Rubber, ethylene-propylene-diene (EPDM) — Evaluation procedure

ISO 4097:2007 specifies physical and chemical tests on raw rubbers; standard materials, standard test formulations, equipment and processing methods for evaluating the vulcanization characteristics of ethylene-propylene-diene (EPDM) rubbers, including oil-extended types.

Caoutchouc éthylène-propylène-diène (EPDM) — Méthode d'évaluation

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Status
Withdrawn
Publication Date
09-Jul-2007
Withdrawal Date
09-Jul-2007
Current Stage
9599 - Withdrawal of International Standard
Completion Date
22-Sep-2014
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ISO 4097:2007 - Rubber, ethylene-propylene-diene (EPDM) -- Evaluation procedure
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INTERNATIONAL ISO
STANDARD 4097
Fifth edition
2007-07-15

Rubber, ethylene-propylene-diene
(EPDM) — Evaluation procedure
Caoutchouc éthylène-propylène-diène (EPDM) — Méthode d'évaluation




Reference number
ISO 4097:2007(E)
©
ISO 2007

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ISO 4097:2007(E)
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ii © ISO 2007 – All rights reserved

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ISO 4097:2007(E)
Contents Page
Foreword. iv
1 Scope. 1
2 Normative references. 1
3 Sampling and sample preparation. 1
4 Physical and chemical tests on raw rubber. 2
4.1 Mooney viscosity. 2
4.2 Volatile matter. 2
4.3 Ash. 2
5 Preparation of test mixes for evaluation . 2
5.1 Standard test formulations . 2
5.2 Procedure. 3
6 Evaluation of vulcanization characteristics by a curemeter test. 7
6.1 Using an oscillating-disc curemeter. 7
6.2 Using a rotorless curemeter . 7
7 Evaluation of tensile stress-strain properties of vulcanized test mixes. 7
8 Precision. 8
8.1 General. 8
8.2 Precision details. 8
8.3 Precision results. 8
9 Test report. 9
Bibliography . 11

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ISO 4097:2007(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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. 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.
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.
ISO 4097 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee
SC 3, Raw materials (including latex) for use in the rubber industry.
This fifth edition cancels and replaces the fourth edition (ISO 4097:2000), which has been technically revised.

iv © ISO 2007 – All rights reserved

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INTERNATIONAL STANDARD ISO 4097:2007(E)

Rubber, ethylene-propylene-diene (EPDM) — Evaluation
procedure
WARNING — Persons using this International Standard should be familiar with normal laboratory
practice. This standard 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 national regulatory conditions.
1 Scope
This International Standard specifies
⎯ physical and chemical tests on raw rubbers;
⎯ standard materials, standard test formulations, equipment and processing methods for evaluating the
vulcanization characteristics of ethene-propene-diene (EPDM) rubbers, commonly termed ethylene-
propylene-diene rubbers, including oil-extended types.
2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 37, Rubber, vulcanized or thermoplastic — Determination of tensile stress-strain properties
ISO 247:2006, Rubber — Determination of ash
ISO 248, Rubber, raw — Determination of volatile-matter content
ISO 289-1, Rubber, unvulcanized — Determinations using a shearing-disc viscometer — Part 1:
Determination of Mooney viscosity
ISO 1795, Rubber, raw natural and raw synthetic — Sampling and further preparative procedures
ISO 2393, Rubber test mixes — Preparation, mixing and vulcanization — Equipment and procedures
ISO 3417, Rubber — Measurement of vulcanization characteristics with the oscillating disc curemeter
ISO 6502, Rubber — Guide to the use of curemeters
ISO 23529, Rubber — General procedures for preparing and conditioning test pieces for physical test
methods
3 Sampling and sample preparation
3.1 Take a laboratory sample of approximately 1,5 kg by the method described in ISO 1795.
3.2 Prepare the test portion in accordance with ISO 1795.
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ISO 4097:2007(E)
4 Physical and chemical tests on raw rubber
4.1 Mooney viscosity
Determine the Mooney viscosity in accordance with ISO 289-1, on a test portion prepared as indicated in 3.2
(without massing).
If massing is necessary, maintain the mill roll surface temperature at 50 °C ± 5 °C (for rubbers with a low
Mooney viscosity, a temperature of 35 °C ± 5 °C can be used). Massing, if used, shall be mentioned in the test
report.
Record the result as ML(1+4) at 125 °C unless another test temperature (100 °C or 150 °C) and/or test time
(1+8) min has been agreed by the interested parties.
4.2 Volatile matter
Determine the volatile-matter content in accordance with ISO 248.
4.3 Ash
Determine the ash in accordance with method A or method B of ISO 247:2006.
5 Preparation of test mixes for evaluation
5.1 Standard test formulations
The standard test formulations are given in Table 1, in which:
⎯ formulation 1 is applicable to non-oil-extended EPDMs with a nominal ethylene content not higher than
67 % by mass;
⎯ formulation 2 is applicable to non-oil-extended EPDMs with a nominal ethylene content equal to or higher
than 67 % by mass;
⎯ formulation 3 is applicable to non-oil-extended low Mooney viscosity EPDMs;
⎯ formulation 4 is applicable to oil-extended EPDMs containing 50 or less parts by mass of oil per 100 parts
of rubber;
⎯ formulation 5 is applicable to oil-extended EPDMs containing more than 50 but less than 80 parts by
mass of oil per 100 parts of rubber;
⎯ formulation 6 is applicable to oil-extended EPDMs containing 80 or more parts by mass of oil per
100 parts of rubber.
The materials used shall be national or international standard reference materials, unless no standard
reference materials are available, in which case the materials to be used shall be agreed between the
interested parties.
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ISO 4097:2007(E)
Table 1 — Standard test formulations for evaluation of EPDM rubbers
Test formulation
Material
1 2 3 4 5 6
Parts by mass
a b c
EPDM 100,00 100,00 100,00 100,00 + x 100,00 + y 100,00 + z
Stearic acid 1,00 1,00 1,00 1,00 1,00 1,00
Industry reference
80,00 100,00 40,00 80,00 80,00 150,00
d
black
e a
ASTM 103 oil 50,00 75,00 — 50,00 − x — —
Zinc oxide 5,00 5,00 5,00 5,00 5,00 5,00
Sulfur 1,50 1,50 1,50 1,50 1,50 1,50
Tetramethyl thiuram
1,00 1,00 1,00 1,00 1,00 1,00
f
disuffide (TMTD)
Mercaptobenzothiazole
0,50 0,50 0,50 0,50 0,50 0,50
(MBT)
b c
Total 239,00 284,00 149,00 239,00
189,00 + y 259,00 + z
a
x is the number of parts by mass of oil per 100 parts of base rubber for types having an oil content of 50 or less.
b
y is the number of parts by mass of oil per 100 parts of base rubber for types having an oil content more than 50 but less than 80.
c
z is the number of parts by mass of oil per 100 parts of base rubber for types having a minimum oil content of 80.
d
The current industry reference black (IRB) shall be used.
e 3
This oil, density 0,92 g/cm , is produced by the Sun Refining and Marketing Company and distributed by R.E. Carroll Inc., 1570
North Olden Avenue Ext, Trenton, NJ 08638, USA. Overseas requests should be directed to Sunoco Overseas Inc., 1801 Market Street,
Philadelphia, PA 19103-1699, USA. Alternative oils can be used but may give slightly different results.
f
A standard reference material for TMTD is available as IRM 1 from Forcoven Products Inc., 22010 E. Martin Dr., Porter, TX 77365,
USA.

5.2 Procedure
5.2.1 Equipment and procedure
Equipment and procedure for the preparation, mixing and vulcanization shall be in accordance with ISO 2393.
5.2.2 Mixing procedures
5.2.2.1 General
Three alternative mixing procedures are specified:
⎯ method A: internal mixing;
⎯ method B: mill mixing;
⎯ method C: use of internal mixer for initial and mill for final mixing.
NOTE Mixing of ethylene-propylene-diene rubbers in the standard test formulations using a mill is more difficult than
for other rubbers and the use of an internal mixer allows better results to be obtained. Because of the difficulty of mill
mixing EPDM rubbers, it is recommended that method B be used only if an internal mixer is not available.
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ISO 4097:2007(E)
5.2.2.2 Method A — Internal mixing
5.2.2.2.1 Initial mixing procedure
 Duration Cumulative time
(min) (min)
a) Adjust the temperature of the internal mixer to achieve a final mix 0 0
temperature of 150° C in about 5 min. Close the discharge door, set the
rotor at 8 rad/s (77 r/min), start the rotor and raise the ram.
b) Load the rubber, the zinc oxide, the carbon black, the oil and the stearic 0,5 0,5
acid. Lower the ram.
c) Allow the batch to mix. 2,5 3,0
d) Raise the ram and clean the mixer throat and the top of the ram. Lower 0,5 3,5
the ram.
e) Discharge the batch when the temperature reaches 150 °C or after max. 1,5 5,0
5 min, whichever occurs first.
Total time (max.) 5,0
f)
Immediately pass the batch three times through a laboratory mill with its mill opening set at 2,5 mm and
at a temperature of 50 °C ± 5 °C. Check-weigh the batch (see ISO 2393). If the mass of the batch differs
+0,5
from the theoretical value by m
...

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