1、BSI Standards PublicationBS ISO 6721-10:2015Plastics Determination ofdynamic mechanical propertiesPart 10: Complex shear viscosity using aparallel-plate oscillatory rheometerBS ISO 6721-10:2015 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 6721-10:2015. It su
2、persedes BS ISO 6721-10:1999 which is withdrawn.The UK participation in its preparation was entrusted to Technical Committee PRI/21, Testing of plastics.A list of organizations represented on this committee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 include all
3、the necessary provisions of a contract. Users are responsible for its correct application. The British Standards Institution 2015.Published by BSI Standards Limited 2015ISBN 978 0 580 83208 6 ICS 83.080.01 Compliance with a British Standard cannot confer immunity from legal obligations.This British
4、Standard was published under the authority of the Standards Policy and Strategy Committee on 31 October 2015.Amendments/corrigenda issued since publicationDate T e x t a f f e c t e dBS ISO 6721-10:2015 ISO 2015Plastics Determination of dynamic mechanical properties Part 10: Complex shear viscosity
5、using a parallel-plate oscillatory rheometerPlastiques Dtermination des proprits mcaniques dynamiques Partie 10: Viscosit complexe en cisaillement laide dun rhomtre oscillations plateaux paralllesINTERNATIONAL STANDARDISO6721-10Third edition2015-09-15Reference numberISO 6721-10:2015(E)BS ISO 6721-10
6、:2015ISO 6721-10:2015(E)ii ISO 2015 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2015, Published in SwitzerlandAll rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including
7、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 officeCh. de Blandonnet 8 CP 401CH-1214 Vernier, Geneva, SwitzerlandTel. +41 2
8、2 749 01 11Fax +41 22 749 09 47copyrightiso.orgwww.iso.orgBS ISO 6721-10:2015ISO 6721-10:2015(E)Foreword iv1 Scope . 12 Normative references 13 Terms and definitions . 14 Principle 25 Apparatus . 25.1 Measurement apparatus . 25.2 Temperature-controlled enclosure . 35.3 Temperature measurement and co
9、ntrol . 35.4 Plate/specimen assembly 45.5 Calibration 46 Sampling 47 Procedure. 57.1 Test temperature . 57.2 Zeroing the gap . 57.3 Introducing the test specimen . 57.4 Conditioning the test specimen 57.5 Test mode (controlled stress or controlled strain) 57.6 Determination of thermal stability of s
10、ample material . 67.7 Determination of region of linear-viscoelastic behaviour . 67.7.1 In the controlled-strain mode. 67.7.2 In the controlled-stress mode 67.7.3 Confirmation of linear-viscoelastic behaviour 77.8 Frequency sweep 77.9 Temperature sweep 77.10 Air entrapment 78 Expression of results 7
11、8.1 Symbols used 78.2 Calculation of complex shear modulus and complex shear viscosity 89 Precision 1010 Test report 11Annex A (informative) Uncertainty limits 12Annex B (informative) Verification of rheometer performance .15Bibliography .19 ISO 2015 All rights reserved iiiContents PageBS ISO 6721-1
12、0:2015ISO 6721-10:2015(E)ForewordISO (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
13、 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 Electrotechnical Commiss
14、ion (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 different approval criteria needed for the different types of ISO documents shou
15、ld 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 may be the subject of patent rights. ISO shall not be held responsible for ide
16、ntifying 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/patents).Any trade name used in this document is information given for the conven
17、ience 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 principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword -
18、 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), which has been technically revised to include informative guidance on verifica
19、tion 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-pendulum method Part 3: Flexural vibration Resonance-curve method Part 4: Tensile vibrat
20、ion 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-propagation method Part 9: Tensile vibration Sonic-pulse propagation method Part 10: Co
21、mplex shear viscosity using a parallel-plate oscillatory rheometer Part 11: Glass transition temperature Part 12: Compressive vibration Non-resonance methodAnnex A and Annex B of this part of ISO 6721 is for information only.iv ISO 2015 All rights reservedBS ISO 6721-10:2015INTERNATIONAL STANDARD IS
22、O 6721-10:2015(E)Plastics Determination of dynamic mechanical properties Part 10: Complex shear viscosity using a parallel-plate oscillatory rheometer1 ScopeThis part of ISO 6721 specifies the general principles of a method for determining the dynamic rheological properties of polymer melts at angul
23、ar 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 method is used to determine values of the following dynamic rheological properties: complex
24、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 measuring complex shear viscosity values typically up to 10 MPas (see Note 2).NOTE 1 The angular-
25、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 rads1, the test time can increase significantly as the time taken to obtain a single measurement is proportional to
26、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 high angular frequencies, the specimen can distort or fracture at the edge, consequently invalid
27、ating 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 of given dimensions, the upper limit of the range is limited by the machines torque capacity,
28、angular-displacement resolution, and compliance. However, correction can be made for compliance effects.2 Normative referencesThe following documents, in whole or in part, are normatively referenced in this document and are indispensable for its application. For dated references, only the edition ci
29、ted applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 472, Plastics VocabularyISO 5725-1, Accuracy (trueness and precision) of measurement methods and results Part 1: General principles and definitionsISO 6721-1, Plastics Determinat
30、ion of dynamic mechanical properties Part 1: General principles3 Terms and definitionsFor the purposes of this document, the terms and definitions given in ISO 6721-1, ISO 5725-1, ISO 472, and the following apply.3.1controlled-strain modetesting by applying a sinusoidal angular displacement of const
31、ant amplitude ISO 2015 All rights reserved 1BS ISO 6721-10:2015ISO 6721-10:2015(E)3.2controlled-stress modetesting by applying a sinusoidal torque of constant amplitude3.3complex shear viscosity*ratio of dynamic stress, given by (t) = 0exp it, and dynamic rate of strain where the shear strain dotnos
32、p 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 frequency, is the phase angle between the stress and strain, and t is timeNote 1 to entry: It is expressed in pa
33、scal seconds.3.4dynamic shear viscosityreal part of the complex shear viscosityNote 1 to entry: It is expressed in pascal seconds.3.5out-of-phase component of the complex shear viscosity”imaginary part of the complex shear viscosityNote 1 to entry: It is expressed in pascal seconds.4 PrincipleThe sp
34、ecimen 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 subjected to either a sinusoidal torque or a sinusoidal angular displacement of constant angular frequency. These are referr
35、ed 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 and displacement are measured. When using the controlled-strain mode, the resultant torque and the phase shift betwee
36、n 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 Clause 3) are determined from the measured torque and displacement and the specimen dimensions. In deriving these values
37、, 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 Apparatus5.1 Measurement apparatusThe measurement apparatus shall consist of two concentric, rigid, circular parallel plates between
38、 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 the apparatus are that it shall permit measurement of the amplitudes of the torque and the angular displacement and the pha
39、se 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 ISO 6721-10:2015ISO 6721-10:2015(E)A torque-measuring device shall be connected to one of the plates, thus permitting measurem
40、ent 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 permitting determination of its angular displacement and angular frequency.The apparatus shall be capable of measuring the torque to w
41、ithin 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 106rad.The apparatus shall be capable of measuring the angular frequency to within 2 % of the absolute value.Key1 test specimen angular
42、 frequencyd specimen thicknessD diameter of plateFigure 1 Parallel-plate rheometer geometry5.2 Temperature-controlled enclosureHeating may be provided by the use of forced convection, radio-frequency heating, or other suitable means.An environmental chamber surrounding the plate/specimen assembly ca
43、n 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 Temperature measurement and controlThe test temperature shall preferably be measured using a device that is either in contact with or embed
44、ded 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 temperatures 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
45、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/specimen assemblyThe plate/specimen assembly comprises two concentric, circular parallel plates with the specimen held between them. The plates shall h
46、ave 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 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 p
47、late 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 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
48、 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 low-viscosity polymeric liquids, it may be necessary to employ dimensions outside these recommended ranges. The total variation in the plate separat
49、ion 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-parallelism of the plates be less than 0,01 mm.5.5 CalibrationThe rheometer and test geometries shall be calibrated periodically by measuring the torque, angular-displacement, ang
