1、BSI Standards Publication BS ISO 6721-10:2015 Plastics Determination of dynamic mechanical properties Part 10: Complex shear viscosity using a parallel-plate oscillatory rheometerBS ISO 6721-10:2015 BRITISH STANDARD National foreword This British Standard is the UK implementation of ISO 6721-10:2015
2、. It supersedes BS ISO 6721-10:1999 which is withdrawn. 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 secretary. This publication does not purport to in
3、clude all the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2015. Published by BSI Standards Limited 2015 ISBN 978 0 580 83208 6 ICS 83.080.01 Compliance with a British Standard cannot confer immunity from legal obligations.
4、This British Standard was published under the authority of the Standards Policy and Strategy Committee on 31 October 2015. Amendments/corrigenda issued since publication Date T e x t a f f e c t e dBS ISO 6721-10:2015 ISO 2015 Plastics Determination of dynamic mechanical properties Part 10: Complex
5、shear viscosity using a parallel-plate oscillatory rheometer Plastiques Dtermination des proprits mcaniques dynamiques Partie 10: Viscosit complexe en cisaillement laide dun rhomtre oscillations plateaux parallles INTERNATIONAL STANDARD ISO 6721-10 Third edition 2015-09-15 Reference number ISO 6721-
6、10:2015(E)BS ISO 6721-10:2015ISO 6721-10:2015(E)ii ISO 2015 All rights reserved COPYRIGHT PROTECTED DOCUMENT ISO 2015, Published in Switzerland All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic
7、 or mechanical, including photocopying, or posting on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below or ISOs member body in the country of the requester. ISO copyright office Ch. de Blandonnet 8 CP 401 CH-1214 Vernier,
8、Geneva, Switzerland Tel. +41 22 749 01 11 Fax +41 22 749 09 47 copyrightiso.org www.iso.orgBS ISO 6721-10:2015ISO 6721-10:2015(E)Foreword iv 1 Scope . 1 2 Normative references 1 3 T erms and definitions . 1 4 Principle 2 5 Apparatus . 2 5.1 Measurement apparatus . 2 5.2 Temperature-controlled enclos
9、ure . 3 5.3 Temperature measurement and control . 3 5.4 Plate/specimen assembly 4 5.5 Calibration 4 6 Sampling 4 7 Procedure. 5 7.1 Test temperature . 5 7.2 Zeroing the gap . 5 7.3 Introducing the test specimen . 5 7.4 Conditioning the test specimen 5 7.5 Test mode (controlled stress or controlled s
10、train) 5 7.6 Determination of thermal stability of sample material . 6 7.7 Determination of region of linear-viscoelastic behaviour . 6 7.7.1 In the controlled-strain mode. 6 7.7.2 In the controlled-stress mode 6 7.7.3 Confirmation of linear-viscoelastic behaviour 7 7.8 Frequency sweep 7 7.9 Tempera
11、ture sweep 7 7.10 Air entrapment 7 8 Expression of results 7 8.1 Symbols used 7 8.2 Calculation of complex shear modulus and complex shear viscosity 8 9 Precision 10 10 Test report 11 Annex A (informative) Uncertainty limits 12 Annex B (informative) V erification of r heomet er performanc e .15 Bibl
12、iography .19 ISO 2015 All rights reserved iii Contents PageBS ISO 6721-10:2015ISO 6721-10:2015(E) 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 ca
13、rried 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 and non-governmental, in liaison with ISO, also take part in the work
14、. ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization. The procedures used to develop this document and those intended for its further maintenance are described in the ISO/IEC Directives, Part 1. In particular the diffe
15、rent approval criteria needed for the different types of ISO documents should be noted. This document was drafted in accordance with the editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives). Attention is drawn to the possibility that some of the elements of this document ma
16、y be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of any patent rights identified during the development of the document will be in the Introduction and/or on the ISO list of patent declarations received (see www.iso.org/paten
17、ts). Any trade name used in this document is information given for the convenience of users and does not constitute an endorsement. For an explanation on the meaning of ISO specific terms and expressions related to conformity assessment, as well as information about ISOs adherence to the WTO princip
18、les in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary information. The committee responsible for this document is ISO/TC 61, Plastics, Subcommittee SC 5, Physical- chemical properties. This third edition cancels and replaces the second edition (ISO 6721-10:1999
19、), which has been technically revised to include informative guidance on verification of the instruments performance ( Annex B). ISO 6721 consists of the following parts, under the general title Plastics Determination of dynamic mechanical properties: Part 1: General principles Part 2: Torsion-pendu
20、lum method Part 3: Flexural vibration Resonance-curve method Part 4: Tensile vibration Non-resonance method Part 5: Flexural vibration Non-resonance method Part 6: Shear vibration Non-resonance method Part 7: Torsional vibration Non-resonance method Part 8: Longitudinal and shear vibration Wave-prop
21、agation method Part 9: Tensile vibration Sonic-pulse propagation method Part 10: Complex shear viscosity using a parallel-plate oscillatory rheometer Part 11: Glass transition temperature Part 12: Compressive vibration Non-resonance method Annex A and Annex B of this part of ISO 6721 is for informat
22、ion only.iv ISO 2015 All rights reservedBS ISO 6721-10:2015INTERNATIONAL ST ANDARD ISO 6721-10:2015(E) Plastics Determination of dynamic mechanical properties Part 10: Complex shear viscosity using a parallel-plate oscillatory rheometer 1 Scope This part of ISO 6721 specifies the general principles
23、of a method for determining the dynamic rheological properties of polymer melts at angular frequencies typically in the range of 0,01 rads -1to 100 rads -1by means of an oscillatory rheometer with a parallel-plate geometry. Angular frequencies outside this range can also be used (see Note 1). The me
24、thod is used to determine values of the following dynamic rheological properties: complex shear viscosity *, dynamic shear viscosity , the out-of-phase component of the complex shear viscosity ”, complex shear modulus G*, shear loss modulus G”, and shear storage modulus G. It is suitable for measuri
25、ng complex shear viscosity values typically up to 10 MPas (see Note 2). NOTE 1 The angular-frequency measurement range is limited by the specification of the measuring instrument and also by the response of the specimen. When testing using angular frequencies lower than 0,1 rads 1 , the test time ca
26、n increase significantly as the time taken to obtain a single measurement is proportional to the reciprocal of the angular frequency. Consequently, when testing at low angular frequencies, degradation or polymerization of the specimen is more likely to occur and have an effect on the results. At hig
27、h angular frequencies, the specimen can distort or fracture at the edge, consequently invalidating the test results. NOTE 2 The range of complex shear viscosity values that can be measured is dependent on the specimen dimensions and also the specification of the measuring instrument. For a specimen
28、of given dimensions, the upper limit of the range is limited by the machines torque capacity, angular-displacement resolution, and compliance. However, correction can be made for compliance effects. 2 Normative references The following documents, in whole or in part, are normatively referenced in th
29、is document and are indispensable for its application. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 472, Plastics Vocabulary ISO 5725-1, Accuracy (trueness and precision) of measure
30、ment methods and results Part 1: General principles and definitions ISO 6721-1, Plastics Determination of dynamic mechanical properties Part 1: General principles 3 T erms a nd definiti ons For the purposes of this document, the terms and definitions given in ISO 6721-1, ISO 5725-1, ISO 472, and the
31、 following apply. 3.1 controlled-strain mode testing by applying a sinusoidal angular displacement of constant amplitude ISO 2015 All rights reserved 1BS ISO 6721-10:2015ISO 6721-10:2015(E) 3.2 controlled-stress mode testing by applying a sinusoidal torque of constant amplitude 3.3 complex shear vis
32、cosity * ratio of dynamic stress, given by (t) = 0exp it, and dynamic rate of strain where the shear strain t is given by (t) = 0exp i(t - ), of a viscoelastic material that is subjected to a sinusoidal vibration, where 0and 0are the amplitudes of the stress and strain cycles, is the angular frequen
33、cy, is the phase angle between the stress and strain, and t is time Note 1 to entry: It is expressed in pascal seconds. 3.4 dynamic shear viscosity real part of the complex shear viscosity Note 1 to entry: It is expressed in pascal seconds. 3.5 out-of-phase component of the complex shear viscosity ”
34、 imaginary part of the complex shear viscosity Note 1 to entry: It is expressed in pascal seconds. 4 Principle The specimen is held between two concentric, circular parallel plates (see Figure 1). The thickness of the specimen is small compared with the diameter of the plates. The specimen is subjec
35、ted to either a sinusoidal torque or a sinusoidal angular displacement of constant angular frequency. These are referred to as “controlled-stress” or “controlled-strain” test modes, respectively. When using the controlled-stress mode, the resultant displacement and the phase shift between the torque
36、 and displacement are measured. When using the controlled-strain mode, the resultant torque and the phase shift between the displacement and torque are measured. The complex shear modulus G*, shear storage modulus G, shear loss modulus G”, phase angle , and corresponding shear viscosity terms (see C
37、lause 3) are determined from the measured torque and displacement and the specimen dimensions. In deriving these values, it is assumed that the specimen exhibits a linear-viscoelastic response. The mode of oscillation used is designated as oscillatory mode I (see ISO 6721-1, Clause 4). 5 Apparatus 5
38、.1 Measurement apparatus The measurement apparatus shall consist of two concentric, rigid, circular parallel plates between which the specimen is placed (see Figure 1). One of these plates shall be made to oscillate at a constant angular frequency while the other remains at rest. The requirements on
39、 the apparatus are that it shall permit measurement of the amplitudes of the torque and the angular displacement and the phase difference between them for a specimen subjected to either a sinusoidal torque or a sinusoidal displacement of constant angular frequency.2 ISO 2015 All rights reservedBS IS
40、O 6721-10:2015ISO 6721-10:2015(E) A torque-measuring device shall be connected to one of the plates, thus permitting measurement of the torque required to overcome the viscoelastic resistance of the specimen. An angular-displacement measuring device shall be fitted to the moving plate, thus permitti
41、ng determination of its angular displacement and angular frequency. The apparatus shall be capable of measuring the torque to within 2 % of the minimum torque amplitude used to determine the dynamic properties. The apparatus shall be capable of measuring the angular displacement to within 20 10 6rad
42、. The apparatus shall be capable of measuring the angular frequency to within 2 % of the absolute value. Key 1 test specimen angular frequency d specimen thickness D diameter of plate Figure 1 Parallel-plate rheometer geometry 5.2 Temperature-controlled enclosure Heating may be provided by the use o
43、f forced convection, radio-frequency heating, or other suitable means. An environmental chamber surrounding the plate/specimen assembly can be used to provide specific test environments, for example a nitrogen atmosphere. Check that the chamber is not in contact with the plate/specimen assembly. 5.3
44、 Temperature measurement and control The test temperature shall preferably be measured using a device that is either in contact with or embedded in the fixed plate. The test temperature shall be accurate to within 0,5 C of the set temperature for set temperatures up to 200 C, within 1,0 C for temper
45、atures in the range 200 C to 300 C, and within 1,5 C for temperatures above 300 C. The temperature-measuring device shall have a resolution of 0,1 C and shall be calibrated using a device accurate to within 0,1 C. ISO 2015 All rights reserved 3BS ISO 6721-10:2015ISO 6721-10:2015(E) 5.4 Plate/specime
46、n assembly The plate/specimen assembly comprises two concentric, circular parallel plates with the specimen held between them. The plates shall have a surface finish corresponding to a maximum roughness of Ra = 0,25 m and shall have no visible imperfections. The results may be dependent on the type
47、of material that is used to form the surfaces of the plates. This can be identified by testing using plates with different surface materials. The plate diameter, D, is typically in the range of 20 mm to 50 mm. It shall be measured to within 0,01 mm. The specimen thickness, d, is defined by the plate
48、 separation and shall be determined to within 0,01 mm. It is recommended that the specimen thickness lie in the range of 0,5 mm to 3 mm and that the ratio of the plate diameter to the specimen thickness lie in the range of 10 to 50 in order to minimize errors in the determination of properties. For
49、low-viscosity polymeric liquids, it may be necessary to employ dimensions outside these recommended ranges. The total variation in the plate separation due to non-parallelism of the plates shall be less than 0,01 mm. Variation in the plate separation during testing shall be less than 0,01 mm. The plates shall be sufficiently flat to enable the requirement on the total variation in the plate separation due to non-p
