Plastics - Determination of the melt mass-flow rate (MFR) and melt volume-flow rate (MVR) of thermoplastics - Part 1: Standard method (ISO 1133-1:2022)

Kunststoffe - Bestimmung der Schmelze-Massefließrate (MFR) und der Schmelze-Volumenfließrate (MVR) von Thermoplasten - Teil 1: Allgemeines Prüfverfahren (ISO 1133-1:2022)

Dieses Dokument legt zwei Verfahren für die Bestimmung der Schmelze Massefließrate (MFR, en: melt mass flow rate) und der Schmelze Volumenfließrate (MVR, en: melt volume flow rate) von thermoplastischen Materialien unter festgelegten Bedingungen für Temperatur und Belastung fest. Verfahren A dient zum Bestimmen der Masse. Verfahren B ist ein Messverfahren für die Weglänge. Üblicherweise sind die Prüfbedingungen für die Messung der Schmelze Fließrate in der Werkstoffnorm mit einem Verweis auf dieses Dokument festgelegt. Die üblicherweise für Thermoplaste angewendeten Prüfbedingungen sind in Anhang A aufgeführt.
Die MVR ist für den Vergleich von Werkstoffen mit unterschiedlichen Füllstoffgehalten und für den Vergleich von gefüllten und ungefüllten Thermoplasten besonders nützlich. Die MFR kann anhand von MVR Messungen bestimmt werden, oder umgekehrt, wenn die Dichte der Schmelze bei der Prüftemperatur bekannt ist.
Dieses Dokument ist auch auf Thermoplaste anwendbar, deren rheologisches Verhalten während der Messung z. B. durch Hydrolyse (Kettenspaltung), Kondensation und Vernetzung beeinflusst wird, jedoch nur dann, wenn diese Beeinflussung begrenzt ist und wenn die Wiederhol  und Vergleichpräzision innerhalb eines zulässigen Bereiches liegen. Für Werkstoffe, die bei der Prüfung ein deutlich beeinflusstes rheologisches Verhalten aufweisen, ist dieses Dokument nicht geeignet. In diesen Fällen gilt ISO 1133 2.
ANMERKUNG   Die Schergeschwindigkeiten bei diesen Verfahren sind wesentlich geringer als diejenigen, die unter den üblichen Verarbeitungsbedingungen angewendet werden, weshalb es möglich ist, dass die Daten, die mit diesen Verfahren für die verschiedenen Thermoplaste erhalten wurden, nicht immer mit ihrem Verhalten bei der Verarbeitung korrelieren. Beide Verfahren werden in erster Linie zur Qualitätskontrolle angewendet.
WARNUNG — Personen, die dieses Dokument anwenden, sollten gegebenenfalls mit der üblichen Laborpraxis vertraut sein. Dieses Dokument erhebt nicht den Anspruch, alle gegebenenfalls mit seiner Anwendung verbundenen Sicherheitsprobleme zu behandeln. Es liegt in der Verantwortung des Anwenders, geeignete Vorkehrungen für den Arbeits und Gesundheitsschutz zu treffen und die Einhaltung jeglicher gesetzlicher Bestimmungen sicherzustellen.

Plastiques - Détermination de l'indice de fluidité à chaud des thermoplastiques, en masse (MFR) et en volume (MVR) - Partie 1: Méthode normale (ISO 1133-1:2022)

Polimerni materiali - Ugotavljanje masnega (MFR) in prostorninskega pretoka taline (MVR) plastomerov - 1. del: Standardna metoda (ISO 1133-1:2022)

General Information

Status
Published
Public Enquiry End Date
22-May-2022
Publication Date
17-Jul-2022
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
13-Jul-2022
Due Date
17-Sep-2022
Completion Date
18-Jul-2022

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SLOVENSKI STANDARD
SIST EN ISO 1133-1:2022
01-september-2022
Nadomešča:
SIST EN ISO 1133-1:2012
Polimerni materiali - Ugotavljanje masnega (MFR) in prostorninskega pretoka
taline (MVR) plastomerov - 1. del: Standardna metoda (ISO 1133-1:2022)

Plastics - Determination of the melt mass-flow rate (MFR) and melt volume-flow rate

(MVR) of thermoplastics - Part 1: Standard method (ISO 1133-1:2022)
Kunststoffe - Bestimmung der Schmelze-Massefließrate (MFR) und der Schmelze-

Volumenfließrate (MVR) von Thermoplasten - Teil 1: Allgemeines Prüfverfahren (ISO

1133-1:2022)

Plastiques - Détermination de l'indice de fluidité à chaud des thermoplastiques, en

masse (MFR) et en volume (MVR) - Partie 1: Méthode normale (ISO 1133-1:2022)
Ta slovenski standard je istoveten z: EN ISO 1133-1:2022
ICS:
83.080.20 Plastomeri Thermoplastic materials
SIST EN ISO 1133-1:2022 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN ISO 1133-1:2022
---------------------- Page: 2 ----------------------
SIST EN ISO 1133-1:2022
EN ISO 1133-1
EUROPEAN STANDARD
NORME EUROPÉENNE
July 2022
EUROPÄISCHE NORM
ICS 83.080.20 Supersedes EN ISO 1133-1:2011
English Version
Plastics - Determination of the melt mass-flow rate (MFR)
and melt volume-flow rate (MVR) of thermoplastics - Part
1: Standard method (ISO 1133-1:2022)

Plastiques - Détermination de l'indice de fluidité à Kunststoffe - Bestimmung der Schmelze-

chaud des thermoplastiques, en masse (MFR) et en Massefließrate (MFR) und der Schmelze-

volume (MVR) - Partie 1: Méthode normale (ISO 1133- Volumenfließrate (MVR) von Thermoplasten - Teil 1:

1:2022) Allgemeines Prüfverfahren (ISO 1133-1:2022)
This European Standard was approved by CEN on 25 June 2022.

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 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 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, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 1133-1:2022 E

worldwide for CEN national Members.
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SIST EN ISO 1133-1:2022
EN ISO 1133-1:2022 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

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SIST EN ISO 1133-1:2022
EN ISO 1133-1:2022 (E)
European foreword

This document (EN ISO 1133-1:2022) 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

identical text or by endorsement, at the latest by January 2023, and conflicting national standards shall

be withdrawn at the latest by January 2023.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN ISO 1133-1:2011.

Any feedback and questions on this document should be directed to the users’ national standards

body/national committee. A complete listing of these bodies can be found on the CEN website.

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, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,

Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of

North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the

United Kingdom.
Endorsement notice

The text of ISO 1133-1 has been approved by CEN as EN ISO 1133-1:2022 without any modification.

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SIST EN ISO 1133-1:2022
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SIST EN ISO 1133-1:2022
INTERNATIONAL ISO
STANDARD 1133-1
Second edition
2022-06
Plastics — Determination of the
melt mass-flow rate (MFR) and
melt volume-flow rate (MVR) of
thermoplastics —
Part 1:
Standard method
Plastiques — Détermination de l'indice de fluidité à chaud des
thermoplastiques, en masse (MFR) et en volume (MVR) —
Partie 1: Méthode normale
Reference number
ISO 1133-1:2022(E)
© ISO 2022
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SIST EN ISO 1133-1:2022
ISO 1133-1:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized 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 ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
© ISO 2022 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 1133-1:2022
ISO 1133-1:2022(E)
Contents Page

Foreword ..........................................................................................................................................................................................................................................v

Introduction .............................................................................................................................................................................................................................. vi

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ..................................................................................................................................................................................... 1

3 Terms and definitions .................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 2

5 Apparatus .................................................................................................................................................................................................................... 3

5.1 Extrusion plastometer ..................................................................................................................................................................... 3

5.2 Accessory equipment ........................................................................................................................................................................ 7

5.2.1 General ........................................................................................................................................................................................ 7

5.2.2 Equipment for procedure A (see Clause 8) .................................................................................................. 8

5.2.3 Equipment for procedure B (see Clause 9): Piston displacement transducer/

timer .............................................................................................................................................................................................. 8

6 Test sample ................................................................................................................................................................................................................ 8

6.1 Sample form .............................................................................................................................................................................................. 8

6.2 Conditioning.............................................................................................................................................................................................. 9

7 Temperature verification, cleaning and maintenance of the apparatus .................................................9

7.1 V erification of the temperature control system ....................................................................................................... 9

7.1.1 V erification procedure .................................................................................................................................................. 9

7.1.2 Material used during temperature verification .................................................................................. 10

7.2 Cleaning the apparatus ................................................................................................................................................................ 10

7.3 Vertical alignment of the instrument .............................................................................................................................. 10

8 Procedure A: mass-measurement method ............................................................................................................................10

8.1 Selection of temperature and load ..................................................................................................................................... 10

8.2 Cleaning ..................................................................................................................................................................................................... 11

8.3 Selection of sample mass and charging the cylinder ......................................................................................... 11

8.4 Measurements ........................................................................................................................................... ...........................................12

8.5 Expression of results ........................................................................................................................................... ...........................13

8.5.1 General .....................................................................................................................................................................................13

8.5.2 Expression of results: standard die ................................................................................................................ 13

8.5.3 Expression of results: half size die .................................................................................................................. 13

9 Procedure B: displacement-measurement method .....................................................................................................14

9.1 Selection of temperature and load ..................................................................................................................................... 14

9.2 Cleaning ..................................................................................................................................................................................................... 14

9.3 Minimum piston displacement distance ...................................................................................................................... 14

9.4 Selection of sample mass and charging the cylinder ......................................................................................... 14

9.5 Measurements ........................................................................................................................................... ........................................... 14

9.6 Expression of results ...................................................................................................................................................................... 15

9.6.1 General .....................................................................................................................................................................................15

9.6.2 Expression of results: standard die ................................................................................................................ 15

9.6.3 Expression of results: half size die .................................................................................................................. 16

10 Flow rate ratio .....................................................................................................................................................................................................16

11 Precision ....................................................................................................................................................................................................................17

12 Test report ...............................................................................................................................................................................................................17

Annex A (normative) Test conditions for MFR and MVR determinations .................................................................19

Annex B (informative) Conditions specified in International Standards for the

determination of the melt flow rate of thermoplastic materials ..................................................................21

iii
© ISO 2022 – All rights reserved
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SIST EN ISO 1133-1:2022
ISO 1133-1:2022(E)
Annex C (informative) Device and procedure for preforming a compacted charge of

material by compression ..........................................................................................................................................................................22

Annex D (informative) Precision data for polypropylene obtained from an intercomparison

of MFR and MVR testing ............................................................................................................................................................................25

Bibliography .............................................................................................................................................................................................................................26

© ISO 2022 – All rights reserved
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SIST EN ISO 1133-1:2022
ISO 1133-1:2022(E)
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 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 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, Part 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 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 received (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 of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to

the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see

www.iso.org/iso/foreword.html.

This document was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-

chemical properties, in collaboration with the European Committee for Standardization (CEN) Technical

Committee CEN/TC 249, Plastics, in accordance with the Agreement on technical cooperation between

ISO and CEN (Vienna Agreement).

This second edition cancels and replaces the first edition (ISO 1133-1:2011), of which it constitutes a

minor revision. The changes are as follows:

— references to withdrawn standards in Annex B (informative), Annex D (informative) and Bibliography

have been updated;
— editorial corrections.
A list of all parts in the ISO 1133 series can be found on the ISO website.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www.iso.org/members.html.
© ISO 2022 – All rights reserved
---------------------- Page: 11 ----------------------
SIST EN ISO 1133-1:2022
ISO 1133-1:2022(E)
Introduction

For stable materials that are not rheologically sensitive to the time-temperature history experienced

during melt flow rate testing, this document is recommended.

For materials whose rheological behaviour is sensitive to the test’s time-temperature history, e.g.

materials which degrade during the test, ISO 1133-2 is recommended. Also, ISO 1133-2 is considered to

be particularly relevant for moisture-sensitive plastics.

NOTE At the time of publication, there is no evidence to suggest that the use of ISO 1133-2 for stable materials

results in better precision in comparison with the use of this document.
© ISO 2022 – All rights reserved
---------------------- Page: 12 ----------------------
SIST EN ISO 1133-1:2022
INTERNATIONAL STANDARD ISO 1133-1:2022(E)
Plastics — Determination of the melt mass-flow rate (MFR)
and melt volume-flow rate (MVR) of thermoplastics —
Part 1:
Standard method

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 use. It is the responsibility of the user to establish appropriate safety and

health practices and to ensure compliance with any regulatory requirements.
1 Scope

This document specifies two procedures for the determination of the melt mass-flow rate (MFR) and

the 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

standard with a reference to this document. 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 measurements,

or vice versa, provided the melt density at the test temperature is known.

This document 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-linking, 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 document is not appropriate. In such cases, ISO 1133-2 applies.

NOTE The 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 quality control.

2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminology databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
© ISO 2022 – All rights reserved
---------------------- Page: 13 ----------------------
SIST EN ISO 1133-1:2022
ISO 1133-1:2022(E)
3.1
melt mass-flow rate
MFR

rate 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 plastometer, the rate

being determined as the mass extruded over a specified time

Note 1 to entry: MFR is expressed in units of grams per 10 min. Alternative units accepted by SI are decigrams

per minute, where 1 g/10 min is equivalent to 1 dg/min.
3.2
melt volume-flow rate
MVR

rate 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 plastometer, the rate

being determined as the volume extruded over a specified time
Note 1 to entry: MVR is expressed in units of cubic centimetres per 10 min.
3.3
load

combined force exerted by the mass of the piston and the added weight, or weights, as specified by the

conditions of the test
Note 1 to entry: Load is expressed as the mass, in kilograms, exerting it.
3.4
preformed compacted charge
test sample prepared as a compressed charge of polymer sample

Note 1 to entry: 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 example, powders or flakes into

a compacted charge.
3.5
time-temperature history

history of the temperature and time to which the sample is exposed during testing including sample

preparation
3.6
standard die
die having a nominal length of 8,000 mm and a nominal bore diameter of 2,095 mm
3.7
half size die
die having a nominal length of 4,000 mm and a nominal bore diameter of 1,050 mm
3.8
moisture-sensitive plastics

plastics having rheological properties that are sensitive to their moisture content

Note 1 to entry: Plastics which, when containing absorbed water and heated above their glass transition

temperatures (for amorphous plastics) or melting point (for semi-crystalline plastics), undergo hydrolysis

resulting in a reduction in molar mass and consequently a reduction in melt viscosity and an increase in MFR and

MVR.
4 Principle

The melt mass-flow rate (MFR) and the melt volume-flow rate (MVR) are determined by extruding

molten material from the cylinder of a plastometer through a die of specified length and diameter under

preset conditions of temperature and load.
© ISO 2022 – All rights reserved
---------------------- Page: 14 ----------------------
SIST EN ISO 1133-1:2022
ISO 1133-1:2022(E)

For measurement of MFR (procedure A), timed segments of the extrudate are weighed and used to

calculate the extrusion rate, in grams per 10 min.

For measurement of MVR (procedure B), the distance that the piston moves in a specified time or the

time required for the piston to move a specified distance is recorded and used to calculate the extrusion

rate in cubic centimetres per 10 min.

MVR can be converted to MFR, or vice versa, if the melt density of the material at the test temperature

is known.

NOTE The density of the melt is required at the test temperature and pressure. In practice, the pressure is

low and values obtained at the test temperature and ambient pressure suffice.
5 Apparatus
5.1 Extrusion plastometer

5.1.1 General. The basic apparatus comprises an extrusion plastometer operating at a fixed

temperature. The general design is as shown in Figure 1. The thermoplastic material, which is contained

in a vertical cylinder, is extruded through a die by a piston loaded with a known weight. The apparatus

consists of the following essential parts.

5.1.2 Cylinder. The cylinder shall have a length between 115 mm and 180 mm and an internal

diameter of (9,550 ± 0,007) mm and shall be fixed in a vertical position (see 5.1.6).

The cylinder shall be manufactured from a material resistant to wear and corrosion up to the maximum

temperature of the heating system. The bore shall be manufactured using techniques and materials

that produce a Vickers hardness of no less than 500 (HV 5 to HV 100) (see ISO 6507-1) and shall be

manufactured by a technique that produces a surface roughness of less than Ra (arithmetical mean

deviation) equal to 0,25 µm (see ISO 21920-2). The finish, properties and dimensions of its surface shall

not be affected by the material being tested.

NOTE 1 For particular materials, it is possible that measurements will be required at temperatures up to

450 °C.

The base of the cylinder shall be thermally insulated in such a way that the area of exposed metal is less

than 4 cm , and it is recommended that an insulating material such as Al O , ceramic fibre or another

2 3
suitable material be used in order to avoid sticking of the extrudate.

A piston guide or other suitable means of minimizing friction due to misalignment of the piston shall be

provided.

NOTE 2 Excessive wear of the piston head, piston and cylinder and erratic results can be indications of

misalignment of the piston. Regular visual checking for wear and change to the surface appearance of the piston

head, piston and cylinder is recommended.

5.1.3 Piston. The piston shall have a working length at least as long as the cylinder. The piston shall

have a head (6,35 ± 0,10) mm in length. The diameter of the head shall be (9,474 ± 0,007) mm. The lower

© ISO 2022 – All rights reserved
---------------------- Page: 15 ----------------------
SIST EN ISO 1133-1:2022
ISO 1133-1:2022(E)
00,

edge of the piston head shall have a radius of (04, ) mm and the upper edge shall have its sharp edge

−01,

removed. Above the head, the piston shall be relieved to ≤ 9,0 mm diameter (see Figure 2).

Key
1 insulation
2 removable weight
3 piston
4 upper reference mark
5 lower reference mark
6 cylinder
7 piston head
8 die
9 die retaining plate
10 insulating plate
11 insulation
12 temperature sensor

Figure 1 — Typical apparatus for determining melt flow rate, showing one possible

configuration

The piston shall be manufactured from a material resistant to wear and corrosion up to the maximum

temperature of the heating system, and its properties and dimensions shall not be affected by the

material being tested. To ensure satisfactory operation of the apparatus, the cylinder and the piston

head shall be made of materials of different hardness. It is convenient for ease of maintenance and

renewal to make the cylinder of the harder material.
© ISO 2022 – All rights reserved
---------------------- Page: 16 ----------------------
SIST EN ISO 1133-1:2022
ISO 1133-1:2022(E)

Along the piston stem, two thin annular reference marks shall be scribed (30 ± 0,2) mm apart and so

positioned that the upper mark is aligned with the top of the cylinder when the distance between the

lower edge of the piston head and the top of the standard die is 20 mm. These annular marks on the

piston are used as reference points during the measurements (see 8.4 and 9.5).

A stud may be added at the top of the piston to position and support the removable weights, but the

piston shall be thermally insulated from the weights.

The piston may be either hollow or solid. In tests with very low loads the piston may need to be hollow,

otherwise it may not be possible
...

SLOVENSKI STANDARD
oSIST prEN ISO 1133-1:2022
01-maj-2022
Polimerni materiali - Ugotavljanje masnega (MFR) in prostorninskega pretoka
taline (MVR) plastomerov - 1. del: Standardna metoda (ISO/FDIS 1133-1:2022)

Plastics - Determination of the melt mass-flow rate (MFR) and melt volume-flow rate

(MVR) of thermoplastics - Part 1: Standard method (ISO/FDIS 1133-1:2022)
Kunststoffe - Bestimmung der Schmelze-Massefließrate (MFR) und der Schmelze-
Volumenfließrate (MVR) von Thermoplasten - Teil 1: Allgemeines Prüfverfahren
(ISO/FDIS 1133-1:2022)

Plastiques - Détermination de l'indice de fluidité à chaud des thermoplastiques, en

masse (MFR) et en volume (MVR) - Partie 1: Méthode normale (ISO/FDIS 1133-1:2022)

Ta slovenski standard je istoveten z: prEN ISO 1133-1
ICS:
83.080.20 Plastomeri Thermoplastic materials
oSIST prEN ISO 1133-1:2022 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
oSIST prEN ISO 1133-1:2022
---------------------- Page: 2 ----------------------
oSIST prEN ISO 1133-1:2022
FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 1133-1
ISO/TC 61/SC 5
Plastics — Determination of the
Secretariat: DIN
melt mass-flow rate (MFR) and
Voting begins on:
2022-03-01 melt volume-flow rate (MVR) of
thermoplastics —
Voting terminates on:
2022-05-24
Part 1:
Standard method
Plastiques — Détermination de l'indice de fluidité à chaud des
thermoplastiques, en masse (MFR) et en volume (MVR) —
Partie 1: Méthode normale
ISO/CEN PARALLEL PROCESSING
RECIPIENTS OF THIS DRAFT ARE INVITED TO
SUBMIT, WITH THEIR COMMENTS, NOTIFICATION
OF ANY RELEVANT PATENT RIGHTS OF WHICH
THEY ARE AWARE AND TO PROVIDE SUPPOR TING
DOCUMENTATION.
IN ADDITION TO THEIR EVALUATION AS
Reference number
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ISO/FDIS 1133-1:2022(E)
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oSIST prEN ISO 1133-1:2022
ISO/FDIS 1133-1:2022(E)
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oSIST prEN ISO 1133-1:2022
ISO/FDIS 1133-1:2022(E)
Contents Page

Foreword ..........................................................................................................................................................................................................................................v

Introduction .............................................................................................................................................................................................................................. vi

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ..................................................................................................................................................................................... 1

3 Terms and definitions .................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 2

5 Apparatus .................................................................................................................................................................................................................... 3

5.1 Extrusion plastometer ..................................................................................................................................................................... 3

5.2 Accessory equipment ........................................................................................................................................................................ 7

5.2.1 General ........................................................................................................................................................................................ 7

5.2.2 Equipment for procedure A (see Clause 8) .................................................................................................. 8

5.2.3 Equipment for procedure B (see Clause 9): Piston displacement transducer/

timer .............................................................................................................................................................................................. 8

6 Test sample ................................................................................................................................................................................................................ 8

6.1 Sample form .............................................................................................................................................................................................. 8

6.2 Conditioning.............................................................................................................................................................................................. 9

7 Temperature verification, cleaning and maintenance of the apparatus .................................................9

7.1 V erification of the temperature control system ....................................................................................................... 9

7.1.1 V erification procedure .................................................................................................................................................. 9

7.1.2 Material used during temperature verification .................................................................................. 10

7.2 Cleaning the apparatus ................................................................................................................................................................ 10

7.3 Vertical alignment of the instrument .............................................................................................................................. 10

8 Procedure A: mass-measurement method ............................................................................................................................10

8.1 Selection of temperature and load ..................................................................................................................................... 10

8.2 Cleaning ..................................................................................................................................................................................................... 11

8.3 Selection of sample mass and charging the cylinder ......................................................................................... 11

8.4 Measurements ........................................................................................................................................... ...........................................12

8.5 Expression of results ........................................................................................................................................... ...........................13

8.5.1 General .....................................................................................................................................................................................13

8.5.2 Expression of results: standard die ................................................................................................................ 13

8.5.3 Expression of results: half size die .................................................................................................................. 13

9 Procedure B: displacement-measurement method .....................................................................................................14

9.1 Selection of temperature and load ..................................................................................................................................... 14

9.2 Cleaning ..................................................................................................................................................................................................... 14

9.3 Minimum piston displacement distance ...................................................................................................................... 14

9.4 Selection of sample mass and charging the cylinder ......................................................................................... 14

9.5 Measurements ........................................................................................................................................... ........................................... 14

9.6 Expression of results ...................................................................................................................................................................... 15

9.6.1 General .....................................................................................................................................................................................15

9.6.2 Expression of results: standard die ................................................................................................................ 15

9.6.3 Expression of results: half size die .................................................................................................................. 16

10 Flow rate ratio .....................................................................................................................................................................................................16

11 Precision ....................................................................................................................................................................................................................17

12 Test report ...............................................................................................................................................................................................................17

Annex A (normative) Test conditions for MFR and MVR determinations .................................................................19

Annex B (informative) Conditions specified in International Standards for the

determination of the melt flow rate of thermoplastic materials ..................................................................21

iii
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oSIST prEN ISO 1133-1:2022
ISO/FDIS 1133-1:2022(E)
Annex C (informative) Device and procedure for preforming a compacted charge of

material by compression ..........................................................................................................................................................................22

Annex D (informative) Precision data for polypropylene obtained from an intercomparison

of MFR and MVR testing ............................................................................................................................................................................25

Bibliography .............................................................................................................................................................................................................................26

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oSIST prEN ISO 1133-1:2022
ISO/FDIS 1133-1:2022(E)
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 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 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, Part 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 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 received (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 of the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to

the World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT), see

www.iso.org/iso/foreword.html.

This document was prepared by Technical Committee ISO/TC 61, Plastics, Subcommittee SC 5, Physical-

chemical properties, in collaboration with the European Committee for Standardization (CEN) Technical

Committee CEN/TC 249, Plastics, in accordance with the Agreement on technical cooperation between

ISO and CEN (Vienna Agreement).

This second edition cancels and replaces the first edition (ISO 1133-1:2011), of which it constitutes a

minor revision. The changes are as follows:

— references to withdrawn standards in Annex B (informative), Annex D (informative) and Bibliography

have been updated;
— editorial corrections.
A list of all parts in the ISO 1133 series can be found on the ISO website.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www.iso.org/members.html.
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oSIST prEN ISO 1133-1:2022
ISO/FDIS 1133-1:2022(E)
Introduction

For stable materials that are not rheologically sensitive to the time-temperature history experienced

during melt flow rate testing, this document is recommended.

For materials whose rheological behaviour is sensitive to the test’s time-temperature history, e.g.

materials which degrade during the test, ISO 1133-2 is recommended. Also, ISO 1133-2 is considered to

be particularly relevant for moisture-sensitive plastics.

NOTE At the time of publication, there is no evidence to suggest that the use of ISO 1133-2 for stable materials

results in better precision in comparison with the use of this document.
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oSIST prEN ISO 1133-1:2022
FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 1133-1:2022(E)
Plastics — Determination of the melt mass-flow rate (MFR)
and melt volume-flow rate (MVR) of thermoplastics —
Part 1:
Standard method

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 use. It is the responsibility of the user to establish appropriate safety and

health practices and to ensure compliance with any regulatory requirements.
1 Scope

This document specifies two procedures for the determination of the melt mass-flow rate (MFR) and

the 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

standard with a reference to this document. 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 measurements,

or vice versa, provided the melt density at the test temperature is known.

This document 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-linking, 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 document is not appropriate. In such cases, ISO 1133-2 applies.

NOTE The 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 quality control.

2 Normative references
There are no normative references in this document.
3 Terms and definitions
For the purposes of this document, the following terms and definitions apply.

ISO and IEC maintain terminology databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
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oSIST prEN ISO 1133-1:2022
ISO/FDIS 1133-1:2022(E)
3.1
melt mass-flow rate
MFR

rate 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 plastometer, the rate

being determined as the mass extruded over a specified time

Note 1 to entry: MFR is expressed in units of grams per 10 min. Alternative units accepted by SI are decigrams

per minute, where 1 g/10 min is equivalent to 1 dg/min.
3.2
melt volume-flow rate
MVR

rate 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 plastometer, the rate

being determined as the volume extruded over a specified time
Note 1 to entry: MVR is expressed in units of cubic centimetres per 10 min.
3.3
load

combined force exerted by the mass of the piston and the added weight, or weights, as specified by the

conditions of the test
Note 1 to entry: Load is expressed as the mass, in kilograms, exerting it.
3.4
preformed compacted charge
test sample prepared as a compressed charge of polymer sample

Note 1 to entry: 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 example, powders or flakes into

a compacted charge.
3.5
time-temperature history

history of the temperature and time to which the sample is exposed during testing including sample

preparation
3.6
standard die
die having a nominal length of 8,000 mm and a nominal bore diameter of 2,095 mm
3.7
half size die
die having a nominal length of 4,000 mm and a nominal bore diameter of 1,050 mm
3.8
moisture-sensitive plastics

plastics having rheological properties that are sensitive to their moisture content

Note 1 to entry: Plastics which, when containing absorbed water and heated above their glass transition

temperatures (for amorphous plastics) or melting point (for semi-crystalline plastics), undergo hydrolysis

resulting in a reduction in molar mass and consequently a reduction in melt viscosity and an increase in MFR and

MVR.
4 Principle

The melt mass-flow rate (MFR) and the melt volume-flow rate (MVR) are determined by extruding

molten material from the cylinder of a plastometer through a die of specified length and diameter under

preset conditions of temperature and load.
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oSIST prEN ISO 1133-1:2022
ISO/FDIS 1133-1:2022(E)

For measurement of MFR (procedure A), timed segments of the extrudate are weighed and used to

calculate the extrusion rate, in grams per 10 min.

For measurement of MVR (procedure B), the distance that the piston moves in a specified time or the

time required for the piston to move a specified distance is recorded and used to calculate the extrusion

rate in cubic centimetres per 10 min.

MVR can be converted to MFR, or vice versa, if the melt density of the material at the test temperature

is known.

NOTE The density of the melt is required at the test temperature and pressure. In practice, the pressure is

low and values obtained at the test temperature and ambient pressure suffice.
5 Apparatus
5.1 Extrusion plastometer

5.1.1 General. The basic apparatus comprises an extrusion plastometer operating at a fixed

temperature. The general design is as shown in Figure 1. The thermoplastic material, which is contained

in a vertical cylinder, is extruded through a die by a piston loaded with a known weight. The apparatus

consists of the following essential parts.

5.1.2 Cylinder. The cylinder shall have a length between 115 mm and 180 mm and an internal

diameter of (9,550 ± 0,007) mm and shall be fixed in a vertical position (see 5.1.6).

The cylinder shall be manufactured from a material resistant to wear and corrosion up to the maximum

temperature of the heating system. The bore shall be manufactured using techniques and materials

that produce a Vickers hardness of no less than 500 (HV 5 to HV 100) (see ISO 6507-1) and shall be

manufactured by a technique that produces a surface roughness of less than Ra (arithmetical mean

deviation) equal to 0,25 µm (see ISO 4287). The finish, properties and dimensions of its surface shall

not be affected by the material being tested.

NOTE 1 For particular materials, it is possible that measurements will be required at temperatures up to

450 °C.

The base of the cylinder shall be thermally insulated in such a way that the area of exposed metal is less

than 4 cm , and it is recommended that an insulating material such as Al O , ceramic fibre or another

2 3
suitable material be used in order to avoid sticking of the extrudate.

A piston guide or other suitable means of minimizing friction due to misalignment of the piston shall be

provided.

NOTE 2 Excessive wear of the piston head, piston and cylinder and erratic results can be indications of

misalignment of the piston. Regular visual checking for wear and change to the surface appearance of the piston

head, piston and cylinder is recommended.

5.1.3 Piston. The piston shall have a working length at least as long as the cylinder. The piston shall

have a head (6,35 ± 0,10) mm in length. The diameter of the head shall be (9,474 ± 0,007) mm. The lower

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oSIST prEN ISO 1133-1:2022
ISO/FDIS 1133-1:2022(E)
00,

edge of the piston head shall have a radius of (04, ) mm and the upper edge shall have its sharp edge

−01,

removed. Above the head, the piston shall be relieved to ≤ 9,0 mm diameter (see Figure 2).

Key
1 insulation
2 removable weight
3 piston
4 upper reference mark
5 lower reference mark
6 cylinder
7 piston head
8 die
9 die retaining plate
10 insulating plate
11 insulation
12 temperature sensor

Figure 1 — Typical apparatus for determining melt flow rate, showing one possible

configuration

The piston shall be manufactured from a material resistant to wear and corrosion up to the maximum

temperature of the heating system, and its properties and dimensions shall not be affected by the

material being tested. To ensure satisfactory operation of the apparatus, the cylinder and the piston

head shall be made of materials of different hardness. It is convenient for ease of maintenance and

renewal to make the cylinder of the harder material.
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oSIST prEN ISO 1133-1:2022
ISO/FDIS 1133-1:2022(E)

Along the piston stem, two thin annular reference marks shall be scribed (30 ± 0,2) mm apart and so

positioned that the upper mark is aligned with the top of the cylinder when the distance between the

lower edge of the piston head and the top of the standard die is 20 mm. These annular marks on the

piston are used as reference points during the measurements (see 8.4 and 9.5).

A stud may be added at the top of the piston to position and support the removable weights, but the

piston shall be thermally insulated from the weights.

The piston may be either hollow or solid. In tests with very low loads the piston may need to be hollow,

otherwise it may not be possible to obtain the lowest prescribed load.
Table 1 — Dimensions of piston head
Dimensions in millimetres
Length of head, A 6,35 ± 0,10
Diameter of head, B 9,474 ± 0,007
Diameter of stem, C ≤ 9,0
00,
Radius of lower edge, R
04,
−01,
Key
A length of head
B diameter of head
C diameter of stem
R radius of lower edge
Sharp edge removed.
Figure 2 — Schematic of piston head

5.1.4 Temperature-control system. For all cylinder temperatures that can be set, the temperature

control shall be such that between (10 ± 1) mm and (70 ± 1) mm above the top of the standard die, the

temperature differences measured do not exceed those given in Table 2 throughout the duration of the

test.

NOTE The temperature can be measured and controlled with, for example, thermocouples or platinum-

resistance sensors embedded in the wall of the cylinder. If the apparatus is equipped in this way, it is possible that

the temperature is not exactly the same as that in the melt, but the temperature-control system can be calibrated

(see 7.1) to read the in-melt temperature.

The temperature-control system shall allow the test temperature to be set in steps of 0,1 °C or less.

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oSIST prEN ISO 1133-1:2022
ISO/FDIS 1133-1:2022(E)

Table 2 — Maximum allowable deviation from required test temperature with distance and

with time over the duration of the test
Temperatures in degrees Celsius
Maximum permitted deviation from the required test temperature:
Test temperature
at (10 ± 1) mm above the top surface of from (10 ± 1) mm to (70 ± 1) mm above
b b
the standard die the top surface of the standard die
125 ≤ T < 250 ±1,0 ±2,0
250 ≤ T < 300 ±1,0 ±2,5
300 ≤ T ±1,0 ±3,0

The maximum permitted deviation from the required test temperature is the difference between the true value of

temperature and the required test temperature. It shall be assessed over the normal duration of a test, typically less than

25 min.

When using a 4 mm length half size die (see 5.1.5), the readings shall be made an additional 4 mm above the top surface

of the die.

For test temperatures < 300 °C, the temperature at 10 mm above the top surface of the die shall not vary with time by

greater than 1 °C in range.

5.1.5 Die. The die shall be made of tungsten carbide or hardened steel. For testing potentially

corrosive materials, dies made of cobalt-chromium-tungsten alloy, chromalloy, synthetic sapphire or

other suitable materials may be used.

The die shall be (8,000 ± 0,025) mm in length. The interior of the bore shall be manufactured circular,

straight and uniform in diameter such that in all positions it is within ± 0,005 mm of a true cylinder of

diameter 2,095 mm.

The bore shall be hardened by a technique that produces a Vickers hardness of no less than 500 (HV 5 to

HV 100) (see ISO 6507-1) and shall be manufactured by a technique that produces a surface roughness

of less than Ra (arithmetical mean deviation) = 0,25 µm (see ISO 4287).

The bore diameter shall be checked regularly with a go/no-go gauge. If outside the tolerance limits, the

die shall be discarded. If the no-go gauge enters the bore to any extent the die shall be discarded.

The die shall have ends that are flat, perpendicular to the axis of the bore and free from visible

machining marks. The flat surfaces of the die shall be checked to ensure that the area around the bore

is not chipped. Any chipping causes errors and chipped dies shall be discarded.
The die shall have an outside diameter such tha
...

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