Iso - 815-1 (2019)
Iso - 815-1 (2019)
Iso - 815-1 (2019)
STANDARD 815-1
Third edition
2019-11
Rubber, vulcanized or
thermoplastic — Determination of
compression set —
Part 1:
At ambient or elevated temperatures
Caoutchouc vulcanisé ou thermoplastique — Détermination de la
déformation rémanente après compression —
Partie 1: À températures ambiantes ou élevées
Reference number
ISO 815-1:2019(E)
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ISO 815-1:2019(E)
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ISO 815-1:2019(E)
Contents Page
Foreword......................................................................................................................................................................................................................................... iv
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Terms and definitions...................................................................................................................................................................................... 2
4 Principle......................................................................................................................................................................................................................... 2
5 Apparatus...................................................................................................................................................................................................................... 2
6 Calibration................................................................................................................................................................................................................... 4
7 Test pieces.................................................................................................................................................................................................................... 4
7.1 Dimensions.................................................................................................................................................................................................. 4
7.2 Preparation................................................................................................................................................................................................. 5
7.3 Number of test pieces........................................................................................................................................................................ 5
7.4 Time interval between production and testing........................................................................................................... 5
7.5 Conditioning............................................................................................................................................................................................... 5
8 Test conditions........................................................................................................................................................................................................ 6
8.1 Duration of test........................................................................................................................................................................................ 6
8.2 Temperature of test.............................................................................................................................................................................. 6
9 Procedure..................................................................................................................................................................................................................... 6
9.1 Preparation of compression assembly................................................................................................................................ 6
9.2 Thickness measurement.................................................................................................................................................................. 6
9.3 Applying the compression............................................................................................................................................................. 6
9.4 Starting the test....................................................................................................................................................................................... 7
9.5 Terminating the test............................................................................................................................................................................ 7
9.5.1 At ambient temperature............................................................................................................................................. 7
9.5.2 At elevated temperature............................................................................................................................................. 7
9.6 Internal examination.......................................................................................................................................................................... 7
10 Expression of results......................................................................................................................................................................................... 7
11 Precision........................................................................................................................................................................................................................ 8
12 Test report.................................................................................................................................................................................................................... 8
Annex A (informative) Precision................................................................................................................................................................................ 9
Annex B (normative) Calibration schedule.................................................................................................................................................12
Bibliography.............................................................................................................................................................................................................................. 14
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ISO 815-1:2019(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 third edition cancels and replaces the second edition (ISO 815‑1:2014), which has been technically
revised.
The main changes compared to the previous edition are as follows:
— normative references have been updated in Clause 2.
— a new precision statement has been added in Annex A.
A list of all parts in the ISO 815 series can be found on the ISO website.
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.
1 Scope
This document specifies methods for the determination of the compression set characteristics of
vulcanized and thermoplastic rubbers at ambient (one method) or elevated temperatures (three
methods, A, B, and C, depending on the way the test piece is released at the end of the test).
The methods are intended to measure the ability of rubbers of hardness within the range 10 IRHD to
95 IRHD to retain their elastic properties at specified temperatures after prolonged compression at
constant strain (normally 25 %) under one of the alternative sets of conditions described. For rubber of
nominal hardness 80 IRHD and above, a lower compression strain is used: 15 % for a nominal hardness
from 80 IRHD to 89 IRHD and 10 % for a nominal hardness from 90 IRHD to 95 IRHD.
NOTE 1 When rubber is held under compression, physical or chemical changes that prevent the rubber
returning to its original dimensions after release of the deforming force can occur. The result is a set, the
magnitude of which depends on the time and temperature of compression as well as on the time, temperature,
and conditions of recovery. At elevated temperatures, chemical changes become increasingly more important
and lead to a permanent set.
NOTE 2 Short-time compression set tests, typically for 24 h, at elevated temperatures are commonly used as
a measure of the state of cure, a means of material classification, and a specification to ensure the quality of a
compound. Longer tests, typically for 1 000 h, at elevated temperatures take account of the effect of ageing and
are often used to predict service performance, including that of sealing materials. Short-time tests at ambient
temperature show mainly the effect of physical changes (re-orientation of the molecular chains and the fillers).
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 188:2011, Rubber, vulcanized or thermoplastic — Accelerated ageing and heat resistance tests
ISO 18899:2013, Rubber — Guide to the calibration of test equipment
ISO 23529:2016, Rubber — General procedures for preparing and conditioning test pieces for physical
test methods
4 Principle
A test piece of known thickness is compressed at standard laboratory temperature to a defined strain,
which is then maintained constant for a specified time at standard laboratory temperature or a fixed
elevated temperature. The compression is released and, after the test piece has been allowed to recover
at a standard laboratory temperature or the elevated temperature for a specified time, the thickness of
the test piece is again measured.
5 Apparatus
5.1 Compression assembly, consisting of compression plates, steel spacers, and clamping device.
5.1.1 Compression plates, consisting of two parallel, flat, highly polished plates made of chromium-
plated steel or stainless-steel or any corrosion-resistant material between the faces of which the test
piece is compressed.
The spacer(s) shall be of such size and shape that contact with the compressed test piece is avoided.
The height of the spacer(s) shall be chosen so that the compression applied to the test piece is
— (25 ± 2) % for hardnesses below 80 IRHD,
— (15 ± 2) % for hardnesses between 80 IRHD and 89 IRHD,
— (10 ± 1) % for hardnesses of 90 IRHD and higher.
5.2 Oven, in accordance with the requirements specified in ISO 188:2011, method A or method B,
and capable of maintaining the compression assembly and test pieces at the test temperature within the
tolerance specified in 8.2.
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NOTE Test results obtained with ovens for method A can be different from those obtained with ovens for
method B.
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ISO 815-1:2019(E)
The time to reach a steady-state temperature depends on the type of oven and the overall heat capacity
of the compression assembly. To obtain comparable results in the case of an elevated test temperature
and a 24 h test duration, it is necessary to reach the steady-state temperature within the specified
tolerances in the interior of the test pieces in not more than 3 h.
5.4 Thickness gauge, with an accuracy of ±0,01 mm (see ISO 23529:2016, 9.1), having a flat circular
foot of 4,0 mm ± 0,5 mm in diameter and a flat solid base-plate and exerting a pressure of 22 kPa ± 5 kPa
for solid rubber of hardness equal to or greater than 35 IRHD, or a pressure of 10 kPa ± 2 kPa if the
hardness is less than 35 IRHD.
NOTE When using a digital gauge, a resolution of 0,001 mm is needed to obtain the required accuracy.
After testing at elevated temperature, an unexpected deformation of the test piece is sometimes
observed. More particularly, the two flat surfaces can be deformed, which complicates the thickness
measurement. In this case, particular care should be taken in positioning the foot on the test piece.
5.5 Timing device, for measuring the recovery time, with an accuracy of ±1 s.
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a) Example 1 b) Example 2
Key
1 test piece 5 lower plate
2 spacer 6 part formed for clamping in a device
3 nut 7 locating pin
4 upper plate 8 screw
6 Calibration
The test apparatus shall be calibrated in accordance with the schedule given in Annex B.
7 Test pieces
7.1 Dimensions
The test pieces shall be one of two sizes, designated type A and type B.
— Type A: a cylindrical disc of diameter 29,0 mm ± 0,5 mm and thickness 12,5 mm ± 0,5 mm.
— Type B: a cylindrical disc of diameter 13,0 mm ± 0,5 mm and thickness 6,3 mm ± 0,3 mm.
4
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ISO 815-1:2019(E)
These two types do not necessarily give the same values for compression set, and comparison of results
obtained using test pieces of different sizes shall be avoided when comparing one compound with
another.
Type A test pieces are preferred for testing rubbers having low compression set, because of the greater
accuracy attainable using these larger test pieces.
Type B test pieces are preferred when it is required to cut test pieces from products. In this case, the test
pieces shall be taken as near to the centre of the product as possible, unless otherwise specified. When
possible, the test piece shall be cut in such a way that its axis is parallel to the direction of compression
of the product in service.
7.2 Preparation
The test pieces shall be prepared by moulding each disc, whenever possible. Preparation by cutting out
each disc or by laminating not more than three discs is permitted. The use of test pieces prepared by
laminating several discs for control of finished products shall be agreed between interested parties.
Cutting shall be performed in accordance with ISO 23529. When cupping (the formation of a concave
surface) is a problem, the test piece shape can be improved by cutting it in two stages: first, cut an
oversize test piece, and then, trim it to the exact dimensions with a second cutter.
Laminated test pieces shall conform to the dimensions specified in 7.1 and shall be prepared by
laminating discs or rubber cut from sheets without adhesives. Discs can be compressed by a few percent
for 1 min so that they stick together. The number of discs laminated to produce a test piece shall not
exceed three. The total thickness shall then be measured.
Test pieces prepared by the various methods described above can give different results and comparison
of values shall be avoided.
NOTE Attention is drawn to the marked effects of the state of cure on compression set values. It might be
necessary to adjust the cure of moulded test pieces to be representative of different thicknesses of sheets or
mouldings.
evaluations intended to be comparable, the tests, as far as possible, shall be carried out after the same
time interval.
For product tests, whenever possible, the time between production and testing shall not exceed
three months. In other cases, tests shall be made within two months of the date of receipt of the product
by the purchaser (see ISO 23529).
7.5 Conditioning
Samples and test pieces shall be protected from light and heat as much as possible during the interval
between production and testing.
Prepared test pieces shall be conditioned immediately before testing for a minimum period of 3 h at one
of the standard laboratory temperatures specified in ISO 23529. The same temperature shall be used
throughout any one test or series of tests intended to be comparable.
Test pieces of thermoplastic rubbers shall be annealed before testing by heating in an oven at a
temperature and for a length of time that are appropriate to the material in order to release internal
stresses caused by the moulding process. They shall then be conditioned at a standard laboratory
temperature.
NOTE 70 °C for 30 min is suitable for many materials.
8 Test conditions
The exposure time shall be 24−02 h, 72−02 h, (168 ± 2) h, or multiples of 168 h, measured from the
moment of placing the compression assembly in the oven (5.2).
The temperature of test shall be one of the standard laboratory temperatures 23 °C ± 2 °C or 27 °C ± 2 °C
(see ISO 23529) for tests at ambient temperature, and one of the following temperatures for tests at
elevated temperatures: 40 °C ± 1 °C, 55 °C ± 1 °C, 70 °C ± 1 °C, 85 °C ± 1 °C, 100 °C ± 1 °C, 125 °C ± 2 °C,
150 °C ± 2 °C, 175 °C ± 2 °C, 200 °C ± 2 °C, 225 °C ± 2 °C, or 250 °C ± 2 °C.
NOTE As oven temperatures are increased, the results become increasingly dependent upon the thermal
stability of the rubber. At still higher temperatures, surface oxidation of the test piece makes a significant
contribution to the observed compression set. There is no simple correlation between the compression set
observed at elevated temperatures and that observed at room temperature.
9 Procedure
If for any reason a lubricant is not used, this shall be mentioned in the test report.
6
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ISO 815-1:2019(E)
If the test is conducted at ambient temperature, release the test pieces after the required test duration
(see 8.1) and transfer them to a wooden bench. Leave them to recover for 30 min ± 3 min at standard
laboratory temperature and then measure their thickness.
Method A: After the required test duration (see 8.1), remove the compression assembly from the oven,
immediately release the test pieces and transfer the test pieces quickly to a wooden bench. Leave them
to recover at a standard laboratory temperature for 30 min ± 3 min, and then measure their thickness.
Method A shall be used unless otherwise specified.
Method B: After the required test duration, remove the compression set assembly from the oven,
allow it to cool to a standard laboratory temperature, but for a minimum of 30 min and a maximum
of 120 min, then release the test pieces and, after a further 30 min ± 3 min at standard laboratory
temperature measure their thickness.
Method C: After the required test duration, do not remove the compression assembly from the oven
but immediately release the test pieces and keep them in the oven. Leave them to recover at the test
temperature for 30 min ± 3 min and, after a further 30 min ± 3 min at standard laboratory temperature,
measure their thickness.
NOTE The temperature of the test piece after release from compression can affect the rate and extent of
recovery and hence the value of compression set. Recovery at elevated temperature is generally quicker than at
standard laboratory temperature and results in a lower compression set.
10 Expression of results
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.
The compression set, expressed as a percentage of the initial compression, is given by Formula (1):
h0 − h1
× 100 (1)
h0 − hs
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where
11 Precision
See Annex A.
12 Test report
The test report shall include the following information:
a) sample details:
1) a full description of the sample and its origin,
2) compound and cure details, where appropriate,
3) the method of preparation of test pieces from samples, for example whether moulded or cut;
b) test method:
1) a full reference to the test method used, i.e. the number of this document (ISO 815‑1:2019),
2) the type of test piece used, i.e. A or B, and whether or not it was laminated,
3) the method of cooling used after the test, i.e. A, B or C, and the exact cooling time for method B,
4) the nature of the lubricant used,
5) whether the test pieces were tested separately or as a set;
c) test details:
1) the standard laboratory temperature used,
2) the temperature and times of conditioning and of recovery,
3) the duration and temperature of test,
4) the compression used,
5) details of any procedures not specified in this document;
d) test results:
1) the number of test pieces used,
2) the initial thickness of the test pieces, if required,
3) the thickness of the test pieces after recovery, if required,
4) the median value of the compression set and the individual test results;
e) the date of the test.
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ISO 815-1:2019(E)
Annex A
(informative)
Precision
A.1 General
The precision calculations to express repeatability and reproducibility were performed in accordance
with ISO/TR 92721). For precision concepts and nomenclature, consult ISO 19983 which replaces the
withdrawn Technical Report.
laboratory only tested two pieces and one laboratory only tested one piece. The average compression
set value was used as the “test result”. The compression set was measured after 30 min ± 3 min
recovery time at standard laboratory temperature after removal from the apparatus in accordance
with method A.
Replicate testing was performed three weeks after the initial testing.
A type 1 precision was measured in the ITP. The time period for repeatability and reproducibility is
on a scale of weeks. Seven laboratories reported data for type A pieces at both temperatures and nine
laboratories reported data for type B pieces at both temperatures.
1) Withdrawn.
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ISO 815-1:2019(E)
A.3.1 The precision results for the 1986 ITP are given in Table A.1 for compression set at 100 °C. The
symbols sr, r, (r), sR, R and (R) as used in Tables A.1 to A.5, are defined as follows:
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Pooled values 28,0 6,0 15 10,0 35
A.3.2 The precision results for the 2015 ITP are given in Tables A.2 to A.5.
Seven laboratories submitted data for the Type A Compression set at 23 °C testing. One laboratory each
was eliminated as a means outlier for the IIR and SBR materials. One laboratory each was eliminated
as a high variability outlier for the IIR and SBR materials. The values shown in Table A.2 are the results
after treatment of the outliers.
Seven laboratories submitted data for the Type A Compression set at 100 °C testing. One laboratory
was eliminated as a means outlier for the IIR material. One laboratory each was eliminated as a high
variability outlier for the EPDM and IIR materials. The values shown in Table A.3 are the results after
treatment of the outliers.
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ISO 815-1:2019(E)
Nine laboratories submitted data for the Type B Compression set at 23 °C testing. One laboratory each
was eliminated as a means outlier for the IIR and SBR materials. One laboratory was eliminated as
a high variability outlier for the EPDM material. The values shown in Table A.4 are the results after
treatment of the outliers.
Nine laboratories submitted data for the Type B Compression set at 100 °C testing. One laboratory each
was eliminated as a means outlier for the EPDM and SBR materials. One laboratory each was eliminated
as a high variability outlier for the EPDM, IIR, and SBR materials. The values shown in Table A.5 are the
results after treatment of the outliers.
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Annex B
(normative)
Calibration schedule
B.1 Inspection
Before any calibration is undertaken, the condition of the items to be calibrated shall be ascertained by
inspection and recorded on any calibration report or certificate. It shall be reported whether calibration
is made in the ‘as-received’ condition or after rectification of any abnormality or fault.
It shall be ascertained that the apparatus is general fit for the intended purpose, including any
parameters specified as approximate and for which the apparatus does not therefore need to be
formally calibrated. If such parameters are liable to change, then the need for periodic checks shall be
written into the detailed calibration procedures.
B.2 Schedule
Verification/calibration of the test apparatus is a normative part of this document. The frequency of
calibration and the procedures used are, unless otherwise stated, at the discretion of the individual
laboratory using ISO 18899 for guidance.
The calibration schedule given in Table B.1 has been compiled by listing all of the parameters specified
in the test method, together with the specified requirement. A parameter and requirement can relate to
the main test apparatus, part of that apparatus or to an ancillary apparatus necessary for the test.
For each parameter, a calibration procedure is indicated by reference to ISO 18899, to another
publication or to a procedure particular to the test method which is detailed (whenever a more specific
or detailed calibration procedure than in ISO 18899 is available, it shall be used in preference).
The verification frequency for each parameter is given by a code letter.
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ISO 815-1:2019(E)
In addition to the items listed in the table, use of the following is implied, which shall be calibrated in
accordance with ISO 18899:
— instruments for determining dimensions of the test pieces.
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ISO 815-1:2019(E)
Bibliography
[1] ISO 4287, Geometrical Product Specifications (GPS) — Surface texture: Profile method — Terms,
definitions and surface texture parameters
[2] ISO/TR 92722), Rubber and rubber products — Determination of precision for test method
standards
[3] ISO 19983, Rubber — Determination of precision of test methods
2) Withdrawn.
14
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ICS 83.060
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