、p 3 Metal plug 4 Thermometer 5 Capillary 6E y e p i e c e 7 Electrical resistance Figure 1 Apparatus for method A 100m1 0 m2 0 m 23 C 2 C (50 5)%3 h EN ISO 3146:20004 4.4.2 Determination 4.4.2.1 Insert the thermometer (4.2.3) and the capillary tube (4.2.2) containing the test sample into the metal b

48、lock 4.2.1 a) and begin heating. Adjust the controller 4.2.1 d) to heat the specimen gradually (at a rate not higher than ) to a temperature that is about lower than the expected melting temperature. When the temperature of the test sample is about below the expected melting temperature, adjust the

49、rate of temperature increase to . Record the temperature at which the test sample begins to change shape. Continue heating at the same rate. Record the temperature at which the last remnants of the crystalline phase disap- pear. 4.4.2.2 Repeat the operations specified in 4.4.2.1 with a second test sample. If the two results obtained by the same operator on the same sample differ by more than , repeat the procedure on two new test samples. 4.5 Test report The