ISO 00188-2023

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INTERNATIONAL ISO

STANDARD 188

Sixth edition
2023-03

Rubber, vulcanized or
thermoplastic — Accelerated
ageing and heat resistance tests
Caoutchouc vulcanisé ou thermoplastique — Essais de résistance au
vieillissement accéléré et à la chaleur

Reference number
ISO 188:2023(E)

© ISO 2023
ISO 188:2023(E)

COPYRIGHT PROTECTED DOCUMENT


© ISO 2023
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of
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ii © ISO 2023 – All rights reserved
ISO 188:2023(E)
Published in Switzerland

© ISO 2023
ISO 188:2023(E)

Contents Page

Foreword........................................................................................................................................................................ iv
Introduction.................................................................................................................................................................... v
1 Scope................................................................................................................................................................... 1
2 Normative references.................................................................................................................................... 1
3 Terms and definitions......................................................................................................................1
4 Principle............................................................................................................................................................. 1
4.1 General......................................................................................................................................1
4.2 Accelerated ageing test.......................................................................................................1
4.3 Heat resistance test..............................................................................................................2
5 Apparatus.......................................................................................................................................................... 2
6 Calibration......................................................................................................................................................... 6
7 Test pieces......................................................................................................................................................... 6
8 Time interval between vulcanization and testing...............................................................................7
9 Ageing conditions (duration and temperature)...................................................................................7
9.1 General.....................................................................................................................................7
9.2 Accelerated ageing test.......................................................................................................7
9.3 Heat resistance test..............................................................................................................7
10 Procedure.......................................................................................................................................................... 8
11 Expression of results...................................................................................................................................... 8
12 Precision............................................................................................................................................................ 8
13 Test report......................................................................................................................................................... 8
Annex A (informative) Determination of the air speed inside the ovens with forced air
circulation
............................................................................................................................................................................
10
Annex B (informative) Precision......................................................................................................................... 12
Annex C (informative) Guidance for using precision results....................................................................19
Annex D (normative) Calibration schedule..................................................................................................... 20
Bibliography................................................................................................................................................................ 22

© ISO 2023 – All rights reserved iii


ISO 188:2023(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 45, Rubber and rubber
products, Subcommittee SC 2, Testing and analysis.
This sixth edition cancels and replaces the fifth edition (ISO 188:2011), which has been
technically
revised.
The main changes are as follows:
— add oven type with a forced air circulation and high air speed/air exchange rate;
— editorial changes for better understanding.
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.

iv © ISO 2023 – All rights reserved


ISO 188:2023(E)

Introduction
Accelerated ageing and heat resistance tests are used to determine the change of
defined properties of rubber and thermoplastic elastomers over a specified period.
These properties are compared before and after the accelerated ageing and heat
resistance tests.
In accelerated ageing, the rubber is exposed to an elevated temperature with the
intention to simulate the effect of natural ageing in a shorter time. The degree of
acceleration depends on the tested material as well as to the property being
evaluated.
In the case of heat resistance tests, the rubber is exposed to prolonged periods at the
operation temperature of the material.
Two types of ovens are specified in this document, cell ovens and cabinet ovens.
Cabinet ovens can be of four types as described in Clause 5.
The duration, temperature, and atmosphere to which the test pieces are exposed and
the type of oven to use depends on the purpose of the test and the type of polymer.
The change of properties not only depends on the temperature but can also depend on
the air speed. Consequently, even tests at the same temperature but at different air
speed (different ovens) may give different results.
Consequences of these effects are
a) accelerated ageing is only a simulation of the natural ageing and can therefore
produce different
results.
b) If different materials are compared, it is recommended to perform the accelerated
ageing tests at more than one elevated temperature as different rubbers might
show a different temperature behaviour (change of properties) at certain operation
temperatures.
c) It is important to determine the properties of the rubber for the accelerated ageing
test, which are used for the intended material application. Only these properties
should be used for the evaluation of the test results. If these properties give a
different ranking of the materials tested, it is recommended to agree on a lead
property for evaluation. It is also recommended, that all evaluated properties are
measured according to an international standard or an equivalent test procedure.
Air-oven ageing should not be used to simulate natural ageing under stress (bent or
stretched test pieces) and the presence of light or ozone.
To estimate lifetime or maximum temperature of use, tests can be performed at
several temperatures and the results can be evaluated by using an Arrhenius plot or
the Williams Landel Ferry (WLF) equation as described in ISO 11346.

© ISO 2023 – All rights reserved v


INTERNATIONAL STANDARD ISO 188:2023(E)

Rubber, vulcanized or thermoplastic — Accelerated


ageing and heat resistance tests
WARNING — Persons using this document should be familiar with normal laboratory practice.
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
determine the applicability of any other restrictions.

1 Scope
This document specifies accelerated ageing or heat resistance tests on vulcanized or
thermoplastic rubbers/thermoplastic elastomers. Four methods are possible, they are
detailed in Clause 5.

2 Normative references
The following documents are referred to in the text in such a way that some or all of
their content constitutes requirements 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 18899, Rubber — Guide to the calibration of test equipment
ISO 23529, Rubber — General procedures for preparing and conditioning test pieces for physical test
methods

3 Terms and definitions


No terms and definitions are listed in this document.
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/

4 Principle

4.1 General
Test pieces are exposed to air at a given elevated temperature and at atmospheric
pressure with controlled conditions of air circulation.
Physical properties are measured before and after exposure and the results compared.
The physical properties that are important for the intended application of the material
should be used to determine the effects of exposure. In the absence of any indication
of these properties, it is recommended that tensile strength, stress at intermediate
elongation, elongation at break (in accordance with ISO 37) and hardness (in
accordance with ISO 48-2) are measured.

4.2 Accelerated ageing test


© ISO 2023 – All rights reserved 1
ISO 188:2023(E)
Test pieces are subjected to a higher temperature than the rubber would experience
in its intended application to simulate the effects of natural ageing in a shorter time.

2 © ISO 2023 – All rights reserved


INTERNATIONAL STANDARD ISO 188:2023(E)

4.3 Heat resistance test


Test pieces are subjected to the temperature they would experience in their intended
application to gain information about their service performance.

5 Apparatus

5.1 Air oven.

The oven shall be of such a size that the total volume of the test pieces does not
exceed 10 % of the free space in the oven. Provision shall be made for suspending test
pieces so that they are at least 10 mm from each other and, in cabinet ovens and
ovens with forced air circulation, at least 50 mm from the sides of the oven.
The temperature of the oven shall be controlled so that the temperature of the test
pieces is kept within the specified tolerance for the specified ageing temperature (see
Clause 9) for the whole ageing period. A temperature sensor shall be placed inside the
heating chamber close to the test pieces to indicate the actual ageing temperature.
No copper or copper alloys shall be used in the construction of the heating chamber.
Method A: using a cell or cabinet oven with low air speed, laminar flow of air past the
stationary test pieces and air exchange rate between 3 and 10 changes per hour.
Method B: using a cabinet oven with high air speed, laminar flow of air past the test
pieces and air exchange rate between 3 and 10 changes per hour.
Method C: using a cabinet oven with high air speed, turbulent flow of air past the test
pieces, rotation of the test piece carrier and air exchange rate between 3 and 10
changes per hour.
For method A, B and method C, provision shall be made for a slow flow of air through
the oven of not less than three and not more than ten air changes per hour.
Method D: Using a cabinet oven with high air speed, turbulent flow of air past the
stationary test pieces and air exchange rate greater than 30 changes per hour.
For method D, an air flow between 0,25 to 3,0 m/s is necessary as well as an air
exchange rate above 30 changes per hour.
Depending on the influence of the air speed/air exchange on the results, to get
comparable results always the same method should be used to compare the ageing
behaviour of different materials.
The incoming air in the oven should be heated up to the temperature within a ±1 °C
tolerance before reaching the test pieces.
The ventilation (or air change rate) can be determined by measuring the volume of the
oven chamber and the flow of air through the chamber.
NOTE To ensure a good precision when doing ageing and heat resistance tests, it is very
important to keep the temperature uniform and stable within the oven and during the test.
Therefore, it is necessary and to verify that the oven used, is within the temperature limits at
all test piece locations and during the complete testing time. Increasing the air speed in the
oven improves temperature homogeneity. However, air circulation in the oven and ventilation
influences the ageing results. With a low air speed, accumulation of degradation products and
evaporated ingredients, as well as oxygen depletion, can happen. A high air speed may
increase the rate of deterioration, due to increased oxidation and migration of plasticizers and
antioxidants.

NOTE Method D oven can be used for short term testing up to 168 h.

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ISO 188:2023(E)

5.2 Method A cell oven.

The oven shall consist of one or more vertical cylindrical cells having a minimum
height of 300 mm. The cells shall be surrounded by a thermostatically controlled good
heat transfer medium (aluminium block, liquid bath, or saturated vapour). Air passing
through one cell shall not enter other cells.
Provision shall be made for a slow flow of air through the cell. The air speed shall
depend on the air change rate only.

5.3 Method A cabinet oven.

The oven should consist of a single chamber without separating walls. Provision shall
be made for a slow flow of air through the oven. The air speed shall depend on the air
change rate only, and no fans are allowed inside the test chamber.

5.4 Method B, C and D cabinet oven with forced air circulation.

One of the following three types shall be used:


a) Method B cabinet oven with laminar air flow and forced air circulation (see Figure 1).
The air flow through the heating chamber shall be as uniform and laminar as
possible. The test pieces shall be placed so that the smallest surface faces the air
flow to avoid disrupting the air flow. The air speed shall be between 0,5 m/s and
1,5 m/s.
The air speed near the test pieces can be measured by means of an anemometer.

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ISO 188:2023(E)

Key
1 test pieces
2 heating element
3 air blower
a Air inlet.

b Air outlet.

c Laminar air flow.

Figure 1 — Example of method B cabinet oven with laminar air flow

b) Method C cabinet oven with forced air circulation, turbulent air flow and provision
for rotating the test piece carrier (see Figure 2).
The air entering from a side-wall air-inlet into the heating chamber is turbulent
around the test pieces, which are suspended on a carrier rotating at a speed of five
to ten rotations per minute so that they are exposed to the heating air as uniformly
as possible. The average air speed shall be 0,5 m/s ± 0,25 m/s.
The average air speed near the test pieces can be calculated from measurements
made with an anemometer at nine different positions (see Figure A.1). A suitable
method of measurement is described in Annex A.

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ISO 188:2023(E)

Key
1 test piece carrier
2 test pieces
3 heating element
4 motor
5 air blower
a Air inlet.

b Air outlet.

c Turbulent air flow.

d Laminar air flow (inlet, outlet and near to wall).

Figure 2 — Example of method C cabinet oven with turbulent air


flow and provision for rotating the test piece carrier

c) Method D cabinet oven with turbulent air flow (see Figure 3).
The air entering from a back-wall air-inlet into the heating chamber is turbulent
around the test pieces, which are suspended inside the oven in such a way that
they are exposed to the heating air as uniformly as possible. The average air speed
shall be between 0,25 m/s and 3,0 m/s.
The average air speed near the test pieces can be calculated from measurements
made with an anemometer at nine different positions (see Figure A.1). A suitable
method of measurement is described in Annex A.

© ISO 2023 – All rights reserved 5


ISO 188:2023(E)

Key
1 test piece carrier
2 test pieces
3 heating element
4 air blower
5 regulator for air exchange rate
a Air inlet.

b Air outlet.

c Turbulent air flow.

Figure 3 — Example of method D cabinet oven with turbulent air flow

NOTE The tolerances for method D are larger which makes it less suitable for exposures longer
than 168 h.

6 Calibration
The test apparatus shall be calibrated in accordance with Annex D.

7 Test pieces
Select and prepare the test pieces necessary for the tests to be carried out, in
accordance with the requirements of ISO 23529.
Only test pieces of the same dimensions, having the same exposed areas shall be
compared with each other. The number of test pieces shall be in accordance with the
International Standard for the appropriate property tests.
The test pieces shall be capable of being identified after the test, for example by
marking. Any method can be used that can withstand the exposure and does not affect
the properties of the test piece or change the air flow.
NOTE Heat resistant tags attached with heat resistant string are satisfactory. Some marking
inks can affect the ageing of the rubber or wear off during exposure.

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ISO 188:2023(E)

Avoid simultaneous heating of different types of compound in the same oven, to


prevent the migration of sulphur, antioxidants, peroxides, or plasticizers. For this
purpose, the use of individual cells is highly recommended. If it is not practicable to
provide equipment with individual cells, it is recommended that only the following
types of material be heated together:
a) polymers of the same general type;
b) vulcanizates containing the same type of accelerator and approximately the same
ratio of sulphur to accelerator;
c) rubbers containing the same type of antioxidant;
d) rubbers containing the same type and amount of plasticizer.

8 Time interval between vulcanization and testing


Unless otherwise specified for technical reasons, the following requirements, in
accordance with ISO 23529 for time intervals, shall be observed.
For test purposes in cases of arbitration, the minimum time shall be 72 h.

9 Ageing conditions (duration and temperature)

9.1 General
Unless otherwise specified for technical reasons, the following requirements, in
accordance with ISO 23529 for ageing time and temperatures, shall be observed.
Different type of rubbers and thermoplastic elastomers may require different periods
of testing to observe any changes in properties. The ageing duration should not lead to
a damage of the test pieces so that it is impossible to measure the required properties.
The use of high ageing temperatures may cause different degradation mechanisms
than at operating temperatures, which invalidates the results.
To get the temperature as accurate as possible a calibrated temperature sensor shall
be placed close to the test pieces and use this to set the oven to the required
temperature. Use the correction factor from the calibration certificate of the oven to
get as close as possible to the true temperature.
For methods A, B and C the ovens shall have a set point resolution of 0,1 °C. For Method
D 1 °C resolution is acceptable.
It is crucial for comparable and reproducible results that the temperature is kept as
stable as possible. Temperature tolerances stated in ISO 23529 are ±1 °C (up to and
including 100 °C) and ±2 °C (125 °C up to and including 300 °C). However, studies
have shown that a 1 °C change in temperature corresponds to a 10 % difference in
ageing time at an Arrhenius factor of 2, or 15 % at a factor of 2,5. This means that two
laboratories carrying out ageing at 125 °C can have ageing times which differ by 60 %
from each other and still be within the specification.

9.2 Accelerated ageing test


If the duration of ageing and the ageing temperature are not in accordance with ISO
23529, they can be agreed between the interested parties based on the product
specification. The ageing shall be performed at atmospheric pressure.

9.3 Heat resistance test


© ISO 2023 – All rights reserved 7
ISO 188:2023(E)
If the duration of ageing and the ageing temperature are not in accordance with ISO
23529, they can be agreed between the interested parties based on the product
specification. The temperature shall

8 © ISO 2023 – All rights reserved


ISO 188:2023(E)

be representative of the operating temperature and the heating shall be performed at


atmospheric
pressure.

10 Procedure
Heat the oven to the required temperature and place the test pieces in it. When using
a cell-type oven, only one rubber or compound shall be placed in each cell. The test
pieces shall be free from strain, freely exposed to air on all sides and not exposed to
light.
When the heating period is complete, remove the test pieces from the oven and
condition them for no less than 16 h and no more than 6 days, strain-free in the
atmosphere as required in the appropriate test method for the property being
measured.

11 Expression of results
The results shall be expressed in accordance with the International Standard for the
appropriate property tests.
The test results for both the unaged and the aged test pieces shall be reported
together, as well as the percentage change in the value of the property measured as
calculated by Formula (1):
xa  x0
100 (1)
x0
where

x0 is the value of the property before ageing;

xa is the value of the property after ageing.


Exception: express changes in hardness always as the difference xa − x0.
NOTE The rubber industry uses the term equation for the relationships herein termed
formula. The term formula is used to describe the table of ingredients in a rubber compound.

12 Precision
See Annex B.

13 Test report
The test report shall include the following information:
a) a reference to this document, i.e. ISO 188:2023;
b) the sample details:
1) a full description of the sample and its origin,
2) details of the compound and its condition of cure, if known,
3) the time interval between forming and testing,
4) the method used to prepare the test pieces (e.g. moulding, cutting from the
sample) and the location where the test pieces were taken from the sample;
© ISO 2023 – All rights reserved 9
ISO 188:2023(E)
c) the test method:
1) a reference to this document,

1 © ISO 2023 – All rights reserved


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ISO 188:2023(E)

2) the method used (A, B, C or D),


3) the properties determined and the type of test piece used;
d) the test details:
1) the type of oven used,
2) the number of test pieces used,
3) whether accelerated ageing or a heat resistance test was carried out,
4) the temperature and duration of ageing,
5) details of any procedures not specified in this document;
e) the test results:
1) the individual values before and after ageing, expressed in accordance with the
International Standards for the appropriate property tests,
2) the changes in the property values, expressed as a percentage or, for hardness,
as the difference between the values;
f) the date of the test.

© ISO 2023 – All rights reserved 11


ISO 188:2023(E)

Annex A
(informative)

Determination of the air speed inside the ovens with forced air
circulation

A.1 Scope
This annex describes a method for determining the air speed method B, method C and
method D type
ovens.

A.2 Apparatus
A portable anemometer can be used.

A.3 Procedure

A.3.1 The air speed should be measured at nine positions at the level of the centre of
a suspended test piece. For this purpose, prepare an at least 2 mm thick transparent
plastic plate made of PVC [(poly(vinyl chloride)] or PMMA [(poly(methyl methacrylate)],
of the same size as the door of the oven chamber. Drill three holes into the plate, each
big enough to allow an anemometer to be inserted through it, two located 70 mm from
the left and right edge, respectively, and one centred between the other two (see
Figure A.1).

A.3.2 The measurement of the air speed should be carried out at a standard laboratory
temperature.

A.3.3 Open the door of the chamber and fix the plastic plate in the door opening.
Make sure that the oven can be operated even the door is open.

A.3.4 Operate the oven and insert the anemometer sensor through each aperture.
Measure the air speed at all nine positions as indicated in Figure A.1. Keep the gap
between the plate and the handle of the anemometer airtight. The two not used
apertures shall be closed during measurement.

A.3.5 For method D type ovens make sure that the anemometer is inserted in the
direction of the main airflow (back to front) of the oven.

A.3.6 Read the maximum value of the air speed at each position to avoid any effect
due to the directionality of the sensor.

A.4 Calculation of result

A.4.1 Calculate the mean value of the air speed measured at the nine measurement positions.

1 © ISO 2023 – All rights reserved


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ISO 188:2023(E)

Dimensions in millimetres

Key
1 plastic plate
2 aperture
3 door opening
4 measurement position

Figure A.1 — Positions for measuring air speed inside the oven

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ISO 188:2023(E)

Annex B
(informative)

Precision

B.1 General
Two interlaboratory test programmes (ITPs) and the precision calculations to express
repeatability and reproducibility were performed in accordance with ISO/TR 92721).
The first ITP was organized in 1996 and the results analysed in 1997, and the second
one in 2005. Consult ISO 19983 for precision concepts and nomenclature. Annex C gives
guidance on the use of repeatability and reproducibility results.

B.2 Precision details of the first ITP

B.2.1 Prepared test pieces were sent out to all participating laboratories using four
compounds (of types NR, NBR, EPDM and AEM). Ageing was carried out by both
method A and method B.

The ageing time was 168 h for all compounds, at 70 °C for NR, 100 °C for NBR, 125
°C for EPDM and 150 °C for AEM.

B.2.2 A total of 16 laboratories participated in this ITP. Eleven of the laboratories


carried out the ageing by method A and ten laboratories by method B. Five of the
laboratories used both method A and
B. For certain of the tests carried out after ageing, values were missing from the
compiled data, and for these tests fewer than these numbers of laboratories were
involved. The actual number for each test is listed in the precision tables.

B.2.3 The hardness was measured in accordance with ISO 48-2, method M, before
and after ageing. The three tensile strength properties were measured in accordance
with ISO 37 on five test pieces before and after ageing. Type 1 and type 2 dumb-bell
test pieces were used.

B.2.4 The precision determined in this ITP is a type 1 precision, i.e. fully prepared
test pieces were submitted to all laboratories. The precision is also an intermediate-
term or intermediate time period precision, with a time of two to three weeks between
the two replicate determinations. This is in distinction to the more usual day 1 to day 2
replication with a few days between the determinations.

The symbols used in the tables are as follows:

r repeatability, in measurement units;

(r) repeatability, expressed as a percentage of the average;

R reproducibility, in measurement units;

(R) reproducibility, expressed as a percentage of the average.


(r) and (R) have only been calculated for all the materials together.

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ISO 188:2023(E)

1) Withdrawn and replaced by ISO 19983.

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ISO 188:2023(E)

B.3 Precision results from the first ITP

B.3.1 The precision results are given in Tables B.1 to B.4 for method A (low air speed)
and in Tables B.5 to B.8 for method B (high air speed). In these tables, no values of the
relative precision (r) and (R) are given for the individual materials because many of the
mean values of the performance parameters are near zero and this gives very large (r)
and (R) values that have little meaning. The tables do give a mean value (similar but
not equal to a pooled value) for all four materials together. These overall means are
useful in comparing the relative precision of the four types of test performed. The
relative precision for these overall means enables the two methods (A and B) to be
compared.

B.3.2 On reviewing the tables, it will be observed that there is only a small difference
between the repeatability r and the reproducibility R, and in several cases the two are
equal. This phenomenon has been observed in the previous edition of this document
ageing-precision testing. This demonstrates that a very large component of the
variation observed in this type of testing is not due to differences between laboratories
but is due to some inherent source of variation that is just as likely to occur “within” a
laboratory as on a “between”-laboratory basis. This unknown source is connected with
the ageing process.

Table B.1 — Ageing precision determined from change in hardness (IRHD)


(method A: low air speed)
Mean change Within laboratory Between laboratories Number of
Material
% r (r) R (R) labs
NR 3,1 3,10 3,63 11
NBR 4,4 2,08 3,68 11
EPDM 22,0 5,50 10,30 11
AEM 3,9 6,78 7,78 11
Absolute mean 8,3 4,4 6,3
(without regard to
sign)
Relative precision 53 76

Table B.2 — Ageing precision determined from change in tensile strength (TSb)
(method A: low air speed)
Mean change Within laboratory Between laboratories Number of
Material
% r (r) R (R) labs
NR −8,7 8,43 9,34 11
NBR 6,6 9,26 11,83 11
EPDM 4,1 8,24 14,92 11
AEM −9,3 8,13 10,71 11
Absolute mean (without 7,2 8,5 11,7
re- gard to sign)
Relative precision 118 162

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ISO 188:2023(E)

Table B.3 — Ageing precision determined from change in stress at 100 % elongation (S100)
(method A: low air speed)
Mean change Within laboratory Between laboratories Number of
Material
% r (r) R (R) labs
NR 25,2 13,4 16,0 11
NBR 38,4 26,8 26,8 11
EPDM 247,1 78,9 135,3 11
AEM 0,4 15,4 22,7 11
Absolute mean 77,7 33,6 50,2
(without regard to
sign)
Relative precision 43 65

Table B.4 — Ageing precision determined from change in elongation at break (Eb)
(method A: low air speed)
Mean change Within laboratory Between laboratories Number of
Material
% r (r) R (R) labs
NR −13,3 10,36 10,36 11
NBR −17,7 14,00 14,00 11
EPDM −66,5 4,85 7,44 11
AEM 0,8 7,72 17,12 11
Absolute mean (without 24,2 9,2 12,2
re- gard to sign)
Relative precision 38 50

Table B.5 — Ageing precision determined from change in hardness (IRHD)


(method B: high air speed)
Mean change Within laboratory Between laboratories Number of
Material
% r (r) R (R) labs
NR 4,1 5,14 5,14 10
NBR 8,7 3,20 5,29 10
EPDM 35,9 3,89 9,67 10
AEM 8,0 5,04 8,00 10
Absolute mean 14,2 4,3 7,0
(without re- gard to
sign)
Relative precision 30 49

Table B.6 — Ageing precision determined from change in tensile strength (TSb)
(method B: high air speed)
Mean change Within laboratory Between laboratories Number of
Material
% r (r) R (R) labs
NR −8,5 7,07 9,23 10
NBR 12,3 12,88 12,88 10
EPDM 7,9 11,88 11,88 10
AEM −4,4 8,93 10,73 10

© ISO 2023 – All rights reserved 17


ISO 188:2023(E)

Table B.6 (continued)


Mean change Within laboratory Between laboratories Number of
Material
% r (r) R (R) labs
Absolute mean 8,3 10,2 11,2
(without re- gard to
sign)
122 134
Relative precision

Table B.7 — Ageing precision determined from change in stress at 100 % elongation (S100)
(method B: high air speed)
Mean change Within laboratory Between laboratories Number of
Material
% r (r) R (R) labs
NR 24,3 10,3 14,0 10
NBR 54,4 25,0 26,7 10
EPDM 392,1 62,5 194,0 10
AEM 19,3 12,0 14,1 10
Absolute mean 122,5 27,4 62,2
(without re- gard to
sign)
Relative precision 22 51

Table B.8 — Ageing precision determined from change in elongation at break (Eb)
(method B: high air speed)
Mean
Within laboratory Between laboratories Number of
Material change
labs
% r (r) R (R)
NR −14,8 6,86 9,65 10
NBR −19,3 9,41 13,14 10
EPDM −73,0 5,76 8,89 10
AEM −3,3 9,39 11,80 10
Absolute mean 27,6 7,9 10,9
(without re- gard to
sign)
Relative precision 29 39

B.4 Precision details of the second ITP

B.4.1 Prepared test pieces were sent out to all participating laboratories using three
compounds (of types of NR, NBR and EPDM). Ageing was carried out in type 1 and
type 2 ovens using method B (method B cabinet ovens and method C cabinet ovens).

The ageing time was 72 h and 168 h for all compounds at 85 °C for NR, 100 °C for NBR
and 125 °C for EPDM.

B.4.2 A total of 11 laboratories participated in this ITP. Five of the laboratories


carried out the ageing in type 1 ovens (method B cabinet ovens) and six laboratories in
type 2 ovens (method C cabinet ovens). The actual number of laboratories for each test
is listed in the precision tables.

B.4.3 The three tensile strength properties were measured in accordance with ISO 37
on five test pieces before and after ageing. Type 1A test pieces were used. Hardness
1 © ISO 2023 – All rights reserved
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ISO 188:2023(E)
was omitted from the analysis because there were insufficient test results.

© ISO 2023 – All rights reserved 19


ISO 188:2023(E)

B.4.4 The precision determined in this ITP is a type 1 precision, i.e. fully prepared
test pieces were submitted to all laboratories. The precision is also an intermediate-
term or intermediate time period precision, with a time of two to three weeks between
the two replicate determinations. This is in distinction to the more usual day 1 to day 2
replication with a few days between the determinations.

The symbols used in Tables B.9 to B.14 are the same as those for the first ITP.

B.5 Precision results from the second ITP

B.5.1 The precision results are given in Tables B.9 to B.11 for type 1 ovens (method B
cabinet ovens) and in Tables B.12 to B.14 for type 2 ovens (method C cabinet ovens).
In these tables, the values for the two ageing times, 72 h and 168 h, are included, but
no values of the relative precision (r) and (R) are given for the individual materials, as
in the first ITP. The relative precision for these overall means enables the two types of
oven to be compared in the same way as in the first ITP.

B.5.2 On reviewing the tables, it can be seen that the type 1 and type 2 ovens
(method B cabinet ovens and method C cabinet ovens) give almost the same precision.
The type 2 oven (method C cabinet oven) in fact gives slightly more uniform ageing and
a slightly larger change in the properties on ageing.

Table B.9 — Ageing precision determined from change in tensile strength (TSb)
(type 1 oven) (method B cabinet oven)
Mean change Within laboratory Between laboratories Number of
Material
% r (r) R (R) labs
NR, 72 h −3,2 4,2 8,7 5
NR, 168 h −11,5 6,7 15,7 5
NBR, 72 h 0,5 6,0 13,8 5
NBR, 168 h −4,0 11,6 11,3 5
EPDM, 72 h −6,0 7,7 10,3 5
EPDM, 168 h −7,8 14,9 19,0 5
Absolute mean 5,5 8,5 13,1
(without regard to
sign)
Relative precision 155 238

Table B.10 — Ageing precision determined from change in stress at 100 % elongation (S100)
(type 1 oven) (method B cabinet oven)
Mean change Within laboratory Between laboratories Number of
Material
% r (r) R (R) labs
NR, 72 h 26,6 30,0 30,8 5
NR, 168 h 45,6 54,1 45,7 5
NBR, 72 h 39,5 7,4 48,5 5
NBR, 168 h 52,1 8,2 59,7 5
EPDM, 72 h 78,3 44,5 58,0 5
EPDM, 168 h 102,5 48,0 78,2 5
Absolute mean 57,4 32,0 53,5
(without regard to
sign)

2 © ISO 2023 – All rights reserved


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ISO 188:2023(E)
Relative precision 56 93

© ISO 2023 – All rights reserved 21


ISO 188:2023(E)

Table B.11 — Ageing precision determined from change in elongation at break (Eb)
(type 1 oven) (method B cabinet oven)
Mean change Within laboratory Between laboratories Number of
Material
% r (r) R (R) labs
NR, 72 h −12,5 11,9 9,6 5
NR, 168 h −19,3 1,4 13,8 5
NBR, 72 h −23,0 4,7 15,6 5
NBR, 168 h −29,3 9,1 13,1 5
EPDM, 72 h −42,8 5,9 4,2 5
EPDM, 168 h −49,3 13,3 11,4 5
Absolute mean 29,4 7,7 11,3
(without re- gard to
sign)
Relative precision 26 38

Table B.12 — Ageing precision determined from change in tensile strength (TSb)
(type 2 oven) (method C cabinet oven)
Mean change Within laboratory Between laboratories Number of
Material
% r (r) R (R) labs
NR, 72 h −4,4 7,5 5,5 6
NR, 168 h −16,1 9,4 9,5 6
NBR, 72 h −6,7 7,8 17,2 6
NBR, 168 h −9,6 7,3 8,2 6
EPDM, 72 h −9,5 7,2 10,3 6
EPDM, 168 h −9,6 12,7 14,0 6
Absolute mean 9,3 8,7 10,8
(without re- gard to
sign)
Relative precision 94 116

Table B.13 — Ageing precision determined from change in stress at 100 % elongation (S100)
(type 2 oven) (method C cabinet oven)
Mean change Within laboratory Between laboratories Number of
Material
% r (r) R (R) labs
NR, 72 h 38,4 31,5 24,5 6
NR, 168 h 59,1 36,7 29,8 6
NBR, 72 h 53,7 10,4 24,7 6
NBR, 168 h 75,0 28,5 28,9 6
EPDM, 72 h 88,2 27,4 32,2 6
EPDM, 168 h 112,1 39,6 59,6 6
Absolute mean 71,1 29,0 33,3
(without re- gard to
sign)
Relative precision 41 47

2 © ISO 2023 – All rights reserved


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ISO 188:2023(E)

Table B.14 — Ageing precision determined from change in elongation at break (Eb)
(type 2 oven) (method C cabinet oven)
Mean change Within laboratory Between laboratories Number of
Material
% r (r) R (R) labs
NR, 72 h −15,6 13,8 10,2 6
NR, 168 h −26,1 13,0 10,2 6
NBR, 72 h −29,6 9,1 12,7 6
NBR, 168 h −36,0 1,6 3,9 6
EPDM, 72 h −47,9 14,5 14,7 6
EPDM, 168 h −53,2 10,4 16,9 6
Absolute mean 34,7 10,4 11,4
(without regard to
sign)
Relative precision 30 33

© ISO 2023 – All rights reserved 23


ISO 188:2023(E)

Annex C
(informative)

Guidance for using precision results

C.1 The general procedure for using precision results is as follows, with the symbol |
x1 − x2| designating a positive difference in any two measurement values (i.e. without
regard to sign).

C.2 Enter the appropriate precision table (for whatever test parameter is being
considered) at an average value (of the measured parameter) nearest to the “test” data
average under consideration. This line will give the applicable r, (r), R or (R) for use in the
decision process.

C.3 With these r and (r) values, the following general repeatability statements may be
used to make
decisions:

a) For an absolute difference: the difference |x1 − x2| between two test (value)
averages, found on nominally identical material test pieces under normal and
correct operation of the test procedure, will exceed the tabulated repeatability r on
average not more than once in twenty cases.
b) For a percentage difference between two test (value) averages: the percentage
difference is given by Formula (C.1):
x1  x2
1 10 (C.1)
 x1  x2 0
2

between two test values, found on nominally identical material test pieces under
normal and correct operation of the test procedure, will exceed the tabulated
repeatability (r) on average not more than once in twenty cases.

C.4 With these R and (R) values, the following general reproducibility statements may
be used to make decisions:

a) For an absolute difference: the absolute difference |x1 − x2| between two
independently measured test (value) averages, found in two laboratories using
normal and correct test procedures on nominally identical material test pieces, will
exceed the tabulated reproducibility R not more than once in twenty cases.
b) For a percentage difference between two test (value) averages: the percentage
difference is given by Formula (C.2):
x1  x2
1 100 (C.2)
 x1  x2
2

between two independently measured test (value) averages, found in two
laboratories using normal and correct test procedures on nominally identical
material test pieces, will exceed the tabulated reproducibility (R) not more than
once in twenty cases.

2 © ISO 2023 – All rights reserved


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ISO 188:2023(E)

Annex D
(normative)

Calibration schedule

D.1 Inspection
Before any calibration is conducted, the condition of the items to be calibrated shall be
determined and documented in a calibration report or certificate. It shall be indicated
whether calibration is carried out before the first operation or after a repair or
correction of the item.
It shall be insured that the item is generally suitable for the intended purpose,
including all needed specifications even they are not necessary for calibration. If such
parameters can change, the need for periodic checks shall be included in the detailed
calibration procedures.

D.2 Schedule
Verification/calibration of the test device is a mandatory part of this document. The
frequency of calibration and procedures used are at the discretion of the individual
laboratory, unless otherwise stated, using ISO 18899 as a guide.
The calibration schedule given in Table D.1 has been compiled by listing all the
parameters given in the test method along with the specified requirement. A
parameter and requirement can relate to the main test device, to part of this device or
to an additional device required for the test.
For each parameter, a calibration procedure is given with reference to ISO 18899, to
another publication or to a procedure specific to the detailed test method. If a more
specific or detailed calibration procedure is available than given in ISO 18899 it shall
be used in preference.
The checking frequency for each parameter is indicated by a code-letter. The code-
letters used in the calibration schedule are:

P particular procedure;

C requirement to be confirmed, but not measured;

N initial check only;

S standard interval as given in ISO 18899;

U in use.

© ISO 2023 – All rights reserved 25


ISO 188:2023(E)

Table D.1 — Calibration frequency schedule


Clause or Verification
Parameter Requirement subclause in frequency Notes
ISO 18899:2013 guide
Oven volume: Sample Such that volume of C U
Vol- ume relationship test piece does not
exceed 10 % of free
space
Provision for suspending At least 10 mm apart 15.2 U
test pieces and (for cabinet and
forced air circu- lation
ovens) at least 50 mm
from sides
Temperature Within tolerances 18 S
specified (procedure B)
in Clause 8
Material of oven No copper or copper C N
chamber alloys used in
construction of heat- ing
chamber
Air flow Between 3 and 10 16.3 S
changes per hour
(method A, B, C)
>30 changes per hour
(Meth- od D)
Method A cell oven
Height 300 mm minimum 15.2 N
Air speed Shall depend only on C
exchange rate
Design C N
Cells surrounded by good
heat transfer medium
and air pass- ing through N
one cell shall not enter
other cells
Method A cabinet oven No fans in heating C N
chamber
Method B, C, D cabinet See Annex A
oven with forced air for a
circulation method of
See 5.4 C N
verification
Layout S
0,5 m/s to 1,5 P
Air speed
m/s (method B)
or
0,5 ± 0,25 m/s (method
C) or 0,25 m/s to 3,0 m/s
(method D)

In addition to the items listed in Table D.1, the use of the following elements is implied,
all of which shall be calibrated in accordance with ISO 18899:
— a timer;
— a thermometer for monitoring the conditioning and test temperatures.

2 © ISO 2023 – All rights reserved


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ISO 188:2023(E)

Bibliography

[1] ISO 37, Rubber, vulcanized or thermoplastic — Determination of tensile stress-strain properties
[2] ISO 48-2, Rubber, vulcanized or thermoplastic — Determination of hardness — Part 2: Hardness
between 10 IRHD and 100 IRHD
[3] ISO/TR 9272, Rubber and rubber products — Determination of precision for test
method standards2)
[4] ISO 11346, Rubber, vulcanized or thermoplastic — Estimation of life-time and
maximum temperature of use
[5] ISO 19983, Rubber — Determination of precision of test methods

2) Withdrawn and replaced by ISO 19983.

© ISO 2023 – All rights reserved 27


ISO 188:2023(E)

2 © ISO 2023 – All rights reserved


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ICS 83.060
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ISO 188:2023(E)
© ISO 2023 – All rights reserved

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