EN ISO 12086-2:1999

SLOVENSKI STANDARD
01-maj-2000
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Plastics - Fluoropolymer dispersions and moulding and extrusion materials - Part 2:
Preparation of test specimens and determination of properties (ISO 12086-2:1995)
Plastiques - Polymeres fluorés: dispersions et matériaux pour moulage et extrusion -
Partie 2: Préparation des éprouvettes et détermination des propriétés (ISO 12086-
2:1995)
Ta slovenski standard je istoveten z: EN ISO 12086-2:1999
ICS:
83.080.20 Plastomeri Thermoplastic materials
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

INTERNATIONAL IS0
STANDARD 12086-Z
First edition
1995-12-15
Plastics - Fluoropolymer dispersions and
moulding and extrusion materials -
Part 2:
Preparation of test specimens and
determination of properties
P/as tiques - Polymh-es fluor&: dispersions et matbiaux pour moulage
et extrusion -
Partie 2: Pbpara tion des kprouve ttes et dhtermina tion des propriMs
Reference number
IS0 12086-2:1995(E)
ISO 12086-2:1995(E)
Contents
Page
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
1 Scope
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
2 Normative references
3 Definitions . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
4 Symbols and abbreviations . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
5 Sampling
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
6 Preparation of test specimens
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 4
7 Conditioning and test conditions
8 General testing of fluoropolymers . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
8.1 Electrical properties . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
8.2 Mechanical properties
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . .a. 6
8.3 Thermal-transition temperatures
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
8.4 Density
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
8.5 Flammability by oxygen index
8.6 Particle size and size distribution . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 8
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 13
9 Testing of fluoropolymer dispersions
9.1 General . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
9.2 Preparation of test samples
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
9.3 Isolation of PTFE from dispersion
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
9.4 Coagulum in dispersions
9.5 Percentage polymer and surfactant in aqueous dispersions 15
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
9.6 PTFE solids content by hydrometer
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
9.7 pH of dispersions
. . . . . . . . . . . . . . . . . . . . . . 16
10 Testing of PTFE and closely related materials
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .~.
10.1 General
. . . . . . . . . . . . . . . . . . . . . . 16
10.2 Preparation of test specimens by moulding
0 IS0 1995
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electronic or mechanical, including photocopying and
microfilm, without permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-1211 Geneve 20 l Switzerland
Printed in Switzerland
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
10.3 Bulk density
10.4 Extrusion pressure .*.*. 23
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
10.5 Powder-flow time 27
10.6 Standard specific gravity (SSG), extended specific gravity (ESG),
and thermal-instability index (TII) . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 27
10.7 Stretching-void index (SVI) . . 30
11 Testing of conventionally melt-processible fluoropolymers . . 32
11.1 Preparation of test specimens by moulding . . . . . . . . . . . . . . . . . . . . . . 32
11.2’ Melt mass-flow rate (MFR) and melt volume-flow rate (MVR) 33
12 Other test methods used with fluoropolymers . . . . . . . . . . . . . . . . . . . . 35
12.1 B.rittleness temperature of plastics and elastomers by impact 35
12.2 Coefficients of static and kinetic friction . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
12.3 Zero-strength time . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 35
Annexes
A Listing of test methods (alphabetical order) . . . . . . . . . . .a. 36
B Designator-y properties for common fluoropolymer types with
cross-reference listing to the tables for codes in IS0 12086-I and the
test methods in IS0 12086-2 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 37
. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
C Bibliography 40
Q IS0
IS0 12086-2:1995(E)
Foreword
IS0 (the International Organization for Standardization) is a worldwide
federation of national standards bodies (IS0 member bodies). The work
of preparing International Standards is normally carried out through IS0
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. IS0
collaborates closely with the International Electrotechnical Commission
(IEC) on all matters of electrotechnical standardization.
Draft International Standards adopted by the technical committees are
circulated to the member bodies for voting. Publication as an International
Standard requires approval by at least 75 % of the member bodies casting
a vote.
International Standard IS0 12086-2 was prepared by Technical Committee
lSO/TC 61, Plastics, Subcommittee SC 9, Thermoplastic materials.
IS0 12086 consists of the following parts, under the general title
P/as tics - Fluoropolymer dispersions and moulding and extrusion ma-
terials:
- Part 7: Designation system and basis for specifications
- Part 2: Preparation of test specimens and determination of proper-
ties
Annexes A, B and C of this part of IS0 12086 are for information only.

IS0 12086-2:1995(E)
INTERNATIONAL STANDARD 0 ISO
Plastics - Fluoropolymer dkpersions and moulding
and extrusion materials -
Part 2:
Preparation of test specimens and determination of
properties
WARNING - This part of IS0 12086 may involve hazardous materials, operations and equipment.
It does not purport to address all of the safety problems associated with its use. It is the
responsibility of the user of this part of IS0 12086 to establish appropriate safety and health
practices and determine the applicability of regulatory limitations prior to use. The warnings in
subclauses 8.6.1 .I, 9.7 and 10.6.1.3 point out specific hazards.
1.3 Agreements between vendor and purchaser
1 Scope
should preferably be based on properties measured
using the specimens and test conditions described in
this part of IS0 12086.
1.1 This part of IS0 12086 describes the prepara-
tion of test specimens and provides test methods to
define characteristics of thermoplastic fluoropolymer
resins. Results from the testing may be used as the
2 Normative references
basis for designation, material specifications, or both.
This part of IS0 12086 describes the conditions of
The following standards contain provisions which,
test for determining both designator-y and other prop-
through reference in this text, constitute provisions
erties of the homopolymers and various copolymers
of this part of IS0 12086. At the time of publication,
of fluoromonomers, as dispersions or powders for
the editions indicated were valid. All standards are
moulding, extrusion, and other uses. The test pro-
subject to revision, and parties to agreements based
cedures included are appropriate for, but are not re-
on this part of IS0 12086 are encouraged to investi-
stricted to, the fluoropolymers listed in clause 4 and
gate the possibility of applying the most recent edi-
for which designatory properties are specified in
tions of the standards indicated below. Members of
IS0 12086-I.
IEC and IS0 maintain registers of currently valid
International Standards.
1.2 The properties of semi-finished and finished
IS0 75-2: 1993, Plastics - Determination of tempera-
products made from fluoropolymer resins depend on
ture of deflection under load - Part 2: Plastics and
the material used, the shape of the product, the
ebonite.
physical and morphological state of the material re-
sulting from the processing operations, and on the
IS0 178:1993, Plastics - Determination of flexural
test conditions. Therefore, to obtain reproducible test properties.
results, the defined methods of preparation of test
IS0 179: 1993, Plastics - Determination of Charpy
specimens and defined test conditions given in this
impact strength.
part of IS0 12086 must be applied.

0 IS0
IS0 12086-2:1995(E)
IS0 12086-I : 1995, Plastics - Fluoropolymer disper-
IS0 180:1993, Piastics - Determination of lzod im-
sions and moulding and extrusion materials -
pact strength.
Part 1: Designation system and basis for specifica-
Standard atmospheres for
IS0 291:1977, Plastics - tions.
conditioning and testing.
IEC 93:1980, Methods of test for volume resistivity
IS0 293:1986, Plastics - Compression moulding test and surface resistivity of solid electrical insulating
specimens of thermoplastic materials. materials.
IEC 243-l : 1988, Methods of test for electric strength
IS0 47211988, Plastics - Vocabulary.
of solid insulating materials - Part 7: Tests at power
IS0 527-l :I 993, Plastics - Determination of tensile frequencies.
properties - Part I: General principles.
IEC 250: 1969, Recommended methods for the deter-
IS0 527-2:1993, Plastics - Determination of tensile
mination of the permittivity and dielectric dissipation
properties - Part 2: Test conditions for moulding and
factor of electrical insulating materials at power, audio
extrusion p/as tics.
and radio frequencies including metre wavelengths.
IS0 527-3:1995, Plastics - Determination of tensile
ASTM D 746-79(1987), Test method for brittleness
properties - Part 3: Test conditions for films and
temperature of plastics and elastomers by impact.
sheets.
ASTM D 1430-91 a, Specification for polychloro-
IS0 565:1990, Test sieves - Metal wire cloth, per-
trifluoroe thylene (PCTFE) p/as tics.
forated metal plate and electroformed sheet - Nom-
inal sizes of openings. ASTM D 1457-91 a, Specification for PTFE molding
and extrusion materials.
IS0 842:1984, Raw materials for paints and varnishes
- Sampling. ASTM D 1894-93, Test method for static and kinetic
coefficients of friction of plastic film and sheeting.
IS0 1043-I :I 987, Plastics - Symbols - Part I:
Basic polymers and their special characteristics. ASTM D 3418-83( 1988), Test method for transition
temperatures of polymers by thermal analysis.
IS0 1043-2:1988, Plastics - Symbols - Part 2: Fill-
ers and reinforcing materials. ASTM D 4052-91, Test method for density and rela-
tive density of liquids by digital density meter.
IS0 1133:1991, Plastics - Determination of the melt
mass-flow rate (MFR) and the melt volume-flow rate ASTM D 4591-93a, Test method for determining
(Ml/t?) of thermoplastics. temperatures and heats of transitions of fluoro-
polymers by differential scanning calorimetry.
IS0 1148:1980, Plastics - Aqueous dispersions of
polymers and copolymers - Determination of pH. ASTM D 4894-91 a, Specification for polytetrafluoro-
ethylene (PTFE) granular molding and ram extrusion
- Methods for determining
IS0 1183:1987, Plastics
materials.
the density and relative density of non-cellular
plastics. ASTM D 4895-91 a, Specification for polytetrafluoro-
ethylene (PTFE) resins produced from dispersion.
Determination of
IS0 4589: 1984, P/as tics -
flammability by oxygen index. BS 3406:Part 5:1983, Methods for determination of
particle size distribution - Part 5: Recommendations
IS0 8962:1987, Plastics - Polymer dispersions -
for electrical sensing zone method (the Coulter prin-
Determination of density.
ciple).
IS0 12000:-1), Plastics/rubber - Polymer disper-
BS 4641: 1986, Method for specifying electroplated
sions and rubber latices (natural and synthetic) -
coatings of chromium for engineering purposes.
Definitions and review of test methods.
1) To be published.
IS0 12086=2:1995(E)
0 IS0
NOTE 2 With PTFE, “moulding” and “compaction” are
3 Definitions
terms used interchangeably with “preforming”.
3.1 The terminology given in IS0 472 is applicable
3.2.9 sintering (as it applies to PTFE): A thermal
to this part of IS0 12086, except for terms defined in
treatment during which the material is melted and
3.2. The terms listed in 3.1 .I to 3.1.3 are repeated
recrystallized by cooling, with coalescence occurring
from IS0 472 to be sure there is no misunderstand-
during the treatment.
ing.
3.2.10 standard specific gravity (SSG): The spe-
3.1.1 dispersion: A heterogeneous system in which
cific gravity of a specimen of PTFE material pre-
a finely divided material is distributed in another ma-
formed, sintered, and cooled through the
terial.
crystallization point at a rate of 1 “C per minute in ac-
cordance with the appropriate sintering schedule as
3.1.2 fluoroplastic: A plastic based on polymers
described in this part of IS0 12086.
made with monomers containing one or more atoms
of fluorine, or copolymers of such monomers with
NOTE 3 The SSG of unmodified PTFE is inversely related
other monomers, the fluoromonomer(s) being in the
to its molecular mass.
greatest amount by mass.
3.2.11 suspension polymer: A polymer isolated
3.1.3 latex: A colloidal aqueous dispersion of a
from its liquid polymerization medium as a solid hav-
polymeric material.
ing a particle size well above colloidal dimensions.
3.2.12 zero-strength tim,e (ET): A measure of the
3.2 For the purposes of this part of IS0 12086, the
relative molecular mass of PCTFE.
following additional definitions apply.
3.2.1 amorphous: Noncrystalline, or devoid of reg-
ular structure.
4 Symbols and abbreviations
3.2.2 bulk density: The mass (in grams) per litre of
material, measured under the conditions of the test.
4.1 The abbreviated terms given in IS0 1043-I and
IS0 1043-2 are applicable to this part of IS0 12086.
3.2.3 copolymer: A polymer formed from two or
more types of monomer.
4.2 This part of IS0 12086 is particularly concerned
3.2.4 emulsion polymer (as it applies to fluoro-
with, but is not limited to, test methods for the ma-
Material isolated from its
polymer materials):
terials listed below:
polymerization medium as a colloidal aqueous disper-
polytetrafluoroethylene
PTFE
sion of the polymer solids.
PFA perfluoro(alkoxy alkane)
NOTE 1 This definition, used in the fluoropolymer indus-
try, is similar to that for “latex” in IS0 472 and is quite dif-
FEP perfluoro(ethylene-propene)
ferent from the definition for “emulsion” in IS0 472.
copolymer
3.2.5 fluorocarbon plastic: A plastic based on
EFEP ethylene-tetrafluoroethylene-
polymers made from perfluoromonomers only.
hexafluoropropene copolymer
3.2.6 fluoropolymer: Synonymous with fluoro-
TFE/PDD tetrafluoroethylene-perfluoro(dioxole)
plastic (see 3.1.2).
copolymer
3.2.7 melt-processible: Capable of being processed
VDF/HFP vinylidene fluoride-
by, for example, injection moulding, screw extrusion,
hexafluoropropene copolymer
and other operations typically used with thermo-
plastics.
VDF/TFE vinylidene fluoride-
tetrafluoroethylene copolymer
3.2.8 preforming: Compacting powdered PTFE ma-
VDF/TFE/HFP vinylidene fluoride-
terial under pressure in a mould to produce a solid
tetrafluoroethylene-
object, called a preform, that is capable of being han-
hexafluoropropene copolymer
dled.
0 IS0
IS0 12086-2:1995(E)
ethylene-tetrafluoroethylene
ETFE
7 Conditioning and test conditions
copolymer
7.1 For tests of specific gravity, tensile properties,
poly(vinylidene fluoride)
PVDF
and electrical properties, condition the moulded test
specimens in atmosphere 23 of IS0 291 for a period
vinylidene fluoride-
VDF/CTFE
of at least 4 h prior to testing. The other tests require
chlorotrifluoroethylene copolymer
no conditioning.
PCTFE polychlorotrifluoroethylene
NOTE 4 For PVDF, some producers recommend waiting
PVF poly(vinyl fluoride)
one week after moulding before testing in order to minimize
the effects of post crystallization.
ethylene-chlorotrifluoroethylene
ECTFE
copolymer
7.2 Conduct tests at a laboratory temperature of
23 “C + 2 “C for determining specific gravity, tensile
properfies, and electrical properties only. (See note 5
for comments related to PTFE.) Since the fluoro-
4.3 For the purposes of this part of IS0 12086, the
polymer resins do not absorb water, the maintenance
following abbreviated terms apply in addition to those
of constant humidity during testing is not necessary.
given in 3.2 and 4.2.
Conduct tests for melt flow rate and melting-peak
AF amorphous fluoropolymer
temperature under ordinary laboratory conditions.
ESG extended specific gravity (see 10.6)
NOTE 5 A minimum temperature of 22 “C should prefer-
ably be maintained with PTFE due to its first-order transition
MFR melt mass-flow rate (see 11.2)
just below 22 “C that affects properties determined at
slightly lower temperatures. This effect of temperature is
MVR melt volume-flow rate (see 11.2)
especially important during the determination of
density/specific gravity.
SSG standard specific gravity (see 10.6)
stretching-void index (see 10.7)
SVI
8 General testing of fluoropolymers
thermal-instability index (see 10.6)
TII
Properties required for designation or specification,
ZST zero-strength time (see 12.3)
or both, shall be determined in accordance with the
international or national standards listed in clause 2
or the procedures given in this part of IS0 12086.
Tables of values of the designatory properties and
corresponding codes are included in IS0 12086-I.
5 Sampling
Tables of values and codes are also included in this
part of IS0 12086 for many of the other properties
The materials should preferably be sampled in ac-
that are needed to supplement the designatory prop-
cordance with IS0 842. Adequate statistical sampling
erties for specification and other purposes.
shall be considered an acceptable alternative. Special
considerations are included in the pertinent clause.
8.1 Electrical properties
8.1 .I Dielectric constant and dissipation factor
Determine these properties on three specimens, each
6 Preparation of test specimens
100 mm in diameter, in accordance with IEC 250.
Where applicable, IS0 standards shall be followed for Typical frequencies used for testing are 100 Hz,
the preparation of test specimens. In some instances, 1 kHz, 1 MHz and 100 MHz. For some applications,
it is important to know the values at subambient and
special procedures are required that are described ei-
elevated temperatures. Codes for test frequencies
ther in the general discussion or in the method.
and values of the properties are given in tables 1 and
2 .
IS0 12086=2:1995(E)
0 IS0
NOTE 6 Electrical properties, like many other properties,
vary with temperature.
Table 3 - Codes and ranges for dielectric
strength
Code Dielectric strength (kV/mm)
A <5
Table 1 - Codes for test frequencies
B 5to<10
Test frequency
Code
C 10to<15
D 15to<20
100 Hz
E 20 to < 25
1 kHz
F 25 to < 30
1 MHz
100 MHz G 30 to < 35
35 to < 40
H
I 40 to < 45
J 45 to < 50
K 50 to < 55
L 55 to < 60
Table 2 - Codes and ranges for dielectric
M 60 to < 65
constant and dissipation factor
N 65 to < 70
0 70 to < 75
Dielectric
Code Code Dissipation factor
P 75 to < 80
constant
Q 80 to < 85
< I,6 A < 0,000 1
A
R 85 to < 90
B 0,000 1 to < 0,000 2
B I,6 to < I,8
S 90 to < 95
I,8 to < 2,0 C 0,000 2 to < 0,000 4
C
T 95 to < 100
D 2,0 to < 2,2 D 0,000 4 to < 0,000 6
U 3 100
E 2,2 to < 2,4 E 0,000 6 to < 0,000 8
F 2,4 to < 2,6 F 0,000 8 to < 0,001 0
G 2,6 to < 2,8 G 0,001 0 to < 0,001 2
H 2,8 to < 3,0 H 0,001 2 to < 0,001 4
I
I 3,0 to < 3,2 0,001 4 to < 0,001 6
8.1.3 Surface resistivity
J 0,001 6 to < 0,001 8
J 3,2 to < 3,4
K 0,001 8 to < 0,002 0
K 3,4 to < 3,6
Determine this property in accordance with IEC 93.
L 0,002 0 to < 0,002 2
L 3,6 to < 4,0
Codes and ranges are listed in table4.
M 4,0 to < 4,5 M 0,002 2 to < 0,002 4
N 4,5 to < 5,0 N 0,002 4 to < 0,002 6
0 5,0 to < 5,5 0 0,002 6 to < 0,002 8
Table 4 - Codes and ranges for surface
P 5,5 to < 6,0 P 0,002 8 to < 0,003 0
resistivity
Q 6,0 to < 6,5 R 0,003 0 to < 0,003 5
S 6,5 to < 7,0 S 0,003 5 to < 0,004 0
Code Surface resistivity (a)
I I
I
T 7,0 to < 8,0 T 0,004 0 to < 0,006 0
U 8,0 to < 9,0 U 0,006 0 to < 0,008 0 A < IO3
V 9,0 to < IO,0 V 0,008 0 to < 0,010 B IO3 to lo'*
W
W IO,0 to < 11 ,o 0,010 to < 0,030 C > lo'*
X 11 ,o to < 12,0 X 0,030 to < 0,lO
Y
Y 12,o to < 14,0
> Ql
Z 3 14,0
8.2 Mechanical properties
8.1.2 Dielectric strength (electric strength)
8.2.1 Impact properties
Determine this property in accordance with the pro- Determine impact properties using the procedures of
cedures of IEC 243-l. Codes for values of the prop- IS0 180 for lzod impact strength and IS0 179 for
erty are given in table3. Charpy impact strength. Codes and ranges are given
in table 5. The test used, the size of the test speci-
NOTE 7 Dielectric strength, which is expressed in kilo-
men, and the type of notch shall be reported in addi-
volts per millimetre, varies with the thickness of the test
tion to the code for impact strength.
specimen.
0 IS0
IS0 12086=2:1995(E)
(078) 15.10.77, Fax: (078) 41.05.45, and Accurate Steel Rule
Die Co., 22 West 21st Street, New York, NY 10010, USA,
Table 5 - Codes and ranges for impact
Tel.: (212) 242-3606. This information is given for the con-
properties
venience of users of this part of IS0 12086 and does not
constitute an endorsement by IS0 of these products. Other
Code Impact strength (J/m)
sources may be available or a die may be constructed from
A < 100
details in figure 1.
I3 120 to < 140
C 140 to < 160
Calculate the percentage elongation using the follow-
D 160 to < 180
ing equation:
180 to E
F 200 to < 300
1 OOd
% elongation = p
G 300 to < 400
22,0m
H 400 to < 500
I 500 to < 600
where
J 600 to < 700
K 700 to < 800
is the distance, in millimetres, on the chart;
d
L 800 to < 900
M > 900
m is the chart-speed magnification
[= chart speed/crosshead speed (both in
same units)];
8.2.2 Tensile properties
22,0 is a factor allowing for the fact that d is in
8.2.2.1 Fluoropolymers for which tensile
millimetres.
modulus is not to be determined
8.2.2.1.3 ASTM D 1457 includes a summary of the
8.2.2.1.1 PTFE skived film with a thickness equal to
precision for tensile strength and percentage elon-
or less than 0,125 mm shall be tested in accordance
gation at break for PTFE, FEP, and PFA. Additional
with the procedure described in IS0 527-3:1995, us-
round-robin testing on use of the microtensile die is
ing test specimen type 2.
in progress within ASTM Committee D-20.
8.2.2.1.2 For test specimens other than the skived
Bias is a systematic error that contributes to the dif-
film referred to in 8.2.2.1 .I (equal to or less than
ference between a test result and a true (or reference)
0,125 mm in thickness), prepare five specimens using
value. There are no recognized standards on which to
the microtensile die described in figure 1. The die shall
base an estimate of bias for this test procedure.
be of the steel-rule type with a curvature of
5 mm + 0,5 mm (see note 8). Determine the tensile
8.2.2.2 Fluoropolymers for which tensile
proper&s in accordance with the procedures de-
modulus is to be determined
scribed in IS0 527-l except that the specimens used
shall be as detailed above, the initial jaw separation
Determine tensile properties in accordance with
shall be 22,0 mm + 0,13 mm, and the speed of test-
IS0 527-2:1993 using test specimen 5A and a cross-
ing shall be 50 mm/min & 5 mm/min. Clamp the
head speed of 50 mm/min + 5 mm/min. For deter-
-
specimens with an essentially equal length in each
mination of tensile modulus, use a crosshead speed
jaw. Determine the elongation from the recorder
of 1 mm/min.
chart, expressing it as a percentage of the initial jaw
separation. In determining elongation from the chart,
8.2.3 Modulus in flexure
draw a perpendicular line from the break point to the
time axis. Measure the distance along the time axis
Determine this property in accordance with the pro-
from the foot of this perpendicular line to the begin-
cedures of IS0 178.
Optionally, an
of the load-time curve.
ning
extensiometer may be used to determine the elon-
8.3 Thermal-transition temperatures
gation.
8.3.1 Deformation temperature under load
NOTE 8 The steel-rule type of die has been found satis-
factory for this purpose. Two sources for these steel-rule
Determine this temperature in accordance with the
dies are: Stansvormenfabriek Vervloet B.V., Postbus 220,
procedures of IS0 75-2.
Gantelweg 15, 3350 AE Papendrecht, Netherlands, Tel.:
IS0 12086=2:1995(E)
Dimensions in millimetres
Rockwell C hardness 45to 50
Steel-rule die
(Inside dimensions for die are the same astestspecimen)
Die to be sharpened on outside edge only (as shown in A-A)
r8 22~0,25 =8
- t *
I I
- -
Possible thicknesses: I,5 ?0,3
I I
+O,lS
1 +O,l
OS
0,125 ?0,03
Test specimen
Figure 1 - Microtensile die
8.3.2 Glass-transition temperature(s) 8.3.3.1 Test samples/specimens for melting-peak
temperature determination may be powder as re-
ceived, dried polymer isolated from a dispersion, or
Determine these temperatures in accordance with the
the required amount cut from a pellet or fabricated
procedures of ASTM D 3418.
-piece of the resin as sold or received. The test shall
be determined on a IO mg + 2 mg specimen of dry
polymer. It is desirable, but not essential, to test two
specimens, each being run twice, using both a heat-
8.3.3 Melting-peak temperature
ing and a cooling cycle.
Melting-peak temperature characteristics are specific Some fluoropolymers such as PTFE show different
for fluoropolymers and help identify a particular ma- melting behaviour the first time a virgin powder is
terial. The procedures of ASTM D 4591 supple- melted compared to the second and subsequent de-
mented by ASTM D 3418 are appropriate for this terminations that have lower melting-peak tempera-
tures. Both the first and second melting points shall
determination.
Q IS0
IS0 12086=2:1995(E)
8.6.1 Wet-sieve analysis
be measured. With PTFE, the second melting point
usually is 327 “C + 10 “C. The first melting point is
8.6.1 .I Significance and use
normally at least 5 “C higher than the second melting
point.
The fabrication of PTFE resins either by moulding or
extrusion is affected significantly by particle (or ag-
8.3.3.2 Use differential scanning calorimetry (DSC)
glomerate) size and size distribution. The average
as described in ASTM D 3418 and ASTM D 4591 for
particle size of PTFE resins is determined by
this determination. The heating rate shall be
fractionation of the material with a series of sieves.
10 “C + 1 “C per minute. Two peaks during the initial
-
Fractionation is facilitated by spraying the powder on
melting test are observed occasionally. In this case,
a sieve with an organic liquid that wets the powder,
report the peak temperatures as q for the lower
breaks up lumps, and prevents clogging of the sieve
temperature and T” for the upper temperature. Report
openings. In published test procedures, the liquid
the temperature corresponding to the peak largest in
specified is perchloroethylene (see warning). Use of
height as the melting point if a single value is re-
isopropyl alcohol or ethyl alcohol has been reported
quired. If a peak temperature is difficult to discern
as giving equivalent results when used as a replace-
from the curves - that is, if the peak is rounded
ment for perchloroethylene.
rather than pointed - draw straight lines tangentially
to the sides of the peak. Take the temperature corre-
WARNING - Perchloroethylene is under investi-
sponding to the point where these lines intersect be-
gation by government agencies and industry for
yond the peak as the peak temperature.
its carcinogenic effects. Protective nitrile or butyl
gloves should be worn to prevent skin contact and
8.3.3.3 Other thermal techniques may be used if the
adequate ventilation provided to remove the va-
user demonstrates that they are capable of measuring
pours.
the melting-peak temperature and give results of
equivalent significance.
8.6.1.2 Apparatus and materials
8.6.1.2.1
Balance, capable of weighing to + 0,l g.
8.4 Density
8.6.1.2.2 Standard sieves, 203-mm diameter, con-
Cut two specimens from the moulding or other solid
forming to IS0 565. It is suggested that the following
sample and test in accordance with IS0 1183. If
sieve openings (sieve numbers) be used: I,4 mm
method D is used, the solution in the tube shall have
(No. 14), 1 mm (No. 18) 710 pm (No. 25) 500 pm
a linear density gradient as specified in the table ap-
(No. 35), 355 pm (No. 45) 250 pm (No. 60) and
propriate for the fluoropolymer being tested.
180 pm (No. 80). The equivalent sieve numbers, given
for information, are those defined in ASTM E 11 (see
8.5 Flammability by oxygen index
annex C). Other sieve configurations may be used
provided they give equivalent results. It is desirable to
Use the procedure of IS0 4589.
use a set of sieves that have openings that are uni-
formly related on a logarithmic scale.
8.6 Particle size and size distribution
8.6.1.2.3 Ventilated hood.
The wet- and dry-sieve procedures of 8.6.1 and 8.6.2
8.6.1.2.4 Six tared beakers, capacity 150 ml.
are widely used with PTFE and closely related ma-
terials. The resistance-variation test procedure in 8.6.3
NOTE 9 As an alternative, the sieves may be tared, dried,
(the Coulter principle) is often used with PVDF, PTFE
and weighed on a balance to avoid errors that can be intro-
filler resin, and fine-cut suspension powders. The
duced during transfer of fractionated samples to the tared
light-scattering procedures in 8.6.4 are becoming
beakers.
more widely used with all the fluoropolymers. Use of
automated or other instruments that have been
8.6.1.2.5 Sieving and solvent-spraying appar-
shown to provide equivalent results shall be an ac-
atus.
ceptable alternative to the detailed procedures given
in this part of IS0 12086. ASTM F 660 (see annex C) A suggested arrangement for an apparatus with re-
provides a standard practice for comparing particle circulating spray liquid is shown in figure2. The ap-
size determined with different types of au.tomatic paratus shall be located, and the operations carried
out, in a ventilated hood or adequately ventilated area.
particle counter.
IS0 12086=2:1995(E)
Dimensions in millimetres
7 Sieve
Pa pe;?,,%,,,,
Table top
@ 460
I I
Portable all-purpose -
-
shower head
Stacked sieves
All plastic tubing
# int. 13 mm
Clamp to adjust
flow rate
Support
20 1 carboy
Centrifugal pump capable
of delivering 6 Umin at
shower head
Perchloroethylene
-7 ~-~e*t.,3mmglasstubing
(or alternative solvent)
*) Use a fine sieve to prevent material from going into the reservoir.
A standard 38 pm sieve has been found to be convenient.
Figure 2 - Apparatus for wet-sieve analysis
IS0 12086=2:1995(E)
where
8.6.1.3 Spray liquid, 20 litres.
See the comments and warning in 8.6.1 .I. Although F = 2 for a 50 g test sample;
perchloroethylene has been the usual choice, an al-
F = 10 for 10 g test sample.
ternative liquid may be used after its applicability and
hazards associated with its use have been investi-
gated thoroughly and use of the liquid shown to be
satisfactory.
8.6.1.5.2 Calculate the cumulative percentage of
resin on each sieve as follows:
8.6.1.4 Procedure
Cumulative percentage of resin on sieve Y = sum
8.6.1.4.1 Weigh out a 10 g test sample for powders
having
of net percentage on sieve Y and on sieves
with a particle size less than 100 pm or a 50 g test
sizes greater (i.e. numbers smaller) than Y
sample for powders with a larger particle size. Adjust
the rate of flow of the spray liquid to
EXAMPLE
6 I/min j, 0,5 I/min.
Cumulative percentage on 500 pm (No. 35 sieve
)
8.6.1.4.2 Place the weighed resin on the top sieve
equals net percentage on I,4 mm (No. 14) plus net
and spray it with the organic spray liquid for
percentage on I,00 mm (No. 18) plus net percentage
1 min + 0,2 min. The shower head shall be about
-
on 710 pm (No. 25) plus net percentage on 500 pm
level with the top of the sieve and be moved in a cir-
(No. 35) sieve.
cular fashion. Take care to break up all of the lumps
and to wash the material from the sides of the sieve.
8.6.1.4.3 Remove the top sieve and place it in the
8.6.1.5.3 Plot the cumulative percentage versus the
hood to dry until all of the sieves are ready for oven
sieve opening size (or sieve number) on log/log paper
drying as described in 8.6.1.4.4.
as shown in the sample plot in figure3. The sieve
numbers and sieve opening sizes in micrometres are
8.6.1.4.4 Repeat the procedure specified in 8.6.1.4.2
indicated below the figure. Draw the best straight line
and 8.6.1.4.3 until all the sieves have been sprayed.
through the points and read the particle size at the
Dry the sieves in a ventilated oven at a temperature
50 % cumulative percentage point (d50). Take this
of at least 90 “C up to a maximum of 130 “C for at
value as the average particle size.
least 15 min up to a maximum of 30 min and then
cool to room temperature. Remove the resin from
It is permissible to carry out the calculation of d50 by
each sieve by tapping on a piece of paper as shown
use of computer programmes that provide “best-fit”
in the insert in figure2. Pour each fraction into a tared analysis using linear regression procedures involving
beaker and weigh to + 0,l g.
a log-normal model.
8.6.1.4.5 Record the mass of resin on each sieve.
8.6.1.6 Precision and bias
8.6.1.4.6 Clean the sieve by inverting it over filter
paper and spraying with spray liquid. Take care to
Because the resin particles have complex shapes, and
prevent the resin from getting into the spray liquid.
because on each sieve there is a distribution of par-
ticle sizes, the values for particle size and particle-size
8.6.1.5 Expression of results
distribution obtained will be only relative numbers.
The 95 % confidence limits based on a limited series
8.6.1.5.1 Calculate the net percentage of resin on
of tests are + 2,8 % for the average particle size.
each sieve as follows:
Since there is no accepted reference material suitable
Net percentage of resin on sieve Y = F x mass, in for determining the bias for this test procedure, no
statement on bias is being made.
grams, on sieve Y
IS0 12086=2:1995(E)
0 IS0
2 5 10 15 20 30 40 50 60 70 80 85 90 95 98
Cumulative percentage, %
Sieve No. Sieve opening
Pm
14 1 400
18 1 000
35 500
45 355
60 250
80 180
Figure 3 - Typical log/log probability plot for sieve analysis
8.6.2 Dry-sieve analysis provided they give equivalent results. It is desirable to
use a set of sieves that have openings that are uni-
formly related on a logarithmic scale.
8.6.2.1 Significance and use
The fabrication of PTFE resins may be affected sig-
8.6.2.2.3 Mechanical sieve shaker, capable of im-
nificantly by particle (or agglomerate) size and size
parting a uniform rotary and tapping action.
distribution. The average particle size of PTFE resins
is determined by fractionation of the material with a
8.6.2.2.4 Freezer: any commercial ice freezer (a
series of sieves. Fractionation is accomplished by
dry-ice chest may be used).
mechanically shaking the material in an assembly of
sieves for a specified period.
8.6.2.3 Procedure
8.6.2.2 Apparatus
8.6.2.3.1 Place 50 g + 0,l g of the sample in an
-
aluminium pan, and cool the pan and contents to less
8.6.2.2.1 Balance, capable of weighing to + 0,l g.
than 10 “C.
8.6.2.2.2 Standard sieves, 203-mm diameter, con-
8.6.2.3.2 Measure the tare mass of each of the
forming to IS0 565. It is suggested that the following
sieves listed in 8.6.2.2.2. Place the conditioned test
sieve openings (sieve numbers) be used: I,4 mm
sample on the top sieve of the assembly and shake
(No. 14), 1 mm (No. 18), 710 pm (No. 251, 500 pm
(No. 35), 355 pm (No. 45), 250 pm (No. 60) and in the sieve shaker for 10 min + 0,5 min. The dew-
180 pm (No. 80). The equivalent sieve numbers, given point temperature of the sieving room shall be less
for information, are those defined in ASTM E 11 (see than the temperature of the conditioned test sample
annex C). Other sieve configurations may be used so that water will not condense on the test sample
0 IS0
IS0 12086=2:1995(E)
8.6.3.1 Significance and use
during the test. Determine the mass of resin retained
on each sieve.
Fluoropolymer powders have various uses that de-
pend on their particle size and distribution. For some
8.6.2.4 Expression of results
of these, such as the powder forms of PVDF, the
sieve analysis procedures are not the method of
8.6.2.4.1 Calculate the net percentage of resin on
choice.
each sieve as follows:
8.6.3.2 Apparatus
Net percentage of resin on sieve Y = 2 x mass, in
grams, on sieve Y
8.6.3.2.1 Electric sensing-zone particle counter,
8.6.2.4.2 Calculate the cumulative percentage of
with an orifice tube such that most of the particles lie
resin on each sieve as follows:
within its measurement range (2 % to 60 % of the
orifice-tube diameter). Calibration of the instrument in
Cumulative percentage of resin on sieve Y = sum
absolute terms shall be done by the count-integration
of net percentage on sieve Y and on sieves having
procedure on narrow distributions of standard latices
er) than Y
sizes greater (i.e. numbers smal
(essentially monosized particles suspended in distilled
water containing a surfactant) that are available from
EXAMPLE
various sources. Poly(styrene-co-divinyl benzene)
latices are particularly recommended.
Cumulative percentage on 500 p n (No. 35) sieve
(No. 14) plus net
equals net percentage on I,4 mm
percentage on 1 mm (No. 18) plus net percentage on
8.6.3.2.2 Analytical balance.
710 pm (No. 25) plus net percentage on 500 pm
(No. 35) sieve.
8.6.3.2.3 Magnetic stirrer.
8.6.2.4.3 Plot the cumulative percentage versus the
8.6.3.2.4 Ultrasonic tank.
sieve opening size (or sieve number) on log/log paper
as shown in the sample plot in figure3. The sieve
numbers and sieve opening sizes in micrometres are
8.6.3.3 Procedure
indicated below the figure. Draw the best straight line
throught the points and read the particle size at the
8.6.3.3.1 Prepare a solution of a non-ionic surfactant
50 % cumulative percentage point (d50). Take this
(see note IO) at a concentration of 0,2 g/l to 0,3 g/l in
value as the average particle size.
an aqueous electrolyte, such as a 1 % (m/V) solution
of sodium chloride or a special 1 % (m/V) saline sol-
It is permissble to carry out the calculation of d50 by
ution (see note 11). For example, four drops of the
use of computer programmes that provide “best-fit”
surfactant in 500 ml of electrolyte solution is sufficient
analysis using linear regression procedures involving
to obtain a satisfactory suspension of the powder with
a log-normal model.
moderate foaming. Filter the solution using a 0,3 pm
barrier filter (see note 12).
8.6.2.5 Precision and bias
NOTES
The test precision is + 3,2 % (two sigma limits) for
the combined sieve fractions for the 710 pm +
10 Triton X-100, a surfactant of the octylphenol series,
500 pm + 355 pm (No. 25 + 35 + 45) sieves for a from Rohm & Haas, has been found to be satisfactory.
Other, similar, materials should be equally effective.
resin where this combination of sieves retains, on the
average, 78 % of the sample. Since there is no ac-
11 A specially prepared solution, known as Isoton, is
cepted reference material suitable for determining the
available from Coulter Counter Ltd.
bias for this test procedure, no statement on bias is
being made.
12 Available from the Millipore Corporation.
13 This information is given for the convenience of users
Particle size and size distribution by the
8.6.3
of this part of IS0 12086 and does not constitute an
Coulter principle using a resistance-variation
endorsement by IS0 of these materials.
tester
A test method for use of this equipment with pow-
...