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1、 Reference number ISO 11443:2005(E) ISO 2005 INTERNATIONAL STANDARD ISO 11443 Second edition 2005-03-01 Plastics Determination of the fluidity of plastics using capillary and slit-die rheometers Plastiques Dtermination de la fluidit au moyen de rhomtres quips dune filire capillaire ou plate Copyrigh
2、t International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/11/2007 18:37:02 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11443:2005(E) PDF disclaimer This PDF file may cont
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5、ameters were optimized for printing. Every care has been taken to ensure that the file is suitable for use by ISO member bodies. In the unlikely event that a problem relating to it is found, please inform the Central Secretariat at the address given below. ISO 2005 All rights reserved. Unless otherw
6、ise specified, no part of this publication may be reproduced or utilized in any form or by any means, 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
7、office Case postale 56 CH-1211 Geneva 20 Tel. + 41 22 749 01 11 Fax + 41 22 749 09 47 E-mail copyrightiso.org Web www.iso.org Published in Switzerland ii ISO 2005 All rights reserved Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technic
8、al Standards 1/9972545001 Not for Resale, 04/11/2007 18:37:02 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11443:2005(E) ISO 2005 All rights reserved iii Contents Page Forewordiv 1 Scope1 2 Normative references .1 3 Terms and definitions.1 4 General principles.4 5 Ap
9、paratus.4 6 Sampling11 7 Procedure.11 8 Expression of results14 9 Precision22 10 Test report23 Annex A (informative) Method of correcting for the influence of H/B on the apparent shear rate.26 Annex B (informative) Measurement errors.28 Annex C (informative) Uncertainties in the determination of she
10、ar viscosity by capillary extrusion rheometry testing29 Bibliography .34 Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/11/2007 18:37:02 MDTNo reproduction or networking permitted witho
11、ut license from IHS -,-,- ISO 11443:2005(E) iv ISO 2005 All rights reserved 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
12、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. ISO collaborates clo
13、sely with the International Electrotechnical 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. Dra
14、ft International Standards adopted by the 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. Attention is drawn to the possibility that some of the elements of this docu
15、ment may be the subject of patent rights. ISO shall not be held responsible for identifying any or all such patent rights. ISO 11443 was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical- chemical properties. This second edition cancels and replaces the first edition (
16、ISO 11443:1995), of which Clause 4, Subclauses 5.1.2, 5.1.3, 5.1.4, 5.4, 5.5, 7.2 and 8.5, Clause 9 and Annex C have been technically revised. Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale
17、, 04/11/2007 18:37:02 MDTNo reproduction or networking permitted without license from IHS -,-,- INTERNATIONAL STANDARD ISO 11443:2005(E) ISO 2005 All rights reserved 1 Plastics Determination of the fluidity of plastics using capillary and slit-die rheometers 1 Scope This International Standard speci
18、fies methods for determining the fluidity of plastics melts subjected to shear stresses at rates and temperatures approximating to those arising in plastics processing. Testing plastics melts in accordance with these methods is necessary since the fluidity of plastics melts is generally not dependen
19、t solely on temperature, but also on other parameters, in particular shear rate and shear stress. The methods described in this International Standard are useful for determining melt viscosities from 10 Pas to 107 Pas, depending on the measurement range of the pressure and/or force transducer and th
20、e mechanical and physical characteristics of the rheometer. The shear rates occurring in extrusion rheometers range from 1 s1 to 106 s1. Elongational effects at the die entrance cause extrudate swelling at the die exit. Methods for assessing extrudate swelling have also been included. The rheologica
21、l techniques described are not limited to the characterization of wall-adhering thermoplastics melts only: for example, thermoplastics exhibiting “slip” effects 1, 2 and thermosetting plastics can be included. However, the methods used for determining the shear rate and shear viscosity are invalid f
22、or materials which are not wall-adhering. Nevertheless, the standard can be used to characterize the rheological behaviour of such fluids for a given geometry. 2 Normative references The following referenced documents are indispensable for the application of this document. For dated references, only
23、 the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies. ISO 4287, Geometrical Product Specifications (GPS) Surface texture: Profile method Terms, definitions and surface texture parameters ISO 6507-1, Metallic materials Vi
24、ckers hardness test Part 1: Test method ISO 11403-2, Plastics Acquisition and presentation of comparable multipoint data Part 2: Thermal and processing properties ISO 1133, Plastics Determination of the melt mass-flow rate (MFR) and the melt volume-flow rate (MVR) of thermoplastics 3 Terms and defin
25、itions For the purposes of this document, the following terms and definitions apply. 3.1 Newtonian fluid fluid for which the viscosity is independent of the shear rate and of time Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical
26、Standards 1/9972545001 Not for Resale, 04/11/2007 18:37:02 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11443:2005(E) 2 ISO 2005 All rights reserved 3.2 non-Newtonian fluid fluid for which the viscosity varies with the shear rate and/or with time NOTE For the purpose
27、s of this International Standard, this definition refers to fluids for which the viscosity varies only with the shear rate. 3.3 apparent shear stress ap fictive shear stress to which the melt in contact with the die wall is subjected, expressed in pascals (Pa) NOTE It is calculated as the product of
28、 test pressure and the ratio of die cross-sectional area to die-wall area. 3.4 apparent shear rate ap ? fictive shear rate that the melt at the wall would experience at the observed volume flow rate if its behaviour were Newtonian, expressed in reciprocal seconds (s1). 3.5 true shear stress actual s
29、hear stress to which the melt in contact with the die wall is subjected, expressed in pascals (Pa) NOTE 1 It is estimated from the test pressure p by applying corrections for entrance and exit pressure losses, or is directly determined from the melt-pressure gradient in the channel. NOTE 2 For the p
30、urposes of notation, the absence of a subscript is used to denote true values. 3.6 true shear rate ? shear rate obtained from the apparent shear rate ap ? by taking into account the deviations from Newtonian behaviour by appropriate correction algorithms (see Note to 8.2.2), expressed in reciprocal
31、seconds (s1) NOTE For the purposes of notation, the absence of a subscript is used to denote true values. 3.7 viscosity viscosity in steady shear, defined as the ratio /? of true shear stress t to true shear rate ?, expressed in pascal seconds (Pas) 3.8 apparent viscosity ap ratio ap/ ap ? of appare
32、nt shear stress ap to apparent shear rate ap ?, expressed in pascal seconds (Pas) 3.9 Bagley corrected apparent viscosity apB ratio / ap ? of true shear stress to apparent shear rate ap ?, expressed in pascal seconds (Pas) 3.10 Rabinowitsch corrected apparent viscosity apR ratio ap/? of apparent she
33、ar stress ap to true shear rate ?, expressed in pascal seconds (Pas) Copyright International Organization for Standardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/11/2007 18:37:02 MDTNo reproduction or networking permitted without l
34、icense from IHS -,-,- ISO 11443:2005(E) ISO 2005 All rights reserved 3 NOTE This term is appropriate for use when testing with a single die of large length to diameter aspect ratio for which entrance effects are negligible. 3.11 volume flow rate Q volume of melt flowing through the die per unit time
35、, expressed in cubic millimetres per second (mm3/s) 3.12 swell ratio at room temperature Sa ratio of the diameter of the extrudate to the diameter of the capillary die, both measured at room temperature 3.13 swell ratio at the test temperature ST ratio of the diameter of the extrudate to the diamete
36、r of the capillary die, both measured at the test temperature 3.14 percent swell at room temperature sa difference between the diameter of the extruded strand and the diameter of the capillary die, expressed as a percentage of the diameter of the capillary die, both measured at room temperature 3.15
37、 percent swell at the test temperature sT difference between the diameter of the extruded strand and the diameter of the capillary die, expressed as a percentage of the diameter of the capillary die, both measured at the test temperature NOTE Equivalent slit-die extrudate swell terms can be derived,
38、 based on the thickness of slit-die extrudate with reference to the slit-die thickness. 3.16 preheating time time interval between completion of charging of the barrel and the beginning of measurement 3.17 dwell time time interval between the completion of charging of the barrel and the end of measu
39、rements NOTE In certain special cases, it may be necessary to note the dwell time at the end of each measurement where more than one measurement per barrel filling is made. 3.18 extrusion time time corresponding to the period of measurement for a given shear rate 3.19 critical shear stress value of
40、the shear stresses at the die wall at which any of the following occur: a discontinuity in the curve plotting shear stress against flow rate or shear rate; roughness (or waving) of the extrudate as it leaves the die NOTE It is expressed in pascals (Pa). Copyright International Organization for Stand
41、ardization Provided by IHS under license with ISO Licensee=NASA Technical Standards 1/9972545001 Not for Resale, 04/11/2007 18:37:02 MDTNo reproduction or networking permitted without license from IHS -,-,- ISO 11443:2005(E) 4 ISO 2005 All rights reserved 3.20 critical shear rate shear rate correspo
42、nding to the critical shear stress, expressed in reciprocal seconds (s1) 4 General principles The plastics melt is forced through a capillary or slit die of known dimensions. Two principal methods can be used: for a specified constant test pressure p the volume flow rate Q is measured (method 1), or
43、 for a specified constant volume flow rate Q the test pressure p is measured (method 2). These methods can be used with capillary dies (method A) and slit dies (method B). For full designation of the test-method options, see Table 1. Table 1 Designation of test methods Preset parameter Die cross-sec
44、tion Test pressure, p Volume flow rate, Q Circular (capillary die) A1 A2 Rectangular (slit die) B1 B2 Measurements can be made using a range of values of the preset parameter (either applied test pressure in method 1, or volume flow rate in method 2). If a slit die with pressure transducers position
45、ed along its length and also upstream of the die entry is used, then entrance and exit pressure-drop values can be determined. If capillary dies of the same radius but of varying length are used, then the sum of the entrance and exit pressure drops can be determined. A slit die with pressure transdu
46、cers positioned along its length is particularly suited for automated measurements using on-line computer evaluation. Recommended values for capillary die dimensions and for flow rates and temperatures to be used in testing are presented either in the relevant clauses below or in ISO 11403-2. NOTE I
47、n using a slit die, either the aspect ratio H/B between the thickness H and the width B of the slit is small or else a correction for H/B (see Annex A) is necessary. In the latter case, the calculated quantities are dependent on assumptions made in deriving the correction equations used, notably tha
48、t elastic effects are irrelevant. 5 Apparatus 5.1 Test device 5.1.1 General The test device shall consist of a heatable barrel, the bore of which is closed at the bottom end by an interchangeable capillary or slit die. The test pressure shall be exerted on the melt contained in this barrel by a piston, screw or by the use of gas pressure. Figures 1 and 2 show typical examples; other dimensions are permitted. Copyright International Organization for Standardization Provid