0% found this document useful (0 votes)
41 views

ISO 188

ISO 188:2023 outlines the procedures for accelerated ageing and heat resistance tests for vulcanized or thermoplastic rubber, detailing methods, apparatus, and testing conditions. The document emphasizes the importance of controlled temperature, air circulation, and the properties to be measured before and after testing. This sixth edition updates previous standards and includes new oven types and editorial improvements for clarity.

Uploaded by

Michael Kessler
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
0% found this document useful (0 votes)
41 views

ISO 188

ISO 188:2023 outlines the procedures for accelerated ageing and heat resistance tests for vulcanized or thermoplastic rubber, detailing methods, apparatus, and testing conditions. The document emphasizes the importance of controlled temperature, air circulation, and the properties to be measured before and after testing. This sixth edition updates previous standards and includes new oven types and editorial improvements for clarity.

Uploaded by

Michael Kessler
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
You are on page 1/ 30

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 this publication may
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: [email protected]
Website: www.iso.org
Published in Switzerland

ii  © ISO 2023 – All rights reserved



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://​w ww​.iso​.org/​obp
— IEC Electropedia: available at https://​w ww​.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


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.

© ISO 2023 – All rights reserved  1


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.

2  © ISO 2023 – All rights reserved



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.

© ISO 2023 – All rights reserved  3



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.

4  © ISO 2023 – All rights reserved



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.

6  © ISO 2023 – All rights reserved



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


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

© ISO 2023 – All rights reserved  7



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):
x a − 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;
c) the test method:
1) a reference to this document,

8  © ISO 2023 – All rights reserved



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  9



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.

10  © ISO 2023 – All rights reserved



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

© ISO 2023 – All rights reserved  11



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.

1)    Withdrawn and replaced by ISO 19983.

12  © ISO 2023 – All rights reserved



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 (without 8,3 4,4 6,3
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 re- 7,2 8,5 11,7
gard to sign)
Relative precision 118 162

© ISO 2023 – All rights reserved  13



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 (without 77,7 33,6 50,2
regard to sign)
Relative precision 43 65

Table B.4 — Ageing precision determined from change in elongation at break (E b)


(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 re- 24,2 9,2 12,2
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 (without re- 14,2 4,3 7,0
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

14  © ISO 2023 – All rights reserved



ISO 188:2023(E)

Table B.6 (continued)


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

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 (without re- 122,5 27,4 62,2
gard to sign)
Relative precision 22 51

Table B.8 — Ageing precision determined from change in elongation at break (E b)


(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 (without re- 27,6 7,9 10,9
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 was omitted from the analysis
because there were insufficient test results.

© ISO 2023 – All rights reserved  15



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 (without 5,5 8,5 13,1
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 (without 57,4 32,0 53,5
regard to sign)
Relative precision 56 93

16  © ISO 2023 – All rights reserved



ISO 188:2023(E)

Table B.11 — Ageing precision determined from change in elongation at break (E b)


(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 (without re- 29,4 7,7 11,3
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 (without re- 9,3 8,7 10,8
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 (without re- 71,1 29,0 33,3
gard to sign)
Relative precision 41 47

© ISO 2023 – All rights reserved  17



ISO 188:2023(E)

Table B.14 — Ageing precision determined from change in elongation at break (E b)


(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 (without 34,7 10,4 11,4
regard to sign)
Relative precision 30 33

18  © ISO 2023 – All rights reserved



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 − x 2
× 100 (C.1)
1
( x1 + x 2 )
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 − x 2
× 100 (C.2)
1
( x1 + x 2 )
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.

© ISO 2023 – All rights reserved  19



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.

20  © ISO 2023 – All rights reserved



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 Vol- Such that volume of test C U
ume relationship piece does not exceed 10 %
of free space
Provision for suspending At least 10 mm apart and (for 15.2 U
test pieces cabinet and forced air circu-
lation ovens) at least 50 mm
from sides
Temperature Within tolerances specified 18 S
in Clause 8 (procedure B)
Material of oven chamber No copper or copper alloys C N
used in construction of heat-
ing chamber
Air flow Between 3 and 10 changes 16.3 S
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 exchange C N
rate
      Design C N
Cells surrounded by good heat
transfer medium and air pass-
ing through one cell shall not
enter other cells
Method A cabinet oven No fans in heating chamber C N
Method B, C, D cabinet oven See Annex A
with forced air circulation for a method
of verification
      Layout See 5.4 C N
      Air speed 0,5 m/s to 1,5 m/s P 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.

© ISO 2023 – All rights reserved  21



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.

22  © ISO 2023 – All rights reserved



ISO 188:2023(E)

ICS 83.060
Price based on 22 pages

© ISO 2023 – All rights reserved 

You might also like