DIN EN ISO 1133-1-2012 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) German.pdf

1、March 2012 Translation by DIN-Sprachendienst.English price group 15No 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“1875097www.din.deDDIN EN ISO 1133-1Plastics Determination of the melt mass-flow rate (MFR) and melt volume-flowrate (MVR) of thermoplastics Part 1: Standard method (ISO 1133-1:2011)English translation of DIN EN ISO 1133-1:2012-03Kunststoffe Bestimmung der Schmelze-Masseflierate (MFR) u

3、nd der Schmelze-Volumenflierate(MVR) von Thermoplasten Teil 1: Allgemeines Prfverfahren (ISO 1133-1:2011)Englische bersetzung von DIN EN ISO 1133-1:2012-03Plastiques Dtermination de lindice de fluidit chaud des thermoplastiques, en masse (MFR) et envolume (MVR) Partie 1: Mthode normale (ISO 1133-1:2

4、011)Traduction anglaise de DIN EN ISO 1133-1:2012-03Together with supersedesDIN EN ISO 1133:2005-09www.beuth.deDocument comprises pagesIn case of doubt, the German-language original shall be considered authoritative.DIN EN ISO 1133-2:2012-03,3203.12 DIN EN ISO 1133-1:2012-03 2 A comma is used as the

5、 decimal marker. National foreword This standard has been prepared by Technical Committee 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 Normen

6、ausschuss Kunststoffe (Plastics Standards Committee), Working Committee NA 054-01-03 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

7、) of thermoplastics Part 1: Standard method (ISO 1133-1:2011) DIN EN ISO 1133-2, 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-temperature history and/or moisture (ISO 1133-2:2011) This first e

8、dition of DIN EN ISO 1133-1, together with the new Part 2 of ISO 1133, cancels and replaces DIN EN ISO 1133:2005-09. In this part of DIN EN ISO 1133, changes have been made to accommodate DIN EN ISO 1133-2. This part of DIN EN ISO 1133 applies to melt flow rate testing broadly equivalent to that of

9、DIN EN ISO 1133:2005-09. DIN EN ISO 1133-2 applies to the testing of polymers that are rheologically sensitive to the time-temperature history to which they are subjected during melt flow rate testing. Amendments This standard differs from DIN EN ISO 1133:2005-09 as follows: a) the standard number h

10、as been changed to reflect the fact that it is now in two parts; b) the standard has been editorially revised; c) normative references have been updated; d) Clause 3 now includes further terms and definitions relevant to both parts of DIN EN ISO 1133; e) Subclause 5.1.3 (formerly 5.1.2) “Piston” now

11、 also specifies the lower edge of the piston head; f) in Subclause 5.1.4 (formerly 5.1.3) “Temperature-control system” temperature tolerances have been updated; g) Subclause 5.2.1.7 “Preforming device” has been added; h) in Subclause 5.2.2.2 “Timer” details regarding cut-off timing accuracy have bee

12、n changed; i) Subclause 7.3 “Vertical alignment of the instrument” has been added; j) Subclause 8.3 “Selection of sample mass and charging the cylinder” now provides cut-off time intervals that are consistent with other specifications in this part of DIN EN ISO 1133; k) Subclauses 8.5.3 and 9.6.3 “E

13、xpression of results: half size die” have been included; l) Subclause 9.2 “Cleaning” has been included; DIN EN ISO 1133-1:2012-03 3 m) Subclause 9.3 (formerly 9.2) “Minimum piston displacement distance” now provides minimum piston displacements that are consistent with other specifications in this p

14、art of DIN EN ISO 1133; n) Annex B (informative) “Conditions specified in International Standards for the determination of the melt flow rate of thermoplastic materials” has been simplified to avoid inconsistencies between this and the materials specification standards; o) Annex C (informative) “Dev

15、ice and procedure for preforming a compacted charge of material by compression” has been included; p) Annex D (informative) “Precision data for polypropylene obtained from an intercomparison of MFR and MVR testing” has been included. Previous editions DIN 53735: 1970-08, 1977-11, 1983-01, 1988-02 DI

16、N ISO 1133: 1993-02 DIN EN ISO 1133: 2000-02, 2005-09 DIN EN ISO 1133-1:2012-03 4 This page is intentionally blank EUROPEAN STANDARD NORME EUROPENNE EUROPISCHE NORM EN ISO 1133-1 December 2011 ICS 83.080.20 Supersedes EN ISO 1133:2005English Version Plastics - Determination of the melt mass-flow rat

17、e (MFR) and melt volume-flow rate (MVR) of thermoplastics - Part 1: Standard method (ISO 1133-1:2011) Plastiques - Dtermination de lindice de fluidit chaud des thermoplastiques, en masse (MFR) et en volume (MVR) - Partie 1: Mthode normale (ISO 1133-1:2011) Kunststoffe - Bestimmung der Schmelze-Masse

18、flierate (MFR) und der Schmelze-Volumenflierate (MVR) von 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 witho

19、ut any alteration. Up-to-date lists and bibliographical 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 l

20、anguage made by translation under the responsibility of 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, Den

21、mark, Estonia, Finland, France, Germany, Greece, Hungary, 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 NORMALIS

22、ATION EUROPISCHES KOMITEE FR NORMUNG Management Centre: 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 1133-1:2011: EThermoplasten - Teil 1: Allgemeines Prfverfahren (ISO 1133-1:2011) Con

23、tents DIN EN ISO 1133-1:2012-03 EN ISO 1133-1:2011 (E) 2 Page Foreword 3 Introduction .4 1 Scope 5 2 Normative references 5 3 Terms and definitions .5 4 Principle 6 5 Apparatus .7 5.1 Extrusion plastometer .7 5.2 Accessory equipment .11 6 Test sample 12 6.1 Sample form .12 6.2 Conditioning .12 7 Tem

24、perature verification, cleaning and maintenance of the apparatus 13 7.1 Verification of the temperature control system 13 7.2 Cleaning the apparatus .14 7.3 Vertical alignment of the instrument .14 8 Procedure A: mass-measurement method .14 8.1 Selection of temperature and load .14 8.2 Cleaning 14 8

25、.3 Selection of sample mass and charging the cylinder 14 8.4 Measurements 15 8.5 Expression of results 16 9 Procedure B: displacement-measurement method .17 9.1 Selection of temperature and load .17 9.2 Cleaning 17 9.3 Minimum piston displacement distance .17 9.4 Selection of sample mass and chargin

26、g the cylinder 17 9.5 Measurements 17 9.6 Expression of results 18 10 Flow rate ratio (FRR) .19 11 Precision .20 12 Test report 20 Annex A (normative) Test conditions for MFR and MVR determinations .22 Annex B (informative) Conditions specified in International Standards for the determination of the

27、 melt flow rate of thermoplastic materials 23 Annex C (informative) Device and procedure for preforming a compacted charge of material by compression .24 Annex D (informative) Precision data for polypropylene obtained from an intercomparison of MFR and MVR testing .27 Bibliography 28 Foreword This d

28、ocument (EN ISO 1133-1:2011) has been prepared by Technical Committee ISO/TC 61 Plastics” in collaboration with Technical Committee CEN/TC 249 “Plastics” 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 iden

29、tical text or by endorsement, at the latest by June 2012, and conflicting national standards shall be withdrawn at the latest by June 2012. Attention 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 respo

30、nsible for identifying any or all such patent rights. This document supersedes EN ISO 1133:2005. According to the CEN/CENELEC Internal Regulations, the national standards organizations of the following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria, Croatia, Cypr

31、us, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. Endorsement notice The text of ISO 11

32、33-1:2011 has been approved by CEN as a EN ISO 1133-1:2011 without any modification. DIN EN ISO 1133-1:2012-03 EN ISO 1133-1:2011 (E) 3 “ IntroductionFor stable materials that are not rheologically sensitive to the time-temperature history experienced during melt flow rate testing, this part of ISO

33、1133 is recommended.For materials whose rheological behaviour is sensitive to the tests time-temperature history, e.g. materials which degrade during the test, ISO 1133-2 is recommended.NOTE At the time of publication, there is no evidence to suggest that the use of ISO 1133-2 for stable materials r

34、esults in better precision in comparison with the use of this part of ISO 1133.DIN EN ISO 1133-1:2012-03 EN ISO 1133-1:2011 (E) 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 problem

35、s, if any, associated with its use. It is the responsibility of the user to establish appropriate safety and health practices and to ensure compliance with any regulatory requirements.1 ScopeThis part of ISO 1133 specifies two procedures for the determination of the melt mass-flow rate (MFR) and the

36、 melt volume-flow rate (MVR) of thermoplastic materials under specified conditions of temperature and load. Procedure A is a mass-measurement method. Procedure B is a displacement-measurement method. Normally, the test conditions for measurement of melt flow rate are specified in the material standa

37、rd with a reference to this part of ISO 1133. The test conditions normally used for thermoplastics are listed in Annex A.The MVR is particularly useful when comparing materials of different filler content and when comparing filled with unfilled thermoplastics. The MFR can be determined from MVR meas

38、urements, or vice versa, provided the melt density at the test temperature is known.This part of ISO 1133 is also possibly applicable to thermoplastics for which the rheological behaviour is affected during the measurement by phenomena such as hydrolysis (chain scission), condensation and cross-link

39、ing, but only if the effect is limited in extent and only if the repeatability and reproducibility are within an acceptable range. For materials which show significantly affected rheological behaviour during testing, this part of ISO 1133 is not appropriate. In such cases, ISO 1133-2 applies.NOTE Th

40、e rates of shear in these methods are much smaller than those used under normal conditions of processing, and therefore it is possible that data obtained by these methods for various thermoplastics will not always correlate with their behaviour during processing. Both methods are used primarily in q

41、uality control.2 Normative referencesThe following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest edition of the referenced document (including any amendments) applies.ISO 1133-2, P

42、lastics Determination of the melt mass-flow rate (MFR) and melt volume-rate (MVR) of thermoplastics Part 2: Method for materials sensitive to time-temperature history and/or moistureISO 4287, Geometrical Product Specifications (GPS) Surface texture: Profile method Terms, definitions and surface text

43、ure parametersISO 6507-1, Metallic materials Vickers hardness test Part 1: Test method3 Terms and definitionsFor the purpose of this document, the following terms and definitions apply.DIN EN ISO 1133-1:2012-03 EN ISO 1133-1:2011 (E) 5 3.1melt mass-flow rateMFRrate of extrusion of a molten resin thr

44、ough a die of specified length and diameter under prescribed conditions of temperature, load and piston position in the cylinder of an extrusion plastometer, the rate being determined as the mass extruded over a specified timeNOTE MFR is expressed in units of grams per 10 min. Alternative units acce

45、pted by SI are decigrams per minute, where 1 g/10 min is equivalent to 1 dg/min.3.2melt volume-flow rateMVRrate of extrusion of a molten resin through a die of specified length and diameter under prescribed conditions of temperature, load and piston position in the cylinder of an extrusion plastomet

46、er, the rate being determined as the volume extruded over a specified timeNOTE MVR is expressed in units of cubic centimetres per 10 min.3.3loadcombined force exerted by the mass of the piston and the added weight, or weights, as specified by the conditions of the testNOTE Load is expressed as the m

47、ass, in kilograms, exerting it.3.4preformed compacted chargetest sample prepared as a compressed charge of polymer sampleNOTE In order to introduce samples quickly into the bore of the cylinder and to ensure void-free extrudate, it may be necessary to preform samples originally in the form of, for e

48、xample, powders or flakes into a compacted charge.3.5time-temperature historyhistory of the temperature and time to which the sample is exposed during testing including sample preparation3.6standard diedie having a nominal length of 8,000 mm and a nominal bore diameter of 2,095 mm3.7half size diedie having a nominal length of 4,000 mm and a nominal bore diameter of 1,050 mm3.8moisture-sensitive plasticsplastics having rheological properties that are sensitive to their moisture contentNOTE Plastics which, when