EN ISO 1133-1:2022
(Main)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)
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)
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.
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 Werkstoffen 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 einer Verweisung 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 möglicherweise 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)
Ta dokument določa dva postopka za ugotavljanje masnega (MFR) in prostorninskega (MVR) pretoka taline plastomerov pod določenimi pogoji temperature ter obremenitve. Postopek A je metoda za merjenje mase. Postopek B je metoda za merjenje premika. Običajno so preskusni pogoji za merjenje pretoka taline določeni v standardu za material s sklicevanjem na ta dokument. Preskusni pogoji, ki se običajno uporabljajo za plastomere, so navedeni v dodatku A. Prostorninski pretok taline je zlasti uporaben pri primerjavi materialov z različno vsebnostjo polnila in primerjavi polnjenih plastomerov z nepolnjenimi. Masni pretok taline je mogoče ugotoviti z meritvami prostorninskega pretoka taline ali obratno, če je gostota taline pri preskusni temperaturi znana. Ta dokument je morda mogoče uporabiti tudi za plastomere, pri katerih se reološko obnašanje med merjenjem spremeni zaradi pojavov, kot so hidroliza (cepljenje verig), kondenzacija in prečno povezovanje, vendar le, če je obseg učinka omejen ter sta ponovljivost in obnovljivost v okviru sprejemljivih vrednosti. Za materiale z bistveno spremenjenim reološkim obnašanjem med preskušanjem ta dokument ni primeren. V takih primerih se uporablja standard ISO 1133-2. OPOMBA: Strižne hitrosti pri teh metodah so veliko manjše od tistih, ki se uporabljajo v običajnih pogojih predelave, zato je mogoče, da se podatki, pridobljeni za različne plastomere s tema metodama, ne bodo vedno ujemali z njihovim obnašanjem med predelavo. Obe metodi se primarno uporabljata pri preverjanju kakovosti.
General Information
Relations
Standards Content (Sample)
SLOVENSKI STANDARD
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
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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.
Contents Page
European foreword . 3
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.
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 1133-1:2022(E)
© 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
ii
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 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
iv
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.
v
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.
vi
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 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 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 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 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
a
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.
ISO 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
a
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
T
c
125 ≤ T < 250 ±1,0 ±2,0
c
250 ≤ T < 300 ±1,0 ±2,5
300 ≤ T ±1,0 ±3,0
a
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.
b
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.
c
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 21920-2).
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 that it moves freely within the cylinder, but that there is no
flow of material along its outside, i.e. between the die and the cylinder, during the test.
The die shall not project beyond the base of the cylinder (see Figure 1) and shall be mounted so that its
bore is co-axial with the cylinder bore.
If testing materials with an MFR > 75 g/10 min or an MVR > 75 cm /10 min, a half size die of length
(4,000 ± 0,025) mm and bore diameter (1,050 ± 0,005) mm may be used. No spacer shall be used in the
cylinder below this die to increase the apparent length to 8,000 mm.
The die of nominal length 8,000 mm and bore of nominal internal diameter 2,095 mm is taken to be the
standard die for use in testing. When reporting MFR and MVR values obtained using a half size die, it
shall be stated that a half size die was used.
5.1.6 Means of setting and maintaining the cylinder vertical. A two-directional bubble level, set
normal to the cylinder axis, and adjustable supports for the apparatus are suitable for the purpose.
NOTE This is to avoid excessive friction caused by the piston leaning to one side or bending under heavy
loads. A dummy piston with a spirit level on its upper end is also a suitable means of checking conformity with
this requirement.
ISO 1133-1:2022(E)
5.1.7 Load. A set of removable weights, selected so that the combined mass of the weights and the
piston gives the required load to within a maximum permissible error of ±0,5 %, are mounted on top of
the piston.
Alternatively, a mechanical loading device combined with a load cell or a pneumatic loading device with
a pressure sensor, providing the same level of accuracy as the removable weights, may be used.
5.2 Accessory equipment
5.2.1 General
5.2.1.1 Packing rod, made of non-abrasive material, for introducing test samples into the cylinder.
5.2.1.2 Cleaning equipment (see 7.2).
5.2.1.3 Go/no-go gauge, one end having a pin with a diameter equal to that of the die bore minus the
allowed tolerance (go gauge) and the opposite end having a pin with a diameter equal to that of the die
bore plus the allowed tolerance (no-go gauge). The pin gauge shall be sufficiently long to check the full
length of the die using the go gauge.
5.2.1.4 Temperature-calibration device (thermocouple, platinum-resistance thermometer or other
temperature-measuring device) for calibration of the cylinder temperature-indicating device.
A light-gauge probe-type temperature-measuring device that has a short sensing length and which is
calibrated at the temperatures and immersion lengths that are to be used when calibrating the cylinder
temperature may be used. The length of the temperature calibration device shall be sufficient to
measure the temperature at (10 ± 1) mm from the top of the die. The temperature calibration device
shall have sufficient accuracy and precision to enable verification of the MVR/MFR instrument to within
the maximum permissible errors in temperature as specified in Table 2. When used, the thermocouple
should be encased in a metallic sheath having a diameter of approximately 1,6 mm with its hot junction
grounded to the end of the sheath.
An alternative technique for verification is to use a sheathed thermocouple or platinum-resistance
temperature sensor inserted into a bronze tip with a diameter of (9,4 ± 0,1) mm for insertion in the bore
without material present. The tip shall be designed so that it holds the sensing point of the thermocouple
or platinum-resistance temperature sensor (10 ± 1) mm from the top surface of the standard die when
it rests directly on top of the die.
A further alternative is to use a rod fitted with thermocouples that would allow it to be used to make
simultaneous temperature determinations at (70 ± 1) mm, (50 ± 1) mm, (30 ± 1) mm and (10 ± 1) mm
above the top of the standard die. The rod shall be (9,4 ± 0,1) mm in diameter so that it fits tightly in the
bore.
5.2.1.5 Die plug. A device shaped at one end so that it effectively blocks the die exit and prevents
drool of molten material while allowing rapid removal prior to initiation of the test.
5.2.1.6 Piston/weight support, of sufficient length to hold the piston, and weights as necessary, so
that the lower reference mark is 25 mm above the top of the cylinder.
5.2.1.7 Preforming device. A device for preforming samples, e.g. powders, flakes, film strips or
fragments, into a compacted charge, thereby allowing quick introduction of the charge into the cylinder
and to ensure void-free filling of the cylinder (see Annex C).
NOTE It is possible that there are other options to achieve void-free filling of the cylinder.
ISO 1133-1:2022(E)
5.2.2 Equipment for procedure A (see Clause 8)
5.2.2.1 Cutting tool, for cutting the extruded sample.
NOTE A sharp-edge spatula or a rotating cutter blade with either manual operation or motor drive has been
found to be suitable.
5.2.2.2 Timer, with sufficient accuracy to enable cutting of the extruded samples with a maximum
permissible error of ±1 % of the cut-off time interval used. For verification, compare the cut-off time
intervals with a calibrated timing device over different time intervals of up to 240 s.
NOTE MFRs < 5 g/10 min can be measured with the maximum allowed cutting time interval of 240 s. In
this case, the maximum permissible error for the cutting time is ±2,4 s. Shorter intervals are allowed, but lead to
smaller maximum permissible errors. MFRs > 10 g/10 min require cutting times in the order of a few seconds or
less. For 1 s, the required maximum permissible error of the cutting time is ±0,01 s or better. Automatic cutters
are recommended for MFR values greater than 10 g/10 min.
Where the timing device makes physical contact with the piston or weight, the load shall not be altered
by more than ±0,5 % of the nominal load.
5.2.2.3 Balance, with a maximum permissible error of ±1 mg or better.
5.2.3 Equipment for procedure B (see Clause 9): Piston displacement transducer/timer
This equipment measures distance and time for the piston movement, using single or multiple
determinations for a single charge (see Table 3).
Table 3 — Piston distance and time measurement accuracy requirements
MFR (g/10 min) Distance Time
3 a
MVR (cm /10 min)
mm s
0,1 to 1,0 ±0,02 ±0,1
> 1,0 to 100 ±0,1 ±0,1
> 100 ±0,1 ±0,01
a
For multiple measurements using a single charge regardless of the MFR or MVR of the material, the requirements shall
be the same as for MFR > 100 g/10 min or MVR > 100 cm /10 min.
NOTE Compliance with distance accuracy requirements for MFR ≤ 1 g/10 min and MVR ≤ 1 cm /10 min also
ensures compliance for MFR > 1 g/10 min and MVR > 1 cm /10 min.
Where the displacement measurement device makes physical contact with the piston or weight, the
load shall not be altered by more than ±0,5 % of the nominal load.
Where the timing device makes physical contact with the piston or weight, the load shall not be altered
by more than ±0,5 % of the nominal load.
6 Test sample
6.1 Sample form
The test sample may be in any form that can be introduced into the bore of the cylinder, e.g. granules,
strips of film, powder or sections of moulded or extruded parts.
NOTE In order to ensure void-free extrudates when testing powders, it can prove necessary to first
compress the material into a preform or pellets. Annex C provides further information on a preparation method
for a preformed compacted charge.
ISO 1133-1:2022(E)
The form of the test sample can be a significant factor in determining the reproducibility of results. The
form of the test sample should therefore be controlled to improve the comparability of inter-laboratory
results and to reduce the variability between runs.
6.2 Conditioning
The test sample shall be conditioned and, if considered necessary, stabilized prior to testing in
accordance with the appropriate material standard.
7 Temperature verification, cleaning and maintenance of the apparatus
7.1 V erification of the temperature control system
7.1.1 Verification procedure
It is necessary to verify regularly the performance of the temperature-control system (5.1.4). Verify
that the temperature over time as well as distance conforms to the requirements stated in Table 2, and
that the pre-heat time (8.3) is sufficient to obtain stabilization.
Set the temperature-control system on the MFR/MVR instrument to the required temperature and
allow it to stabilize for not less than 15 min.
It is preferable to preheat the calibrated temperature-indicating device to the same temperature as that
being measured prior to its insertion into the cylinder.
If the cylinder temperature is to be verified using material in the cylinder, charge the cylinder within a
period of 15 s up to at least 100 mm above the top of the standard die with the material to be tested or a
material representative thereof (see 7.1.2), using the same technique as for a test (see 8.3).
Within 90 s after completing the charging of the material, introduce the calibrated temperature-
indicating device (5.2.1.4) along the wall into the cylinder, immersing it in the material therein until
the sensor is (10 ± 1) mm above the top surface of the standard die. Immediately, start recording the
temperature indicated by the calibrated temperature-indicating device. Determine the time taken from
completion of charging until the temperature has stabilized to within the temperature limits specified
in Table 2 for (10 ± 1) mm above the top surface of the standard die. This time period shall not be
greater than 5 min.
The temperature profile along the cylinder shall be verified similarly. For this, measure the
temperatures of the material also at (30 ± 1) mm, (50 ± 1) mm and (70 ± 1) mm above the top surface
of the standard die. Determine the time taken from completion of charging until the temperature has
stabilized to within the temperature limits specified in Table 2 for between (10 ± 1) mm to (70 ± 1) mm
above the top surface of the standard die. This time period shall not be greater than 5 min.
If the time to reach temperature stabilization to within the temperature limits specified in Table 2 is
longer than 5 min at any of the set distances above the top surface of the die, this shall be recorded in
the test report under item f) “pre-heating time”.
It is recommended that when verifying the temperature profile along the cylinder, the measurements
are started at the highest point above the die.
An alternative technique for verification of the temperature accuracy to within the specification of
Table 2 is to use a sheathed thermocouple or platinum-resistance temperature sensor with tip diameter
of (9,4 ± 0,1) mm for insertion in the cylinder without material present. Another technique is to use a
piston fitted with thermocouples at heights of (70 ± 1) mm, (50 ± 1) mm, (30 ± 1) mm and (10 ± 1) mm
above the top surface of the standard die when inserted completely into the cylinder and which fits the
bore closely. This configuration allows simultaneous verification of the temperature with
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.
Loading comments...