SIST EN ISO 3146:2000

SLOVENSKI STANDARD
SIST EN ISO 3146:2000
01-december-2000
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Plastics - Determination of melting behaviour (melting temperature or melting range) of
semi-crystalline polymers by capillary tube and polarizing-microscope methods (ISO
3146:2000)
Kunststoffe - Bestimmung des Schmelzverhaltens

(Schmelztemperatur oder Schmelzbereich) von teilkristallinen

Polymeren im Kapillarrohr- und Polarisationsmikroskop-Verfahren

(ISO 3146:2000)
Plastiques - Détermination du comportement a la fusion (température de fusion ou plage
de températures de fusion) des polymeres semi-cristallins par méthodes du tube
capillaire et du microscope polarisant (ISO 3146:2000)
Ta slovenski standard je istoveten z: EN ISO 3146:2000
ICS:
83.080.10 Duromeri Thermosetting materials
SIST EN ISO 3146:2000 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 3146:2000

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SIST EN ISO 3146:2000
EUROPEAN STANDARD
EN ISO 3146
NORME EUROPÉENNE
EUROPÄISCHE NORM
June 2000
ICS 83.080.10 Supersedes EN ISO 3146:1997
English version
Plastics - Determination of melting behaviour (melting
temperature or melting range) of semi-crystalline polymers by
capillary tube and polarizing-microscope methods (ISO
3146:2000)
Plastiques - Détermination du comportement à la fusion Kunststoffe - Bestimmung des Schmelzverhaltens
(température de fusion ou plage de températures de (Schmelztemperatur oder Schmelzbereich) von
fusion) des polymères semi-cristallins par méthodes du teilkristallinen Polymeren im Kapillarrohr- und
tube capillaire et du microscope polarisant (ISO 3146:2000) Polarisationsmikroskop-Verfahren (ISO 3146:2000)
This European Standard was approved by CEN on 9 April 2000.
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 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 Management Centre has the same status as the official
versions.
CEN members are the national standards bodies of Austria, Belgium, Czech Republic, Denmark, Finland, France, Germany, Greece,
Iceland, Ireland, Italy, Luxembourg, Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
Management Centre: rue de Stassart, 36  B-1050 Brussels
© 2000 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 3146:2000 E
worldwide for CEN national Members.

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SIST EN ISO 3146:2000
Page 2
EN ISO 3146:2000
CORRECTED  2002-03-13
Foreword
This document (ISO 3146:2000) 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 IBN.
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 December 2000, and conflicting national
standards shall be withdrawn at the latest by December 2000.
This document supersedes EN ISO 3146:1997.
According to the CEN/CENELEC Internal Regulations, the national standards organizations of
the following countries are bound to implement this European Standard: Austria, Belgium, Czech
Republic, Denmark, Finland, France, Germany, Greece, Iceland, Ireland, Italy, Luxembourg,
Netherlands, Norway, Portugal, Spain, Sweden, Switzerland and the United Kingdom.
Endorsement notice
The text of the International Standard ISO 3146:2000 has been approved by CEN as a
European Standard without any modifications.
NOTE Normative references to International Standards are listed in annex ZA (normative).

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SIST EN ISO 3146:2000
Page 3
EN ISO 3146:2000
Annex ZA
(normative)
Normative references to international publications
with their relevant European publications
This European Standard incorporates by dated or undated reference, provisions from other
publications. These normative references are cited at the appropriate places in the text and the
publications are listed hereafter. For dated references, subsequent amendments to or revisions of
any of these publications apply to this European Standard only when incorporated in it by
amendment or revision. For undated references the latest edition of the publication referred to
applies (including amendments).
NOTE Where an International Publication has been modified by common modifications, indicated
by (mod.), the relevant EN/HD applies.
Publication Year Title EN Year
ISO 291 1997 Plastics - Standard atmospheres for EN ISO 291 1997
conditioning and testing

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SIST EN ISO 3146:2000

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SIST EN ISO 3146:2000
International Standard
INTERNATIONAL ORGANIZATION FOR STANDARDIZATION@MEIK,QYHAPOI1HAF OPrAHM3AUMR fl0 CTAHfiAPTM3AL(MM.ORGANISATION INTERNATIONALE DE NORMALISATION
Plastics - Determination of melting behaviour (melting
temperature or melting range) of semi-crystalline
polymers
Plas tiques - Dhrmination du comportement 5 Ia fusion ftempba ture de fusion ou plage de tempkrature de fusion) des polym&res
semi- cris tallins
Second edition - 1985-12-15
UDC 678.7 : 620.1 : 536.421.1 Ref n No. ISO 31464985 (E)
Descriptors : plastics, polymers, tests, determination, melting Points, test equipment.
Price based on IO pages

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SIST EN ISO 3146:2000
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. Esch 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, govern-
mental and non-governmental, in liaison with ISO, also take patt in the work.
Draft International Standards adopted by the technical committees are circulated to
the member bodies for approval before their acceptance as International Standards by
the ISO Council. They are approved in accordance with ISO procedures requiring at
least 75 % approval by the member bodies voting.
International Standard ISO 3146 was prepared by Technical Committee ISO/TC 61,
Hastics.
This second edition cancels and replaces the first edition (ISO 3146-19741, of which it
constitutes a minor revision.
Users should note that all International Standards undergo revision from time to time
and that any reference made herein to any other International Standard implies its
latest edition, unless otherwise stated.
0 International Organization for Standardization, 1985
Printed in Switzerland

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SIST EN ISO 3146:2000
INTERNATIONAL STANDARD
ISO 31464985 (E)
Plastics - Determination of melting behaviour (melting
temperature or melting range) of semi-crystalline
polymers
This method is applicable to Polymers containing a birefringent
0 Introduction
crystalline Phase; it may not be suitable for plastics compounds
containing Pigments and/or other additives which could
The melting behaviour of a crystalline or partly crystalline
interfere with the birefringence of the polymeric crystalline
polymer is a structure-sensitive property.
Zone.
In Polymers a sharp melting Point, such as is observed for low
Section three specifies a thermal analytical method
molecular mass substances, usually does not occur; instead a
(method C), h aving two variants :
melting temperature range is observed on heating, from the
first Change of shape of the solid particles to the transformation
-
method Cl, which uses Differential Thermal Analysis
into a highly viscous or viscoelastic liquid, with accompanying
(DTA) ;
disappearance of the crystalline Phase, if present. The melting
-
range depends upon a number of Parameters, such as
method C2, which uses Differential Scanning
molecular mass, molecular mass distribution, per cent
Calorimetry (DSC).
crystallinity, and thermodynamic properties.
Both are applicable to all Polymers containing a crystalline
Phase and their compounds.
lt may also depend on the previous thermal history of the
specimens. The lower or upper limit of the melting range, or its
The melting temperatures determined by the different methods
average value, is sometimes conventionally referred to as the
usually differ by several kelvins for the reasons explained in the
“melting temperature”.
lntroduction.
Of the methods given above, experiments have indicated DSC
(Differential Scanning Calorimetry) to be the method of choice
1 Scope and field of application
as having the best reproducibility of results.
This International Standard specifies three methods for
evaluating the melting behaviour of semi-crystalline Polymers.
2 Definitions
Section one specifies a capillary tube method (method A),
2.1 semi-crystalline Polymers : Polymers containing a
which is based on the changes in shape of the polymer. This
crystalline Phase surrounded by amorphous materials.
method is applicable to all Polymers and their compounds, even
if there is no crystalline Phase.
22 melting range : The temperature range over which
ciystalline Polymers lose their crystallinity when heated.
Section two specifies a polarizing microscope method
(method B), which is based on changes in the Optical proper-
NOTE - The conventional “melting temperatures” determined by
methods A and B are defined in clauses 3 and 8.
ties of the polymer.
1

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SIST EN ISO 3146:2000
ISO 3146-1985 (EI
Section one : Method A - Capillary tube
3 Principle c) heating System for the metal block a) provided, for
example, by an electrical resistance enclosed in the block;
Heating of a specimen, at a controlled rate, and Observation for
d) rheostat for regulation of the power input, if electrical
Change In shape.
heating is used;
Reporting of men at the first visible
the temperature of the speci
e) four windows of heat-resistant glass on the lateral Walls
deformation as the melting temperature.
of the chamber, diametrically disposed at right angles to
each other. In front of one of these windows is mounted an
NOTE - This method may also be used for non-crystalline materials
eyepiece for observing the capillary tube. The other three
according to the relevant specifications or by agreement between the
windows are used for illuminating the inside of the
interested Parties.
enclosure by means of lamps.
NOTE - Other suita ble melting apparatuses may be used,
provided
that they give the same results.
4 Apparatus (sec figure 1)
4.2 Capillary tube, of heat-resistant glass, closed at one
41 . Melting apparatus, consisting of the following items :
end.
a) cylindrical metal block, the upper part of which is
NOTE - The maximum extemal diameter should preferably be
hollow and forms a chamber;
1,5 mm.
b) metal plug, with two or more holes, allowing a ther-
4.3 Calibrated thermometer, graduated in divisions of 1 K.
mometer and one or more capillary tubes to be mounted
The thermometer probe shall be positioned in such a way that
into the metal block a);
heat dispersion in the apparatus is not impeded.
Thermometer
I resistance
Metal heatir
Figure 1 - Apparatus for method A

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SIST EN ISO 3146:2000
ISO 3146-1985 (EI
- Calibration Standards
Other suitable temperature-measuring devices may be used. Table 1
NOTE -
Melting
Chemical
temperaturel) (OC)
L-Menthol-l 42,5
5 Test specimens
Azobenzene 69,0
8-Hydroxyquinoline 75,5
The specimens used shall be representative of the Sample of
Naphthalene 80,2
material to be tested. Benzyl
96,0
Acetanilide 113,5
Benzoic acid
121,7
5.1 Characteristics
136,0
Phenacetin [N (4-ethoxyphenyl) acetamidel
Adipic acid 151,5
Powder of particle size up to 100 Fm or tut pieces of films of
Indium 156,4
thickness 10 to 20 pm should preferably be used. Comparison
Sulfanilamide 165,7
tests shall be carried out on specimens of the same or similar
Hydroquinone 170,3
particle size, or similar thickness in the case of layers or films.
Succinic acid
189,5
208,o
2-Chloroanthraquinone
5.2 Conditioning
Anthracene 217,0
Saccharin
229,4
If not otherwise specified or agreed to by the interested Parties,
Tin 231,9
the Sample shall be conditioned at 23 + 2 OC and relative
Tin( II) chloride 247,0
humidity of 50 + 5 % for 3 h Prior to the measurement. Phenolphthalein 261,5
1) The temperatures indicated refer to theoretically pure chemicals;
the values of the actual melting Point for the Standard materials used
should be certified by the supplier.
6 Procedure
6.1 Calibration 7 Test report
The test report shall include the following information :
Calibrate the temperature-measuring System periodically over
the temperature range used for the test, with reagent grade or
a) reference to this International Standard;
certified chemicals.
b) reference of the method used (method A);
Chemicals recommended for calibration are listed in table 1,
c) complete identification and description of the material
6.2 Determination tested;
d) shape and size (or mass) of the specimens;
6.2.1 Insert the thermometer (4.3) and the capillary tube (4.2)
containing the specimen into the heating chamber [4.la)] and
e) previous thermal history of the specimens;
Start the heating. When the temperature of the specimen is
about 20 K below the expected melting temperature, regulate f) conditioning;
the rate of temperature increase to 2 k 0,5 K/min. Record the
g) heating rate;
temperature at which the specimen begins to Change shape.
h) temperatures, in degrees Celsius or in kelvins, of two
6.2.2 Repeat the sperations specified in 6.2.1 with a second successive individual measurements, and their arithmetic
specimen. If the two results obtained by the same Operator on
mean ;
the same Sample differ by more than 3 K, repeat the procedure
i) any operational details not specified in this International
on two new specimens.
Standard or regarded as optional, as well as any incidents
liable to have affected the results.
Insufficient data are available for establishing reproducibility.

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SIST EN ISO 3146:2000
ISO 31464985 (E)
- Polarizing microscope
Section two : Method B
8 Principie
10.3 Film or sheet materials
Cut a 2 to 3 mg Portion of the film or sheet, place it on a clean
Heating of a specimen, positioned between the polarizer and
slide, cover with a cover glass and proceed as specified in IO. 1.
analyser of a microscope, at a controlled rate.
NOTE - The preliminary melting of the specimens between slide and
Measurement of the temperature at which the crystalline
cover presents the advantage of destroying any birefringence due to
polymer loses its Optical anisotropy, as detected by the disap-
orientation or internal Stresses, and also of reducing the danger of
pearance of birefringence, as the melting temperature.
Oxidation during the test. The need for an inert gas stream - as
described in 11.2 - is thus limited to very special cases. The
reproducibility of th
...