ISO 2302:2005

Isobutene-isoprene rubber (IIR) — Evaluation procedures

ISO 2302:2005 specifies physical and chemical tests on raw rubbers; standardized materials, a standardized test formulation, equipment and processing methods for evaluating the vulcanization characteristics of all types of isobutene-isoprene rubber (IIR). The precision data in ISO 2302:2005 have been taken, with permission of ASTM, from ASTM D 3188-95, Standard Test Methods for Rubber -- Evaluation of IIR (Isobutene-Isoprene Rubber), copyright ASTM.

Caoutchouc isobutène-isoprène (IIR) — Méthodes d'évaluation

General Information

• Status: Withdrawn
• Publication Date: 04-Jan-2005
• Withdrawal Date: 04-Jan-2005
• ICS: 83.060 - Rubber
• Technical Committee: ISO/TC 45/SC 3 - Raw materials (including latex) for use in the rubber industry
• Drafting Committee: ISO/TC 45/SC 3/WG 5 - Synthetic and reclaimed rubber
• Current Stage: 9599 - Withdrawal of International Standard
• Completion Date: 15-Oct-2014

Relations

• Revised: ISO 2302:2014 - Isobutene-isoprene rubber (IIR) — Evaluation procedure
• Effective Date: 21-Dec-2013
• Revises: ISO 2302:1995 - Isobutene-isoprene rubber (IIR) — Evaluation procedures
• Effective Date: 15-Apr-2008

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 2302
Fifth edition
2005-01-15
Corrected version
2007-03-01

Isobutene-isoprene rubber (IIR) —
Evaluation procedures
Caoutchouc isobutène-isoprène (IIR) — Méthodes d'évaluation




Reference number
ISO 2302:2005(E)
©
ISO 2005

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ISO 2302:2005(E)
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ii © ISO 2005 – All rights reserved

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ISO 2302:2005(E)
Contents Page
Foreword. iv
1 Scope . 1
2 Normative references . 1
3 Sampling and further preparative procedures . 2
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 of isobutene-isoprene rubbers. 2
5.1 Standard test formulation . 2
5.2 Procedure . 3
6 Evaluation of vulcanization characteristics by a curemeter test. 6
6.1 Using oscillating-disc curemeter . 6
6.2 Using rotorless curemeter . 7
7 Evaluation of tensile stress-strain properties of vulcanized test mixes. 7
8 Precision. 7
8.1 General. 7
8.2 Precision details . 7
8.3 Precision results. 8
9 Test report . 8
Bibliography . 10

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ISO 2302:2005(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 2302 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 2302:1995), which has been technically revised.
The precision data in this edition have been taken, with permission of ASTM, from ASTM D 3188-95,
Standard Test Methods for Rubber — Evaluation of IIR (Isobutene-Isoprene Rubber), copyright ASTM.
In this corrected version of ISO 2302:2005, the reference in the Bibliography to ASTM D 3188-95 has been
transferred to Clause 1.

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INTERNATIONAL STANDARD ISO 2302:2005(E)

Isobutene-isoprene rubber (IIR) — Evaluation procedures
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;
 standardized materials, a standardized test formulation, equipment and processing methods for
evaluating the vulcanization characteristics of all types of isobutene-isoprene rubber (IIR).
The precision data in this International Standard have been taken, with permission of ASTM, from
ASTM D 3188-95, Standard Test Methods for Rubber — Evaluation of IIR (Isobutene-Isoprene Rubber),
copyright ASTM.
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 247:1990, Rubber — Determination of ash
ISO 248, Rubbers, raw — Determination of volatile-matter content
ISO 289-1, Rubber, unvulcanized — Determinations using a shearing-disc viscometer — Part 1:
Determination of Mooney viscosity
ISO 1795:2000, Rubber, raw natural and raw synthetic — Sampling and further preparative procedures
ISO 2393:1994, 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
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ISO 2302:2005(E)
3 Sampling and further preparative procedures
A laboratory sample of approximately 1,5 kg shall be taken in accordance with the method described in
ISO 1795. Preparation of the sample shall be in accordance with ISO 1795.
4 Physical and chemical tests on raw rubber
4.1 Mooney viscosity
Prepare a test portion in accordance with the preferred procedure in ISO 1795, i.e. without milling, cutting the
test portion directly from the laboratory sample. The test portion shall be as free as possible from air and
pockets that may trap air against the rotor and die surface.
If agreed between the interested parties or if the condition of the sample (e.g. excessive porosity) makes
milling necessary, it shall be performed in accordance with ISO 1795:2000, Subclause 8.3.2.2, paragraphs 1
and 2.
Determine the Mooney viscosity in accordance with ISO 289-1 on this test portion, as ML(1+8) at 125 °C.
4.2 Volatile matter
Determine the volatile-matter content by the hot-mill method or by the oven method as specified in ISO 248.
4.3 Ash
Determine the ash in accordance with either method A or method B of ISO 247:1990.
5 Preparation of test mixes for evaluation of isobutene-isoprene rubbers
5.1 Standard test formulation
The standard test formulation is given in Table 1. The materials shall be national or international standard
reference materials (or as agreed by the interested parties).
Table 1 — Standard test formulation
Material Parts by mass
Isobutene-isoprene rubber (IIR) 100,00

a
1,00
Stearic acid
b
50,00
Industry reference black
a
3,00
Zinc oxide
a
1,75
Sulfur
a
1,00
Tetramethylthiuram disulfide(TMTD)
Total 156,75
a
Powder materials shall be used (standard curing ingredients used in the industry).
b
The current industry reference black shall be used.

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ISO 2302:2005(E)
5.2 Procedure
5.2.1 Equipment and procedure
The equipment and procedure for the preparation, mixing and vulcanization shall be in accordance with
ISO 2393:1994, Clauses 6, 7, 8 and 9.
5.2.2 Mixing procedures
5.2.2.1 General
Three alternative mixing procedures are specified:
 Method A: mixing with a laboratory mill;
 Method B: mixing with a miniature internal mixer (MIM);
 Method C: mixing with an internal mixer.
NOTE These procedures may not give identical results.
5.2.2.2 Method A — Mixing with a laboratory mill
The standard laboratory mill-batch mass, in grams, shall be based on four times the formulation mass (i.e.
4 × 156,75 g = 627 g). The surface temperature of the rolls shall be maintained at 45 °C ± 5 °C throughout the
mixing.
A good rolling bank at the nip of the rolls shall be maintained during mixing. If this is not obtained with the nip
settings specified hereunder, small adjustments to the mill openings may be necessary.
A mill batch mass based on two times the formulation mass may also be used, but, in this case, more
adjustments to the mill openings will be necessary.
Duration Cumulative
time
(min) (min)
a) Band the rubber with the mill opening set at 0,65 mm. 1,0 1,0
b) Mix the carbon black and the stearic acid and add evenly across the mill rolls10,0 11,0
at a uniform rate. Increase the mill opening at intervals to maintain a constant
rolling bank. When all the carbon black has been incorporated, make a 3/4 cut
from each side.
Do not cut the batch while free carbon black is evident in the bank or on the
milling surface. Be certain to return to the batch any materials that drop
through the mill.
c) Add the zinc oxide, the sulfur and the TMTD. 3,0 14,0
d) Make three alternating 3/4 cuts from each side. 2,0 16,0
e) Cut the batch from the mill. Set the mill opening to 0,8 mm and pass the rolled 2,0 18,0
batch endwise through the mill six times.
f) Sheet the batch to approximately 6 mm and check-weigh the batch (see ISO 2393). If the mass of the
+ 0,5
batch differs from the theoretical value b
...