BS PD CEN ISO TR 22007-5-2014 Plastics Determination of thermal conductivity and thermal diffusivity Results of interlaboratory testing of poly(methyl methacrylate) sample.pdf

1、BSI Standards Publication PD CEN ISO/TR 22007-5:2014 Plastics Determination of thermal conductivity and thermal diffusivity Part 5: Results of interlaboratory testing of poly(methyl methacrylate) samples (ISO/TR 22007-5:2011)PD CEN ISO/TR 22007-5:2014 PUBLISHED DOCUMENT National foreword This Publis

2、hed Document is the UK implementation of CEN ISO/TR 22007-5:2014. It is identical to ISO/TR 22007-5:2011. The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics. A list of organizations represented on this committee can be obtained on request to its

3、secretary. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2014. Published by BSI Standards Limited 2014 ISBN 978 0 580 85157 5 ICS 83.080.01 Compliance with a British Standa

4、rd cannot confer immunity from legal obligations. This Published Document was published under the authority of the Standards Policy and Strategy Committee on 31 July 2014. Amendments issued since publication Date Text affected TECHNICAL REPORT RAPPORT TECHNIQUE TECHNISCHER BERICHT CEN ISO/TR 22007-5

5、 July 2014 ICS 83.080.01 English Version Plastics - Determination of thermal conductivity and thermal diffusivity - Part 5: Results of interlaboratory testing of poly(methyl methacrylate) samples (ISO/TR 22007-5:2011) Plastiques - Dtermination de la conductivit thermique et de la diffusivit thermiqu

6、e - Partie 5 : Rsultats dessais interlaboratoires du poly(mthacrylate de mthyle) (ISO/TR 22007-5:2011) Kunststoffe - Bestimmung der Wrmeleitfhigkeit und der Temperaturleitfhigkeit - Teil 5: Ergebnisse des Ringversuchs an Polymethylmethacrylatproben (ISO/TR 22007-5:2011) This Technical Report was app

7、roved by CEN on 28 June 2014. It has been drawn up by the Technical Committee CEN/TC 249. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary,

8、Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG CEN-CENELEC M

9、anagement Centre: Avenue Marnix 17, B-1000 Brussels 2014 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. CEN ISO/TR 22007-5:2014 EPD CEN ISO/TR 22007-5:2014 CEN ISO/TR 22007-5:2014 (E) 3 Foreword The text of ISO/TR 22007-5:2011 has be

10、en prepared by Technical Committee ISO/TC 61 “Plastics” of the International Organization for Standardization (ISO) and has been taken over as CEN ISO/TR 22007-5:2014 by Technical Committee CEN/TC 249 “Plastics” the secretariat of which is held by NBN. Attention is drawn to the possibility that some

11、 of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. Endorsement notice The text of ISO/TR 22007-5:2011 has been approved by CEN as CEN ISO/TR 22007-5:2014 without any modification. PD C

12、EN ISO/TR 22007-5:2014 ISO/TR 22007-5:2011(E) ISO 2011 All rights reserved iiiContents Page Foreword iv Introduction.v 1 Scope1 2 Symbols and definitions.1 3 Specimen preparation and characterization 1 4 Measurement apparatus .2 5 Measurement procedure.3 6 Calculations .3 7 Results and conclusions 3

13、 8 Results3 9 Uncertainty and repeatability .4 10 Acknowledgment.4 Annex A (informative) Instructions sent to interlaboratory comparison participants: Procedure for thermal conductivity and diffusivity intercomparison in support of the development of ISO 22007 parts 1-4 .9 Annex B (informative) Labo

14、ratory 1 results 12 Annex C (informative) Laboratory 2 results 18 Annex D (informative) Laboratory 3 results 22 Annex E (informative) Laboratory 4 results.29 Annex F (informative) Laboratory 5 results.31 Bibliography34 PD CEN ISO/TR 22007-5:2014 ISO/TR 22007-5:2011(E) iv ISO 2011 All rights reserved

15、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. Each member body interested in a subject for which a t

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

17、 of electrotechnical standardization. International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2. The main task of technical committees is to prepare International Standards. Draft International Standards adopted by the technical committees are circulate

18、d to the member bodies for voting. Publication as an International Standard requires approval by at least 75 % of the member bodies casting a vote. In exceptional circumstances, when a technical committee has collected data of a different kind from that which is normally published as an internationa

19、l Standard (“state of the art”, for example), it may decide by a simple majority vote of its participating members to publish a Technical Report. A Technical Report is entirely informative in nature and does not have to be reviewed until the data it provides are considered to be no longer valid or u

20、seful. Attention is drawn to the possibility that some of the elements of this document may be the subject of patent rights. ISO shall not be held responsible for identifying any or such patent rights. ISO/TR 22007-5 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physica

21、l- chemical properties. ISO 22007 consists of the following parts under the general title Plastics Determination of thermal conductivity and thermal diffusivity: Part 1: General principles Part 2: Transient plane heat source (hot disc) method Part 3: Temperature wave analysis method Part 4: Laser fl

22、ash method Part 5: Results of interlaboratory testing of poly(methyl methacrylate) samples Technical Report PD CEN ISO/TR 22007-5:2014 ISO/TR 22007-5:2011(E) ISO 2011 All rights reserved vIntroduction The purpose of this document is to record the results of the interlaboratory comparison of measurem

23、ents of the thermal conductivity and thermal diffusivity of poly(methyl methacrylate) PMMA specimens, as a source of information in support of the development of the series of standards on thermal conductivity and diffusivity of plastics, ISO 220071 - 4 . PD CEN ISO/TR 22007-5:2014PD CEN ISO/TR 2200

24、7-5:2014 TECHNICAL REPORT ISO/TR 22007-5:2011(E) ISO 2011 All rights reserved 1Plastics Determination of thermal conductivity and thermal diffusivity Part 5: Results of interlaboratory testing of poly(methyl methacrylate) samples IMPORTANT The electronic file of this document contains colours which

25、are considered to be useful for the correct understanding of the document. Users should therefore consider printing this document using a colour printer. 1 Scope This Technical Report presents the results of interlaboratory testing for the determination of thermal conductivity and thermal diffusivit

26、y of two poly(methyl methacrylate) (PMMA) materials by means of the transient and the modulated methods presented in ISO 22007 parts 2 to 41 - 4and additional transient and steady state methods. The instructions for the intercomparison are presented in Annex A with key items reproduced in the main p

27、art of this Technical Report. The detailed results of individual laboratories are presented in Annexes B to F. 2 Symbols and definitions Symbol Meaning Unit Thermal diffusivity m 2 /s d Thickness of specimen m Thermal conductivity W/(mK) For definitions of the terms used, the reader is referred to I

28、SO 4725and ISO 22007-11 . 3 Specimen preparation and characterization 3.1 Specimens Two types of PMMA material were used in the intercomparison: Sumipex 000 (cast grade), Lot. 6621114, supplied by Sumitomo Chemical Co. Ltd, Japan6 . Referred to as “Sumipex cast PMMA“ herein. Sheet thickness 2 mm. AA

29、JHF (extruded grade), supplied via NPL, UK. Referred to as “extrusion grade PMMA“ herein. Sheet thickness 3 mm. PD CEN ISO/TR 22007-5:2014 ISO/TR 22007-5:2011(E) 2 ISO 2011 All rights reservedThe Sumipex cast PMMA was supplied in sheet form only whereas the extrusion grade PMMA was supplied in both

30、sheet and pellet forms. 3.2 Specimen preparation Depending on the test method, test specimens needed to be prepared from the sheet samples. For the temperature wave analysis the specimens were reduced in thickness. For laser flash testing they were reduced in thickness by one laboratory, but not by

31、the second laboratory. For transient line source testing the specimens were prepared by cutting small pieces from the sheet for insertion into the barrel of the instrument. For Hot Disk testing, most of the data reported are for measurements on single sheets, although two sheets were stacked in some

32、 cases to form the test specimen (see Table 1). 4 Measurement apparatus The experimental apparatus is described in ISO 22007 Parts 1 - 4 and in further detail in references 7 17. Table 1 - The measured thermal properties and various specimen sizes for the methods used in this study. Method / Lab No.

33、 Measured parameter (thermal conductivity and/or thermal diffusivity) Nominal specimen thickness mm Specimen size mm ( : diameter) Additional pre-treatments Hot Disk / 1 , , ( C p ) 12, 3 (4, 6: stacked) 5, 10 Laser flash / 2 2 10 silver paint (30 m) Laser flash / 3 1,14 cast, 1,49 extruded 12,7 spu

34、ttered graphite Transient line- source probe / 3 moulded in-situ 50 moulded in-situ Heat flow meter / 3 2, 3 50 Heat flow meter / 4 2, 3 80 Temperature wave analysis / 5 0,01 3 x 5 1 The factor C p , the specific heat per unit volume J/(m 3 .K), is determined from the ratio of the measured thermal c

35、onductivity and thermal diffusivity values where is the density (kg/m 3 ) and C pis the specific heat capacity per unit mass (J/kg.K).PD CEN ISO/TR 22007-5:2014 ISO/TR 22007-5:2011(E) ISO 2011 All rights reserved 35 Measurement procedure The procedures used were as specified in the relevant parts of

36、 ISO 220072 - 4for the methods covered by that standard. The other methods are specified by ASTM D59307for the line source probe technique, by ASTM E15308for the guarded heat flow meter method, and as described by 9 for the second heat flux meter method. Experimental details and variations from thes

37、e references are reported in the intercomparison instructions, Annex A, and in the individual laboratory test reports, Annexes B to F. 6 Calculations All laboratories carried out the necessary analyses of their raw data to determine thermal conductivity, thermal diffusivity and heat capacity values.

38、 7 Results and conclusions The test reports of the individual laboratories are presented in Annexes B to F along with tabulated data as provided or abbreviated as appropriate. 8 Results The results of the measurements are presented in Figures 1 - 4. In addition, in each of these figures, values of t

39、hermal diffusivity have been calculated from thermal conductivity, or vice-versa, to demonstrate the level of agreement between the two types of measurement. The individual results were typically within a range of approximately 10 % of the mean value at any given temperature for both thermal conduct

40、ivity and thermal diffusivity18 . The reasons for the discrepancy in results are not entirely clear from the intercomparison and require further examination to reduce further the variation in results. Three particular issues highlighted by the intercomparison that should be covered by good measureme

41、nt practice are: Need to ensure that the specimens are of the appropriate thickness for the test method, satisfying any criteria on thickness that the method imposes. This may necessitate machining of the specimen to an appropriate thickness. Effect of anisotropy of the sample. When using the Hot Di

42、sk method, testing can yield either anisotropic properties or bulk properties depending on the specific method used. As properties of polymers can be anisotropic, normally due to processing induced effects, it may be necessary to take this into account in testing, depending on the application for th

43、e data. When calculating thermal diffusivity from thermal conductivity, and vice-versa, it is important to assess the uncertainties in the specific heat capacity values used as these can contribute significantly to the overall uncertainty in calculated values. In the testing carried out here the spe

44、cific heat capacity values varied by up to approximately 10 % from the mean, and density values by 1 % from the mean. This would contribute an uncertainty of approximately 10 % to the calculation of thermal diffusivity (see Table 2). PD CEN ISO/TR 22007-5:2014 ISO/TR 22007-5:2011(E) 4 ISO 2011 All r

45、ights reserved9 Uncertainty and repeatability Estimates of the uncertainties or repeatabilities of the experimentally measured and calculated values are presented in Table 2. The uncertainty of measurement (coverage factor k = 2) was calculated according to the Guide to the expression of uncertainty

46、 in measurement19 . The expanded uncertainty was calculated when thermal diffusivity was calculated from thermal conductivity, or vice-versa, by the use of the equation = C p according to the Guide to the expression of uncertainty in measurement. In Table 2 the uncertainties are shown with the k-num

47、bers in parenthesis; values without k-numbers are the repeatabilities. Table 2 - Estimates of the uncertainties or repeatability for the experimental and calculated values. Sumipex cast PMMA C p Lab. 1 - 0,25 % - 2,89 % * 0,32 % - 3,16 % 0,12 % - 0,52 % (ISO 22007-2) (ISO 22007-2) (ISO 22007-2) Lab.

48、 2 1 % 4 % 8 % (k = 2) 9 % (k = 2) (ISO 1183-1) (ISO 11357-4) (ISO 22007-4) (calc, ISO 22007-4) Lab. 3 per standard - 0,49 % - 2,9 % 3 % ASTM D792 (ASTM E1269-05) (ASTM E1461-01) (ASTM E1530) Lab. 4 0,08 % 1,8 % - 4,8 % - 3 % Lab. 5 - - 2,6 % (k = 2) 8,4 % *(k = 2) (ISO22007-3) (calc, ISO22007-3) Ex

49、trusion grade PMMA C p Lab. 1 - 0,12 % - 1,95 % * 0,16 % - 1,6 % 0,07 % - 0,35 % (ISO 22007-2) (ISO 22007-2) (ISO 22007-2) Lab. 3 per standard - 0,87 % - 5,6 % per standard ASTM D792 (ASTM E1269-05) (ASTM E1461-01) ASTM D5930 Lab. 4 0,22 % 3,2 % - 4,3 % - 3 % Lab. 5 - - 5,0 % (k = 2) 9,5 % *(k = 2) (ISO 22007-3) (calc, ISO 22007-3) *apparent value as C p*calculated with Lab. 2 C pand density data *calculated with L