1、BSI Standards PublicationBS ISO 11443:2014Plastics Determinationof the fluidity of plasticsusing capillary and slit-dierheometersBS ISO 11443:2014 BRITISH STANDARDNational forewordThis British Standard is the UK implementation of ISO 11443:2014. Itsupersedes BS ISO 11443:2005 which is withdrawn.The
2、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 publication does not purport to include all the necessaryprovisions of a contract. Users are respo
3、nsible for its correctapplication. The British Standards Institution 2014. Published by BSI StandardsLimited 2014ISBN 978 0 580 84785 1ICS 83.080.01Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards
4、Policy and Strategy Committee on 31 March 2014.Amendments issued since publicationDate Text affectedBS ISO 11443:2014 ISO 2014Plastics Determination of the fluidity of plastics using capillary and slit-die rheometersPlastiques Dtermination de la fluidit au moyen de rhomtres quips dune filire capilla
5、ire ou plateINTERNATIONAL STANDARDISO11443Third edition2014-04-01Reference numberISO 11443:2014(E)BS ISO 11443:2014ISO 11443:2014(E)ii ISO 2014 All rights reservedCOPYRIGHT PROTECTED DOCUMENT ISO 2014All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or ut
6、ilized otherwise in any form or by any means, electronic 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 copyri
7、ght officeCase postale 56 CH-1211 Geneva 20Tel. + 41 22 749 01 11Fax + 41 22 749 09 47E-mail copyrightiso.orgWeb www.iso.orgPublished in SwitzerlandBS ISO 11443:2014ISO 11443:2014(E) ISO 2014 All rights reserved iiiContents PageForeword iv1 Scope . 12 Normative references 13 Terms and definitions .
8、14 General principles . 45 Apparatus . 45.1 Test device 45.2 Temperature control 95.3 Measurement of temperature and calibration 95.4 Measurement of pressure and calibration . 105.5 Measurement of the volume flow rate of the sample .116 Sampling .117 Procedure117.1 Cleaning the test device 117.2 Sel
9、ection of test temperatures 117.3 Preparation of samples . 127.4 Preheating 137.5 Determination of the maximum permissible test duration 137.6 Determination of test pressure at constant volume flow rate: Method 2 .137.7 Determination of volume flow rate at constant test pressure: Method 1 .137.8 Wai
10、ting periods during measurement. 147.9 Measurement of extrudate swelling 148 Expression of results .158.1 Volume flow rate .158.2 Apparent shear rate .158.3 Apparent shear stress 168.4 True shear stress 178.5 True shear rate . 218.6 Viscosity . 228.7 Determination of extrudate swelling 229 Precision
11、 2310 Test report 2410.1 General 2410.2 Test conditions . 2410.3 Flow characteristics .2510.4 Visual examination .26Annex A (informative) Method of correcting for the influence of H/B on the apparent shear rate .27Annex B (informative) Measurement errors .29Annex C (informative) Uncertainties in the
12、 determination of shear viscosity by capillary extrusion rheometry testing .30Bibliography .36BS ISO 11443:2014ISO 11443:2014(E)ForewordISO (the International Organization for Standardization) is a worldwide federation of national standards bodies (ISO member bodies). The work of preparing Internati
13、onal Standards is normally carried 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 IS
14、O, also take part in the work. 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, Par
15、t 1. In particular the different 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
16、elements of this document may 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 rec
17、eived (see www.iso.org/patents). 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 a
18、dherence to the WTO principles in the Technical Barriers to Trade (TBT) see the following URL: Foreword - Supplementary informationThe committee responsible for this document is ISO/TC 61, Plastics, Subcommittee SC 5, Physical-chemical properties.This third edition cancels and replaces the second ed
19、ition (ISO 11443:2005), of which it constitutes a minor revision with the following changes: polybutene-1 (PB-1) with typical temperature range of 150 C to 230 C has been added in Table 3; normative references have been updated.iv ISO 2014 All rights reservedBS ISO 11443:2014INTERNATIONAL STANDARD I
20、SO 11443:2014(E)Plastics Determination of the fluidity of plastics using capillary and slit-die rheometers1 ScopeThis International Standard specifies methods for determining the fluidity of plastics melts subjected to shear stresses at rates and temperatures approximating to those arising in plasti
21、cs processing. Testing plastics melts in accordance with these methods is necessary since the fluidity of plastics melts is generally not dependent solely on temperature, but also on other parameters, in particular shear rate and shear stress.The methods described in this International Standard are
22、useful for determining melt viscosities from 10 Pas to 107Pas, depending on the measurement range of the pressure and/or force transducer and the mechanical and physical characteristics of the rheometer. The shear rates occurring in extrusion rheometers range from 1 s1to 106s1.Elongational effects a
23、t the die entrance cause extrudate swelling at the die exit. Methods for assessing extrudate swelling have also been included.The rheological techniques described are not limited to the characterization of wall-adhering thermoplastics melts only; for example, thermoplastics exhibiting “slip” effects
24、12and thermosetting plastics can be included. However, the methods used for determining the shear rate and shear viscosity are invalid for materials which are not wall-adhering. Nevertheless, this International Standard can be used to characterize the rheological behaviour of such fluids for a given
25、 geometry.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 cited applies. For undated references, the latest edition of the referenced document (including
26、any amendments) applies.ISO 1133-1, Plastics Determination of the melt mass-flow rate (MFR) and melt volume-flow rate (MVR) of thermoplastics Part 1: Standard methodISO 1133-2, Plastics Determination of the melt mass-flow rate (MFR) and melt volume-flow rate (MVR) of thermoplastics Part 2: Method fo
27、r materials sensitive to time-temperature history and/or moistureISO 4287, Geometrical Product Specifications (GPS) Surface texture: Profile method Terms, definitions and surface texture parametersISO 6507-1, Metallic materials Vickers hardness test Part 1: Test methodISO 11403-2, Plastics Acquisiti
28、on and presentation of comparable multipoint data Part 2: Thermal and processing properties3 Terms and definitionsFor the purposes of this document, the following terms and definitions apply.3.1Newtonian fluidfluid for which the viscosity is independent of the shear rate and of time ISO 2014 All rig
29、hts reserved 1BS ISO 11443:2014ISO 11443:2014(E)3.2non-Newtonian fluidfluid for which the viscosity varies with the shear rate and/or with timeNote 1 to entry: For the purposes of this International Standard, this definition refers to fluids for which the viscosity varies only with the shear rate.3.
30、3apparent shear stressapfictive shear stress to which the melt in contact with the die wall is subjected, expressed in pascals (Pa)Note 1 to entry: It is calculated as the product of test pressure and the ratio of die cross-sectional area to die wall area.3.4apparent shear rateapfictive shear rate t
31、hat the melt at the wall would experience at the observed volume flow rate if its behaviour were Newtonian, expressed in reciprocal seconds (s1)3.5true shear stressactual shear stress to which the melt in contact with the die wall is subjected, expressed in pascals (Pa)Note 1 to entry: It is estimat
32、ed 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 to entry: For the purposes of notation, the absence of a subscript is used to denote true values.3.6true shear rateshear rate obt
33、ained from the apparent shear rate apby taking into account the deviations from Newtonian behaviour by appropriate correction algorithms (see Note to 8.2.2), expressed in reciprocal seconds (s1)Note 1 to entry: For the purposes of notation, the absence of a subscript is used to denote true values.3.
34、7viscosityviscosity in steady shear, defined as the ratio / of true shear stress to true shear rate , expressed in pascal seconds (Pas)3.8apparent viscosityapratio / apof apparent shear stress apto apparent shear rate ap, expressed in pascal seconds (Pas)3.9Bagley corrected apparent viscosityapBrati
35、o / apof true shear stress to apparent shear rate ap, expressed in pascal seconds (Pas)2 ISO 2014 All rights reservedBS ISO 11443:2014ISO 11443:2014(E)3.10Rabinowitsch corrected apparent viscosityapRratio ap/ of apparent shear stress apto true shear rate , expressed in pascal seconds (Pas)Note 1 to
36、entry: 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.3.11volume flow rateQvolume of melt flowing through the die per unit time, expressed in cubic millimetres per second (mm3/s)3.12swell ratio at roo
37、m temperatureSaratio of the diameter of the extrudate to the diameter of the capillary die, both measured at room temperature3.13swell ratio at the test temperatureSTratio of the diameter of the extrudate to the diameter of the capillary die, both measured at the test temperature3.14percent swell at
38、 room temperaturesadifference 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 temperature3.15percent swell at the test temperaturesTdifference between the diameter of the extruded
39、 strand and the diameter of the capillary die, expressed as a percentage of the diameter of the capillary die, both measured at the test temperatureNote 1 to entry: Equivalent slit-die extrudate swell terms can be derived based on the thickness of slit-die extrudate with reference to the slit-die th
40、ickness.3.16preheating timetime interval between completion of charging of the barrel and the beginning of measurement3.17dwell timetime interval between the completion of charging of the barrel and the end of measurementsNote 1 to entry: In certain special cases, it can be necessary to note the dwe
41、ll time at the end of each measurement where more than one measurement per barrel filling is made.3.18extrusion timetime corresponding to the period of measurement for a given shear rate3.19critical shear stressvalue of the shear stresses at the die wall at which any of the following occur: a discon
42、tinuity in the curve plotting shear stress against flow rate or shear rate; roughness (or waving) of the extrudate as it leaves the die ISO 2014 All rights reserved 3BS ISO 11443:2014ISO 11443:2014(E)Note 1 to entry: It is expressed in pascals (Pa).3.20critical shear rateshear rate corresponding to
43、the critical shear stress, expressed in reciprocal seconds (s1)4 General principlesThe 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 for a spe
44、cified 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 methodsDie cross sec-tionPreset parameterTest pr
45、essure, pVolume flow rate, QCircular (capillary die)A1 A2Rectangular (slit die)B1 B2Measurements 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 positioned along its length
46、 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 lengths are used, then the sum of the entrance and exit pressure drops can be determined.A slit die with pressure transducers positioned alo
47、ng its length is particularly suited for automated measurements using online 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 In using a slit die, ei
48、ther 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 formulae used, notably that elastic effects are i
49、rrelevant.5 Apparatus5.1 Test device5.1.1 GeneralThe 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.5.1.2 Rheometer barrelThe barrel shall consist of a material resistant to wear and co
