ISO TR 22007-5-2011 Plastics - Determination of thermal conductivity and thermal diffusivity - Part 5 Results of interlaboratory testing of poly(methyl methacry.pdf

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1、 Reference number ISO/TR 22007-5:2011(E) ISO 2011TECHNICAL REPORT ISO/TR 22007-5 First edition 2011-04-01 Plastics Determination of thermal conductivity and thermal diffusivity Part 5: Results of interlaboratory testing of poly(methyl methacrylate) samples Plastiques Dtermination de la conductivit t

2、hermique et de la diffusivit thermique Partie 5: Rsultats dessais interlaboratoires du poly(mthacrylate de mthyle) ISO/TR 22007-5:2011(E) PDF disclaimer This PDF file may contain embedded typefaces. In accordance with Adobes licensing policy, this file may be printed or viewed but shall not be edite

3、d unless the typefaces which are embedded are licensed to and installed on the computer performing the editing. In downloading this file, parties accept therein the responsibility of not infringing Adobes licensing policy. The ISO Central Secretariat accepts no liability in this area. Adobe is a tra

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5、es. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. COPYRIGHT PROTECTED DOCUMENT ISO 2011 All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any m

6、eans, electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail cop

7、yrightiso.org Web www.iso.org Published in Switzerland ii ISO 2011 All rights reservedISO/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 Measur

8、ement procedure.3 6 Calculations .3 7 Results and conclusions 3 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 d

9、evelopment of ISO 22007 parts 1-4 .9 Annex B (informative) Laboratory 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 ISO/TR 22007-5:201

10、1(E) iv ISO 2011 All rights reservedForeword 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 i

11、nterested 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 with ISO, also take part in the work. ISO collaborates closely with the International Electrotechn

12、ical Commission (IEC) on all matters 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 th

13、e 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. In exceptional circumstances, when a technical committee has collected data of a different kind from that which is n

14、ormally published as an international 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 c

15、onsidered to be no longer valid or useful. 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,

16、Plastics, Subcommittee SC 5, Physical- 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 w

17、ave analysis method Part 4: Laser flash method Part 5: Results of interlaboratory testing of poly(methyl methacrylate) samples Technical Report 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

18、 measurements 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 . TECHNICAL REPORT ISO/TR 22007-5:201

19、1(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 the correct

20、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) (PMMA) ma

21、terials 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 detailed r

22、esults 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 ISO 4725and ISO 22007-11 . 3 Specimen prepara

23、tion 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, UK.

24、Referred to as “extrusion grade PMMA“ herein. Sheet thickness 3 mm. 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 sheet and pellet forms. 3.2 Specimen preparation Depending on the test

25、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 line source testing the specimens

26、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 Table 1). 4 Measurement apparatus

27、 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 conductivity and/or thermal diffusivity) N

28、ominal 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 sputtered graphite Transient line- source probe / 3 moulded in-situ 50 mou

29、lded 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 conductivity and thermal diffusivity values where is the density (kg/m 3

30、 ) and C pis the specific heat capacity per unit mass (J/kg.K).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 ISO 220072 - 4for the methods covered by that standard. The other methods are specified by ASTM D

31、59307for 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 instructions, Annex A, and in the individual labo

32、ratory 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 individual laboratories are presented in Annexe

33、s 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 thermal conductivity, or vice-versa, to demonstrate t

34、he 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 the discrepancy in results are not entirely clea

35、r 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 are of the appropriate thickness for the test m

36、ethod, 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 properties or bulk properties depending on the spe

37、cific 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 thermal conductivity, and vice-versa, it is impo

38、rtant 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 approximately 10 % from the mean, and density values by

39、 1 % from the mean. This would contribute an uncertainty of approximately 10 % to the calculation of thermal diffusivity (see Table 2). ISO/TR 22007-5:2011(E) 4 ISO 2011 All rights reserved9 Uncertainty and repeatability Estimates of the uncertainties or repeatabilities of the experimentally measure

40、d 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 calculated when thermal diffusivity was calculated from thermal conductivity

41、, 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-numbers in parenthesis; values without k-numbers are the repeatabilities. Table 2 - Estimates of the uncertainties or repeatabil

42、ity 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. 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 %

43、- 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 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) La

44、b. 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 Lab. 2 a

45、nd Lab. 4 C pand density data10 Acknowledgment We express our special thanks to Sumitomo Chemical Co. Ltd. for supplying us the cast PMMA. ISO/TR 22007-5:2011(E) ISO 2011 All rights reserved 50.4 0.8 1.2 1.6 0 50 100 150 200 Sumipex cast PMMA Lab. 1 / HD axial Lab. 2 / LF Lab. 3 / LF Lab. 1 / HD sta

46、cked Lab. 5 / TWA / 10 -7 m 2 s -1 T / C 5 2 1 3 1Figure 1 - Thermal diffusivity of Sumipex cast PMMA in the through-thickness direction measured by the different laboratories at various temperatures T: (i) directly measured values:- Lab. 2 by the Laser flash method (LF) (thickness d = 2 mm), Lab. 3

47、 by LF (d = 1,14 mm), and Lab. 5 by the Temperature wave analysis method (TWA) (d = 0,011 mm); (ii) calculated values from thermal conductivity:- Lab. 1 by the Hot disk method (HD) (d = 2 mm for axial measurement, d = 4 mm for isotropic measurement). ISO/TR 22007-5:2011(E) 6 ISO 2011 All rights rese

48、rved0.14 0.16 0.18 0.20 0.22 0.24 0 50 100 150 200 Lab.1 / HD axial Lab.2 / LF Lab.3 / LF Lab.3 / HFM Lab.3 / LS cool Lab.3 / LS heat Lab.4 / HFM Lab.1 / HD stack Lab.5 / TWA / Wm -1 K -1 T / C 1 1 3 2 3 3 3 4 5 cast grade PMMAFigure 2 - Thermal conductivity of Sumipex cast PMMA in the through-thick

49、ness direction measured by the different laboratories at various temperatures T: (i) directly measured values:- Lab. 1 by the Hot disk method (HD) (thickness d = 2 mm for axial measurement, d = 4 mm for isotropic measurement), Lab. 3 by the Heat flow meter method (HFM) (d = 2 mm) and the Line source method (LS) (d = 2 mm), and Lab. 4 by HFM (d = 2 mm); (ii) calculated values from thermal diffusi