1、BSI Standards PublicationPD CEN ISO/TR 22007-5:2014Plastics Determinationof thermal conductivity andthermal diffusivityPart 5: Results of interlaboratory testing ofpoly(methyl methacrylate) samples (ISO/TR22007-5:2011)PD CEN ISO/TR 22007-5:2014 PUBLISHED DOCUMENTNational forewordThis Published Docum
2、ent is the UK implementation of CEN ISO/TR22007-5:2014. It is identical to ISO/TR 22007-5:2011.The UK participation 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
3、 publication does not purport to include all the necessaryprovisions of a contract. Users are responsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 85157 5ICS 83.080.01Compliance with a British Standard cannot confer immu
4、nity fromlegal obligations.This Published Document was published under the authority of theStandards Policy and Strategy Committee on 31 July 2014.Amendments issued since publicationDate Text affectedTECHNICAL REPORT RAPPORT TECHNIQUE TECHNISCHER BERICHT CEN ISO/TR 22007-5 July 2014 ICS 83.080.01 En
5、glish 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 thermique - Partie 5 : Rsultats des
6、sais 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 approved by CEN on 28 June 201
7、4. 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, Iceland, Ireland, Italy, La
8、tvia, 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 Management Centre: Avenue Ma
9、rnix 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 22007-5:2014CEN ISO/TR 22007-5:2014 (E) 3 Foreword The text of ISO/TR 22007-5:2011 has been prepared by Technical Com
10、mittee 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 of the elements of this doc
11、ument 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 CEN ISO/TR 22007-5:2014ISO/TR
12、 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 8 Results3 9 Uncertainty and
13、 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) Laboratory 1 results 12 Annex C (
14、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 22007-5:2014ISO/TR 22007-5:2011(E) iv ISO 2011 All rights reservedForeword ISO (the Internationa
15、l 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 technical committee has been es
16、tablished 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 of electrotechnical standardi
17、zation. 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 circulated to the member bodies for vot
18、ing. 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 international Standard (“state of the art”
19、, 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 useful. Attention is drawn to t
20、he 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, Physical-chemical properties. ISO 220
21、07 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 flash method Part 5: Results of i
22、nterlaboratory testing of poly(methyl methacrylate) samples Technical Report PD CEN ISO/TR 22007-5:2014ISO/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 measurements of the thermal conductivity
23、 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 22007-5:2014TECHNICAL REPORT ISO/TR 2
24、2007-5:2011(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 are considered to be useful for th
25、e 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 diffusivity of two poly(methyl methacrylate)
26、 (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 part of this Technical Report. The
27、detailed results of individual laboratories are presented in Annexes B to F. 2 Symbols and definitions Symbol Meaning Unit Thermal diffusivity m2/s d Thickness of specimen m Thermal conductivity W/(mK) For definitions of the terms used, the reader is referred to ISO 4725and ISO 22007-11. 3 Specimen
28、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. AAJHF (extruded grade), supplied via NPL
29、, UK. Referred to as “extrusion grade PMMA“ herein. Sheet thickness 3 mm. PD CEN ISO/TR 22007-5:2014ISO/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 sheet and pellet forms. 3.2 Specimen pr
30、eparation 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 the second laboratory. For transient li
31、ne 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 cases to form the test specimen (see T
32、able 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. Measured parameter (thermal conductivi
33、ty and/or thermal diffusivity) Nominal specimen thickness mm Specimen size mm ( : diameter) Additional pre-treatments Hot Disk / 1 , , ( Cp)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 sputtered graphite Transient line-source prob
34、e / 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 Cp, the specific heat per unit volume J/(m3.K), is determined from the ratio of the measured thermal conductivity and thermal diffusivity values wher
35、e is the density (kg/m3) and Cpis the specific heat capacity per unit mass (J/kg.K).PD CEN ISO/TR 22007-5:2014ISO/TR 22007-5:2011(E) ISO 2011 All rights reserved 35 Measurement procedure The procedures used were as specified in the relevant parts of ISO 220072 - 4for the methods covered by that stan
36、dard. 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 these references are reported in the intercomparison in
37、structions, 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. 7 Results and conclusions The test reports of the
38、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 thermal diffusivity have been calculated from therma
39、l 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 conductivity and thermal diffusivity18. The reasons for th
40、e 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 measurement practice are: Need to ensure that the specimens a
41、re 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 Disk method, testing can yield either anisotropic prop
42、erties 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 the data. When calculating thermal diffusivity from th
43、ermal 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 specific heat capacity values varied by up to approxima
44、tely 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 22007-5:2014ISO/TR 22007-5:2011(E) 4 ISO 2011 All rights reserved9 Uncertainty and repeatability Estimat
45、es 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 in measurement19. The expanded uncertainty was calcu
46、lated when thermal diffusivity was calculated from thermal conductivity, or vice-versa, by the use of the equation = Cp according to the Guide to the expression of uncertainty in measurement. In Table 2 the uncertainties are shown with the k-numbers in parenthesis; values without k-numbers are the r
47、epeatabilities. Table 2 - Estimates of the uncertainties or repeatability for the experimental and calculated values. Sumipex cast PMMA Cp Lab. 1 - 0,25 % - 2,89 % *0,32 % - 3,16 % 0,12 % - 0,52 % (ISO 22007-2) (ISO 22007-2) (ISO 22007-2) Lab. 2 1 % 4 % 8 % (k = 2) 9 % (k = 2) (ISO 1183-1) (ISO 1135
48、7-4) (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) Extrusion grade PMMA Cp Lab. 1 - 0,12 % - 1,95 % *0,16 % -
49、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 Cp*calculated with Lab. 2 Cpand density data *calculated with Lab. 2 and Lab. 4 Cpand density data10 Acknowledgment We expres
