DIN EN ISO 1133-2-2012 Plastics - Determination of the melt mass-flow rate (MFR) and melt volume-flow rate (MVR) of thermoplastics - Part 2 Method for materials sensitive to time-t.pdf

1、March 2012 Translation by DIN-Sprachendienst.English price group 12No part of this translation may be reproduced without prior permission ofDIN Deutsches Institut fr Normung e. V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany,has the exclusive right of sale for German Standards (DIN-Normen).ICS

2、83.080.20!$zU“1875096www.din.deDDIN EN ISO 1133-2Plastics Determination of the melt mass-flow rate (MFR) and melt volume-flowrate (MVR) of thermoplastics Part 2: Method for materials sensitive to time-temperature history and/ormoisture (ISO 1133-2:2011)English translation of DIN EN ISO 1133-2:2012-0

3、3Kunststoffe Bestimmung der Schmelze-Masseflierate (MFR) und der Schmelze-Volumenflierate(MVR) von Thermoplasten Teil 2: Verfahren fr Materialien, die empfindlich gegen eine zeit- bzw.temperaturabhngige Vorgeschichte und/oder Feuchte sind (ISO 1133-2:2011)Englische bersetzung von DIN EN ISO 1133-2:2

4、012-03Plastiques Dtermination de lindice de fluidit chaud des thermoplastiques, en masse (MFR) et envolume (MVR) Partie 2: Mthode pour les matriaux sensibles lhistorique temps-temprature et/ou lhumidit (ISO 1133-2:2011)Traduction anglaise de DIN EN ISO 1133-2:2012-03Together with supersedesDIN EN IS

5、O 1133:2005-09www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.DIN EN ISO 1133-1:2012-03,2403.12 DIN EN ISO 1133-2:2012-03 2 A comma is used as the decimal marker. National foreword This standard has been prepared by Technical Commi

6、ttee ISO/TC 61 “Plastics” (Secretariat: SAC, China) in collaboration with Technical Committee CEN/TC 249 “Plastics” (Secretariat: NBN, Belgium). The responsible German body involved in its preparation was the Normenausschuss Kunststoffe (Plastics Standards Committee), Working Committee NA 054-01-03

7、AA Physikalische, rheologische und analytische Prfungen. DIN EN ISO 1133 consists of the following two parts: DIN EN ISO 1133-1, Plastics Determination of the melt mass-flow rate (MFR) and melt volume-flow rate (MVR) of thermoplastics Part 1: Standard method (ISO 1133-1:2011) DIN EN ISO 1133-2, Plas

8、tics Determination of the melt mass-flow rate (MFR) and melt volume-flow rate (MVR) of thermoplastics Part 2: Method for materials sensitive to time-temperature history and/or moisture (ISO 1133-2:2011) This new Part 2 of ISO 1133, together with the first edition of DIN EN ISO 1133-1, cancels and re

9、places DIN EN ISO 1133:2005-09. In DIN EN ISO 1133-1 changes have been made to accommodate DIN EN ISO 1133-2. DIN EN ISO 1133-1 applies to melt flow rate testing broadly equivalent to that of DIN EN ISO 1133:2005-09. This part of DIN EN ISO 1133 applies to the testing of polymers that are rheologica

10、lly sensitive to the time-temperature history to which they are subjected during melt flow rate testing. The DIN Standards corresponding to the International Standards referred to in this document are as follows: ISO 472 DIN EN ISO 472 ISO 15512 DIN EN ISO 15512 Amendments This standard differs from

11、 DIN EN ISO 1133:2005-09 as follows: a) the standard has been editorially revised; b) tighter tolerances on the temperature in the cylinder and on the time duration over which the material is subjected to that temperature have been specified; c) additional information for preparation and handling of

12、 moisture sensitive materials has been given. Previous editions DIN 53735: 1970-08, 1977-11, 1983-01, 1988-02 DIN ISO 1133: 1993-02 DIN EN ISO 1133: 2000-02, 2005-09 DIN EN ISO 1133-2:2012-03 3 National Annex NA (informative) Bibliography DIN EN ISO 472, Plastics Vocabulary DIN EN ISO 15512, Plastic

13、s Determination of water content DIN EN ISO 1133-2:2012-03 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 1133-2 December 2011 ICS 83.080.20 Supersedes EN ISO 1133:2005English Version Plastics - Determination of the melt mass-flow rate (MFR) and melt volu

14、me-flow rate (MVR) of thermoplastics - Part 2: Method for materials sensitive to time-temperature history and/or moisture (ISO 1133-2:2011) Plastiques - Dtermination de lindice de fluidit chaud des thermoplastiques, en masse (MFR) et en volume (MVR) - Partie 2: Mthode pour les matriaux sensibles lhi

15、storique temps-temprature et/ou lhumidit Kunststoffe - Bestimmung der Schmelze-Masseflierate (MFR) und der Schmelze-Volumenflierate (MVR) von Thermoplasten - Teil 2: Verfahren fr Materialien, die empfindlich gegen eine zeit- bzw. temperaturabhngige Vorgeschichte und/oder Feuchte sind (ISO 1133-2:201

16、1) This European Standard was approved by CEN on 30 November 2011. CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical

17、 references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member. This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of

18、 a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions. CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungar

19、y, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and United Kingdom. EUROPEAN COMMITTEE FOR STANDARDIZATION COMIT EUROPEN DE NORMALISATION EUROPISCHES KOMITEE FR NORMUNG Management Centre:

20、 Avenue Marnix 17, B-1000 Brussels 2011 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 1133-2:2011: E(ISO 1133-2:2011) Contents EN ISO 1133-2:2011 (E) DIN EN ISO 1133-2:2012-03 2 Page Foreword 3 Introduction .4 1 Scope 5 2 Nor

21、mative references 6 3 Terms and definitions .6 4 Principle 6 5 Apparatus .6 5.1 Extrusion plastometer .6 5.2 Accessory equipment .7 6 Test sample 8 6.1 Sample form .8 6.2 Sample pre-treatment and storage 8 7 Temperature verification, cleaning and maintenance of the apparatus 9 7.1 Verification of th

22、e temperature-control system 9 7.2 Cleaning the apparatus .9 7.3 Vertical alignment of the instrument .9 8 Procedural set-up 9 8.1 General 9 8.2 Selection of temperature and load .10 8.3 Cleaning 10 8.4 Selection of sample mass and charging the cylinder 10 9 Procedure .11 9.1 Selection of temperatur

23、e and load .11 9.2 Minimum piston displacement distance .11 9.3 Timer device .11 9.4 Preparation for the test .11 9.5 Measurement 11 9.6 Expression of results 12 10 Flow rate ratio (FRR) .12 11 Precision .12 12 Test report 13 Annex A (informative) Verification of temperature in the cylinder .14 Anne

24、x B (informative) Repeated MVR determinations on different materials carried out in line with this part of ISO 1133 18 Bibliography 20 Foreword This document (EN ISO 1133-2:2011) has been prepared by Technical Committee ISO/TC 61 Plastics” in collaboration with Technical Committee CEN/TC 249 “Plasti

25、cs” the secretariat of which is held by NBN. This European Standard shall be given the status of a national standard, either by publication of an identical text or by endorsement, at the latest by June 2012, and conflicting national standards shall be withdrawn at the latest by June 2012. Attention

26、is drawn to the possibility that some of the elements of this document may be the subject of patent rights. CEN and/or CENELEC shall not be held responsible for identifying any or all such patent rights. This document supersedes EN ISO 1133:2005. According to the CEN/CENELEC Internal Regulations, th

27、e national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Nether

28、lands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 1133-2:2011 has been approved by CEN as a EN ISO 1133-2:2011 without any modification. “ EN ISO 1133-2:2011 (E) DIN EN ISO 1133-2:2012-03 3 Introduction

29、This part of ISO 1133 provides a method that is appropriate to those materials that exhibit a high rheological sensitivity to the time-temperature history experienced by the sample during the test and/or moisture. For such materials, ISO 1133-1, which has less-tightly specified testing conditions th

30、an this part of ISO 1133, is considered to be unsuitable for obtaining data of an acceptable level of precision (i.e. at least equivalent to that obtained by ISO 1133-1 for stable materials). This part of ISO 1133 is considered to be particularly relevant for moisture sensitive materials.The primary

31、 difference between this part of ISO 1133 and ISO 1133-1 is that this part of ISO 1133 specifies tighter tolerances on the temperature, time line, sample amount and pre-treatment, resulting in more reproducible and accurate measurements.The accuracy of MVR determination of thermoplastic materials wh

32、ose rheological behaviour is affected by phenomena such as hydrolysis and condensation is often significantly influenced by: moisture content and sample conditioning; sample handling; a small difference in temperature, i.e. the temperature variation in the cylinder with position and/or time; the tot

33、al time that the material is exposed to the test temperature; the sample volume; sample form (shape and size pellets, powder, flake, etc.); cleaning of the apparatus.In order to obtain accurate repeatable and reproducible results, not only does the equipment need to meet the requirements specified i

34、n this part of ISO 1133, but also the material handling and test procedure need to be followed precisely and consistently, particularly with respect to those details mentioned above to which the results are sensitive. Minor deviations from the equipment requirements, procedure and/or sample handling

35、 can result in considerable loss of repeatability, reproducibility and accuracy of the measurement.In general, the test conditions for determination of MVR and MFR values are specified in the material standard and shall be referred to prior to conducting tests. Test conditions for the determination

36、of MVR and MFR of materials whose rheological behaviour is affected by hydrolysis, condensation or cross-linking during the measurement are in many cases not yet mentioned in the materials standards. Standards for these materials are likely to be revised or developed in the future. Where no relevant

37、 material standard exists or where no test conditions are specified, then the drying and test conditions should be agreed between the interested parties.NOTE At the time of publication, there is no evidence to suggest that the use of this part of ISO 1133 for stable materials results in better preci

38、sion in comparison with the use of ISO 1133-1.EN ISO 1133-2:2011 (E) DIN EN ISO 1133-2:2012-03 4 WARNING Persons using this document should be familiar with normal laboratory practice, if applicable. This document does not purport to address all of the safety problems, if any, associated with its us

39、e. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any regulatory requirements.IMPORTANT The equipment shall meet the requirements specified in this document and the measurements shall be carried out under specified conditions o

40、f temperature and load with special attention being paid to sample pre-treatment, strictly following the procedure prescribed in this document and in any applicable material standard.1 ScopeThis part of ISO 1133 specifies a procedure for the determination of the melt volume-flow rate (MVR) and melt

41、mass-flow rate (MFR) of thermoplastic materials that exhibit a high rheological sensitivity to the time-temperature history experienced by the sample during the test and/or to moisture.NOTE 1 Some grades of materials affected by hydrolysis are of, for example, poly(ethylene terephthalate) (PET), pol

42、y(butylene terephthalate) (PBT), poly(ethylene naphthalate) (PEN), other polyester types and polyamides; and by cross-linking are of, for example, thermoplastic elastomers (TPE) and thermoplastic vulcanizates (TPV). It is possible that this method will also be suitable for use with other materials.I

43、t is possible that this method will not be appropriate for materials whose rheological behaviour is extremely affected during testing (see Note 2).NOTE 2 For materials where the coefficient of variation of the MFR or MVR results is found to be higher than the precision mentioned in ISO 1133-1, the v

44、iscosity number in dilute solution (ISO 307, ISO 1628) can be more appropriate for characterization purposes.NOTE 3 Minor deviations from the equipment requirements, procedure and/or sample handling can result in considerable loss of reproducibility, repeatability and accuracy of the measurement. MV

45、R results determined on different materials, indicating the repeatability of the test method of this part of ISO 1133 when measured under ideal measurement conditions, are reported in Annex B.MFR values can be determined by calculation from MVR measurements provided the melt density at the test temp

46、erature and pressure is known, or by measurement using a cutting device provided that the accuracy of the measurement is at least the same as that of the MVR measurement.NOTE 4 The density of the melt is required at the test temperature and pressure. In practice, the pressure is low and values obtai

47、ned at the test temperature and ambient pressure suffice.The primary difference between this part of ISO 1133 and ISO 1133-1 is that this part of ISO 1133 specifies tighter tolerances on the temperature in the cylinder and on the time duration over which the material is subjected to that temperature

48、. Thus the time-temperature history of the material is more tightly controlled and consequently, for materials that are likely to be affected by exposure to elevated temperatures, the variability of test results is reduced compared with whether the specifications of ISO 1133-1 were used.EN ISO 1133-2:2011 (E) DIN EN ISO 1133-2:2012-03 5 This part of ISO 1133 also provides information for preparation and handling of moisture sensitive materials that again are critical to obtaining repeata