INTERNATIONAL ISO

STANDARD 1817

Sixth edition
2015-02-15

Rubber, vulcanized or
thermoplastic — Determination of the
effect of liquids
Caoutchouc vulcanisé ou thermoplastique — Détermination de
l’action des liquides

Reference number
ISO 1817:2015(E)

© ISO 2015
ISO 1817:2015(E)


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 ISO 1817:2015(E)


Contents Page

Foreword......................................................................................................................................................................................................................................... iv
Introduction...................................................................................................................................................................................................................................v
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Apparatus...................................................................................................................................................................................................................... 1
4 Calibration................................................................................................................................................................................................................... 3
5 Test liquids.................................................................................................................................................................................................................. 3
6 Test pieces.................................................................................................................................................................................................................... 3
6.1 Preparation................................................................................................................................................................................................. 3
6.2 Dimensions.................................................................................................................................................................................................. 3
6.3 Time interval between vulcanization and testing..................................................................................................... 4
6.4 Conditioning............................................................................................................................................................................................... 4
7 Immersion in the test liquid...................................................................................................................................................................... 4
7.1 Temperature............................................................................................................................................................................................... 4
7.2 Duration......................................................................................................................................................................................................... 5
8 Procedure..................................................................................................................................................................................................................... 5
8.1 General............................................................................................................................................................................................................ 5
8.2 Change in mass........................................................................................................................................................................................ 6
8.3 Change in volume.................................................................................................................................................................................. 6
8.4 Change in dimensions........................................................................................................................................................................ 7
8.5 Change in surface area...................................................................................................................................................................... 8
8.6 Change in hardness.............................................................................................................................................................................. 8
8.7 Change in tensile stress-strain properties....................................................................................................................... 9
8.8 Testing with liquid on one surface only.............................................................................................................................. 9
8.9 Determination of extractable matter................................................................................................................................. 10
9 Precision..................................................................................................................................................................................................................... 11
10 Test report................................................................................................................................................................................................................. 11
Annex A (normative) Reference liquids..........................................................................................................................................................12
Annex B (normative) Calibration schedule.................................................................................................................................................15
Annex C (informative) Precision results from an interlaboratory test programme.........................................17
Bibliography.............................................................................................................................................................................................................................. 23

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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 on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is ISO/TC 45, Rubber and rubber products, Subcommittee
SC 2, Testing and analysis.
This sixth edition cancels and replaces the fifth edition (ISO 1817:2011), which has been revised to
include a precision statement (see Annex C). Additionally, the flash point of oil No. 2 has been adjusted to
the actual value and the CAS (Chemical Abstracts Service) numbers have been incorporated in Table A1
and A2 as well as in Clause A.3.

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Introduction
The action of a liquid on vulcanized or thermoplastic rubber can generally result in:
a) absorption of the liquid by the rubber;
b) extraction of soluble constituents from the rubber;
c) a chemical reaction with the rubber.
The amount of absorption [a)] is usually larger than that of extraction [b)] so that the net result is an
increase in volume, commonly termed “swelling”. The absorption of liquid can profoundly alter physical
and chemical properties and hence change tensile strength, extensibility and hardness of the rubber,
so it is important to measure these properties after treatment of the rubber. The extraction of soluble
constituents, especially plasticizers and antidegradants, can likewise alter the rubber’s physical
properties and chemical resistance after drying (assuming the liquid to be volatile). Therefore, it is
necessary to test these properties following immersion and drying of the rubber. This International
Standard describes the methods necessary for determining the changes in the following properties:
— change in mass, volume and dimensions;
— extractable matter;
— change in hardness and tensile stress-strain properties after immersion and after immersion and
drying.
Although in some respects these tests might simulate service conditions, no direct correlation with
service behaviour is implied. Thus, the rubber giving the lowest change in volume is not necessarily the
best one in service. The thickness of the rubber needs to be taken into account since the rate of penetration
of liquid is time-dependent and the bulk of a very thick rubber product might remain unaffected for the
whole of the projected service life, especially with viscous liquids. Moreover, it is known that the action
of a liquid on rubber, especially at high temperatures, can be affected by the presence of atmospheric
oxygen. The tests described in this International Standard can, however, provide valuable information
on the suitability of a rubber for use with a given liquid and, in particular, constitute a useful control
when used for developing rubbers resistant to oils, fuels, or other service liquids.
The effect of a liquid might depend on the nature and magnitude of any stress within the rubber. In this
International Standard, test pieces are tested in an unstressed condition.

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INTERNATIONAL STANDARD ISO 1817:2015(E)

Rubber, vulcanized or thermoplastic — Determination of

the effect of liquids
WARNING 1 — 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
ensure compliance with any national regulatory conditions.
WARNING 2 — Certain procedures specified in this document might involve the use or generation
of substances, or the generation of waste, that could constitute a local environmental hazard.
Reference should be made to appropriate documentation on safe handling and disposal after use.

1 Scope
This International Standard describes methods of evaluating the resistance of vulcanized and
thermoplastic rubbers to the action of liquids by measurement of properties of the rubbers before and
after immersion in test liquids. The liquids concerned include current service liquids, such as petroleum
derivatives, organic solvents and chemical reagents, as well as reference test liquids.

2 Normative references
The following referenced documents are indispensable for the application of this document. For dated
references, only the edition cited applies. For undated references, the latest edition of the referenced
document (including any amendments) applies.
ISO 37, Rubber, vulcanized or thermoplastic — Determination of tensile stress-strain properties
ISO 48, Rubber, vulcanized or thermoplastic — Determination of hardness (hardness between 10 IRHD and
100 IRHD)
ISO 175, Plastics — Methods of test for the determination of the effects of immersion in liquid chemicals
ISO 7619‑1, Rubber, vulcanized or thermoplastic — Determination of indentation hardness — Part 1:
Durometer method (Shore hardness)
ISO 18899:2013, Rubber — Guide to the calibration of test equipment
ISO 23529:2010, Rubber — General procedures for preparing and conditioning test pieces for physical test
methods
ASTM D5964, Standard Practice for Rubber IRM 901, IRM 902, and IRM 903 Replacement Oils for ASTM
No. 1, ASTM No. 2, and ASTM No. 3 Oils

3 Apparatus

3.1 Total immersion apparatus, designed to take account of the volatility of the test liquid and of the
immersion temperature in order to prevent and minimize evaporation of the test liquid and the ingress of
air.

For tests at temperatures considerably below the boiling point of the test liquid, a stoppered glass bottle
or tube shall be used. For tests at temperatures near the boiling point of the test liquid, the bottle or tube
shall be fitted with a reflux condenser or other suitable means of minimizing the evaporation of liquid.

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The bottle or tube shall be so dimensioned that the test pieces remain completely immersed and all
surfaces are completely exposed to the liquid without any restriction. The volume of liquid shall be at
least 15 times the combined volume of the test pieces and the volume of air above the liquid shall be kept
to a minimum.
The test pieces shall be mounted in jigs, preferably hanging on a rod or wire, and separated from any
adjacent test piece, for instance by glass rings or other non-reactive spacers.
The materials of the apparatus shall be inert to the test liquid and to the rubber; for example, materials
containing copper shall not be used.

3.2 Apparatus for testing one surface only, which holds the test piece in contact with the liquid on
only one of its surfaces.

A suitable apparatus is illustrated in Figure 1. It comprises a base-plate (A) and an open-ended cylindrical
chamber (B), which is held tightly against the test piece (C) by wing nuts (D) mounted on bolts (E). A
hole of approximately 30 mm diameter is allowed in the base-plate for examination of the surface not
in contact with the liquid. During the test, the opening on the top of the chamber shall be closed by a
close-fitting plug (F).
Dimensions in millimetres

Figure 1 — Apparatus for testing one surface only

3.3 Balance, accurate to 1 mg.

3.4 Instrument for measuring the thickness of the test piece, consisting of a micrometre dial gauge,
of adequate accuracy, firmly held in a rigid stand over a flat base-plate. The instrument shall comply with
the requirements given for such apparatus in ISO 23529:2010, method A.

3.5 Instrument for measuring the length and width of the test piece, having a scale graduated in
divisions of 0,01 mm and preferably operating without contact with the test piece, for example using an
optical system complying with the requirements given for such apparatus in ISO 23529:2010, method D.

3.6 Instrument for measuring the change in surface area, capable of measuring the lengths of the
diagonals of the test piece. It shall have a scale graduated in divisions of 0,01 mm and should preferably

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operate without contact with the test piece, for example using an optical system complying with the
requirements given for such apparatus in ISO 23529:2010, method D.

4 Calibration
The requirements for calibration of the test apparatus are given in Annex B.

5 Test liquids
The choice of the test liquid shall depend on the purpose of the test.
When information is required on the service behaviour of a vulcanized or thermoplastic rubber in
contact with a particular liquid, then this liquid shall, if possible, be chosen for the test. Commercial
liquids are not always constant in composition, and the test shall, whenever practicable, include a
reference material of known characteristics. Any abnormal results due to unexpected variations in the
composition of the commercial liquid will thus become apparent. It might then be necessary to set aside
a bulk supply of the liquid for a particular series of tests.
Mineral oils and fuels are liable to vary considerably in chemical composition even when supplied at a
recognized specification. The aniline point of a mineral oil gives some indication of its aromatic content
and helps to characterize the action of the oil on rubber, but the aniline point alone is not sufficient to
characterize a mineral oil; other things being equal, the lower the aniline point, the more pronounced
the action. If a mineral oil is used as test liquid, the test report shall include the density, refractive index,
viscosity and aniline point or aromatic content of the oil.
Service oils having similar fluid characteristics to the reference liquids (see Clauses A.1 to A.3) will
not necessarily have the same effect on the material as the reference liquids. Some fuels, particularly
gasoline, vary widely in composition and, for some possible constituents, minor variations can have
a large influence on the effect on rubber. Complete details of the composition of the fuel used shall
therefore be included in the test report.
As commercial liquids do not always have a constant composition, a standard liquid consisting of well-
defined chemical compounds or mixtures of compounds shall be used as reference liquid for the purpose
of classification of vulcanized or thermoplastic rubbers or quality control. Some suitable liquids are
listed in Annex A.
When testing to determine the effect of chemical solutions, the concentration of the solution shall be
appropriate to the intended use.
Ensure that the composition of the test liquid does not change significantly during immersion. The
ageing of the test liquid and any interaction with the test pieces shall be taken into consideration. If
there are chemically active additives in the liquid, or if there is a significant change in composition by
extraction, absorption or reaction with the rubber, either the volume shall be increased or the liquid
shall be replaced with fresh liquid at specified intervals.

6 Test pieces

6.1 Preparation
Test pieces shall be prepared in accordance with ISO 23529:2010.

6.2 Dimensions
Data obtained on test pieces having different original thicknesses might not be comparable. Therefore,
where possible, test pieces shall be of uniform thickness of (2 ± 0,2) mm.

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Test pieces cut from commercial articles may be used. For products thinner than 1,8 mm, use the original
thickness. If the material is thicker than 2,2 mm, reduce the thickness to (2 ± 0,2) mm.
Test pieces for the determination of the change in volume and mass shall have a volume of 1 cm3 to
3 cm3.
Test pieces for the determination of the change in hardness shall have lateral dimensions of no less than
8 mm.
Test pieces for the determination of the change in dimensions shall be quadrilateral with sides between
25 mm and 50 mm in length, or circular with a diameter of 44,6 mm (internal diameter of type B test
piece in ISO 37). This type of test piece can also be used for the determination of mass and volume.
Test pieces for the determination of the change in surface area shall be rhomboid, with the sides cut
cleanly and at right angles to the top and bottom surfaces. This can be achieved by two consecutive
cuts at approximately right angles to each other, with a cutter consisting of two parallel blades, suitably
spaced. The length of the sides shall be nominally 8 mm.
NOTE For the determination of the change in surface area, it might be convenient to use smaller or thinner
test pieces, for example when cut from products or when rapid attainment of equilibrium is required. However,
the results might not be comparable with those obtained using the specified thickness. Smaller test pieces will
reduce the precision of the results.

Test pieces for the determination of tensile properties shall be in accordance with ISO 37. Type 2 dumb-
bells are preferred because their size makes them more convenient to immerse in liquid than type 1. The
type 2 test piece can also be used when determining the change in mass, volume or hardness.
For tests with liquid contact on one surface only, the test piece shall consist of a disc with a diameter of
about 60 mm.

6.3 Time interval between vulcanization and testing

Unless otherwise specified for technical reasons, the following requirements, in accordance with
ISO 23529:2010 for time intervals, shall be observed.
For all test purposes, the minimum time between vulcanization and testing shall be 16 h.
For non-product tests, the maximum time between vulcanization and testing shall be 4 weeks and, for
evaluations intended to be comparable, the tests shall be carried out using, as far as possible, the same
time interval.
For product tests, whenever possible, the time between vulcanization and testing shall not exceed
3 months. In other cases, tests shall be made within 2 months of the date of receipt of the product by the
customer.

6.4 Conditioning
Test pieces for test in the “as received” condition shall be conditioned for not less than 3 h at one of the
standard laboratory temperatures specified in ISO 23529:2010. The same temperature shall be used
throughout any test or any series of tests intended to be comparable.

7 Immersion in the test liquid

7.1 Temperature
Unless otherwise specified, the immersion shall be carried out at one or more of the temperatures listed
in 8.2.2 of ISO 23529:2010.

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As elevated temperatures can greatly increase the oxidation of the rubber, volatilization or decomposition
of the immersion liquid and the effect of any chemically active additives in the liquid (for example in
service liquids), appropriate selection of the test temperatures is very important.
In tests intended to simulate service conditions, and using the actual liquid with which the rubber will
be used, the test conditions shall approximate to those found in service, using the closest standard
temperature equal to or higher than the service temperature.

7.2 Duration
Since the rate of penetration of liquids into rubbers depends on the temperature, the type of rubber
material and the type of liquid, the use of only one standard period of immersion is precluded. For
acceptance purposes, it is recommended that repeated determinations be made and recorded after
successive periods of immersion so as to indicate the change in properties with time. The total immersion
time shall, if possible, extend well beyond the point of maximum absorption.
For control purposes, a single period of immersion can suffice, preferably chosen such that maximum
absorption is reached. For such purposes, one of the following periods shall be used:

24 −02 h; 72 −02 h; 7 days ± 2 h; multiples of 7 days ± 2 h

NOTE 1 Since the amount of liquid absorbed is initially proportional to the square root of time rather than time
itself, it is helpful to assess the “time to maximum absorption” by plotting the amount absorbed against the square
root of time.

NOTE 2 The percentage change during the early stages of immersion is inversely proportional to the test piece
thickness. Therefore, lower tolerances for thickness are advisable to obtain consistent results when maximum
absorption is not reached.

8 Procedure

8.1 General
Use three test pieces for each set of measurements and make any identification marks required before
immersion.
Immerse the test pieces in the appropriate apparatus described in 3.1 or 3.2, using the liquid selected
(see Clause 5) and the temperature selected (see 7.1).
For total immersion, place the test pieces at a distance of at least 5 mm from the sides of the container
and at least 10 mm from the bottom and top surfaces. If the density of the rubber is less than that of the
liquid, means shall be provided for holding the test pieces completely below the surface of the liquid.
The ingress of air shall be avoided. If the influence of air is to be tested, the degree of access of air shall
be determined by agreement between the interested parties.
At the end of the period of immersion, bring the test pieces, if necessary, to the standard laboratory
temperature within 30 min. This can be done by quickly transferring the test pieces to a fresh portion of
the test liquid at this temperature and allowing to stand for a period of 10 min to 30 min.
Remove surplus test liquid from the surface. When volatile liquids are used, remove and quickly wipe the
test pieces with a filter paper or a piece of lint-free fabric. Viscous non-volatile liquids can be removed by
filter paper and, if necessary, by quickly immersing the test pieces in a volatile liquid, such as ethanol or
petroleum ether, then quickly wiping them.
Following removal of the test pieces from volatile test liquids, it is important that each subsequent
manipulation takes place as soon as possible. Carry out the tests immediately after the removal of
surplus liquid or, for change in mass or volume, by placing the test piece immediately in a weighing
bottle.

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If, after the measurement of mass or dimensions, the same test pieces are used for the measurement
of other properties, immerse the test pieces in the volatile liquid again. The total immersion time shall
be in accordance with 7.2. The maximum time between removal from the test liquid and the end of the
measurement shall, for a volatile liquid, be:
— change in dimensions: 1 min;
— change in hardness: 2 min;
— tensile test: 2 min.
If the immersion is to be continued, put the test pieces back in the liquid immediately and return them
to the temperature-controlled oven or bath.
The changes in properties can also be determined after drying. For this purpose, dry the test pieces
under an absolute air pressure of approximately 20 kPa at approximately 40 °C to constant mass, i.e.
until the difference between successive weighings at 30 min intervals does not exceed 1 mg. Cool to
room temperature and condition by keeping at the standard laboratory temperature for not less than
3 h.

8.2 Change in mass

Weigh each test piece to the nearest milligram at the standard laboratory temperature before and after
immersion.
Calculate the percentage change in mass Δm100 using Formula (1):
mi − m0
∆m100 = × 100 (1)
m0
where
m0 is the initial mass of the test piece;

mi is the mass of the test piece after immersion.

Report the result as the median value for the three test pieces.

8.3 Change in volume

The water displacement method is used for test liquids which are immiscible with water.
Weigh each test piece in air to the nearest milligram (mass m0), and then reweigh each test piece in
distilled water at the standard laboratory temperature (mass m0,w), taking care to ensure that all air
bubbles are removed (a detergent can be used). If the density of the material is less than 1 g/cm3, it
will be necessary to use a sinker when weighing in water to ensure that the test pieces are completely
immersed. If a sinker is used, determine the mass of the sinker alone in distilled water separately (mass
ms,w). Blot the test pieces dry with filter paper or lint-free fabric.
Immerse each test piece in the test liquid. At the end of the period of immersion, weigh each test piece in
air (mass mi) to the nearest milligram, and then reweigh each test piece in distilled water (mass mi,w),
also at the standard laboratory temperature.

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Calculate the percentage change in volume ΔV100 using Formula (2):

 m − mi,w + ms,w 
∆V100 =  i − 1  × 100 (2)
 m −m 
 0 0,w + ms,w 
where
m0 is the initial mass of the test piece;

mi is the mass of the test piece after immersion;

m0,w is the initial mass of the test piece (plus sinker if used) in water;

mi,w is the mass of the test piece (plus sinker if used) after immersion in water;

ms,w is the mass of the sinker, if used, in water.

Report the result as the median value for the three test pieces.
If the test liquid is readily miscible with water or reacts with it, water cannot be used after immersion. If
the test liquid is not too viscous or volatile at room temperature, a fresh portion of the test liquid can be
used. If the test liquid is not suitable, use another liquid after immersion and calculate using Formula (3):

 1  mi − mi,liq + ms,liq  
∆V100 =    − 1 × 100 (3)
 ρ  m0 − m0,w + ms,w  
where
ρ is the density of the liquid;

mi,liq is the mass of the test piece (plus sinker, if used) in the liquid;

ms,liq is the mass of the sinker, if used, in the liquid;

the other symbols are as defined for Formula (2).

8.4 Change in dimensions

Measure the initial length of each test piece along its centre line to the nearest 0,5 mm at the standard
laboratory temperature (taking measurements along the top and bottom surfaces and averaging the
two results). Similarly, measure the initial width by taking four measurements in all (top and bottom,
both sides) near each end of the test piece.
Measure the initial thickness with the thickness gauge at four different points along the test piece and
calculate the average of the results.
After immersion, re-measure the length, width and thickness of each test piece as described above.
Make all measurements with the test piece at the standard laboratory temperature.

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Calculate the percentage change in length Δl100 using Formula (4):

l i − l0
∆l100 = × 100 (4)
l0
where
l0 is the initial length;

li is the length after immersion.

Similarly, calculate the percentage changes in width and thickness.

Report the results as the median values for the three test pieces. The change in surface area can be
calculated from the values obtained for the length and the width.

8.5 Change in surface area

Measure the initial lengths of the diagonals of each test piece to the nearest 0,01 mm at the standard
laboratory temperature.
After immersion, re-measure the lengths of the diagonals as described above. If an optical measuring
system is used, this may be done in a suitable glass container without removing the test pieces from the
test liquid.
Calculate the percentage change in area ΔA100 using Formula (5):

l l 
∆A100 =  A B − 1  × 100 (5)
 lal b 
where
la and lb are the lengths of the diagonals before immersion;

lA and lB are the lengths of the diagonals after immersion.

If required, the percentage volume change ΔV100 may be calculated using Formula (6):

 l l  3/2 
∆V100 =  A B  − 1 × 100 (6)
 l a l b  
 
The equation for percentage volume change assumes isotropic swelling. If any doubt exists, determine
the percentage volume change as specified in 8.3, which is the preferred method.
Report the result as the median value for the three test pieces.

8.6 Change in hardness

Measure the IRHD hardness using the microtest described in ISO 48 on each test piece before and after
immersion.
As an alternative, the normal IRHD hardness may be used with three plied-up test pieces, but in this
case express the result as the apparent hardness.

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Calculate the change in IRHD hardness ΔH, before and after immersion, using Formula (7):
∆H = H i − H 0 (7)

where
H0 is the initial hardness;

Hi is the hardness after immersion.

Report the result as the median value for the three test pieces.
Alternatively, the method specified in ISO 7619‑1 may be used.

8.7 Change in tensile stress-strain properties

Measure tensile stress-strain properties before and after immersion in accordance with ISO 37.
Calculate the selected tensile properties using the initial cross-section of the test piece for stress
calculations. Calculate the change in the property ΔX100 as a percentage of the value for un-immersed
material using Formula (8):
Xi − X0
∆X 100 = × 100 (8)
X0
where
X0 is the initial value of the property;

Xi is the value of the property after immersion.

Report the result as the median value for the three test pieces.

8.8 Testing with liquid on one surface only

This test is applicable to relatively thin sheet materials, for example rubber diaphragms, which are
exposed to liquid on one surface only during use.
Measure the nominal thickness of the test piece and then weigh it in air to the nearest milligram (mass
m0).
Then place the test piece in the apparatus as indicated in Figure 1. Fill the chamber of the apparatus
with the test liquid to a depth of approximately 15 mm and insert the plug (F). Maintain the apparatus
at the required temperature for the duration of the test.
At the end of the contact period, bring the apparatus, if necessary, to the standard laboratory temperature.
Remove the liquid and release the test piece. Remove any surplus liquid from the surface of the test piece
by wiping with filter paper or a lint-free fabric. Then weigh the test piece to the nearest milligram (mass
mi) and measure the thickness at the standard laboratory temperature.
If the test liquid is volatile at room temperature, make the measurement within 2 min following removal
from the liquid.

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Express the change in mass per unit surface area ΔmA , in grams per square metre, using Formula (9):
mi − m0
∆m A = (9)
A
where
m0 is the initial mass, in grams, of the test piece;

mi is the final mass, in grams, of the test piece;

A is the area, in square metres, of the circular surface of the test piece in contact with the test
liquid.

Report the result as the median for the three test pieces.
Calculate the change in thickness as specified in 8.4.

8.9 Determination of extractable matter

8.9.1 General

If the test liquid is readily volatile, the amount of matter which it extracts from the test piece can be
determined
a) either by drying the treated test piece and comparing its mass with the mass before immersion;
b) or by evaporating the test liquid to dryness and weighing the non-volatile residue.
Both methods are susceptible to error. In the method in which the dried test piece is weighed, the material
can be oxidized if air is present during immersion, especially at high temperatures. In the method
in which the test liquid is evaporated, there can be some loss of volatile extracted matter, especially
plasticizers. Both methods are described in this International Standard and the choice between them
depends on the nature of the material and the conditions of test.
It is difficult to define precisely what is meant by a “readily volatile” liquid, but it is suggested that the
procedures described are not suitable for liquids less volatile than standard liquids A, B, C, D and E in
Annex A, i.e. for liquids boiling at above 110 °C.
The determination of extractable matter shall be made after having determined the change in mass (see
8.2), the change in volume (see 8.3) and the change in dimensions (see 8.4).
Report the result as the median for the three test pieces.

8.9.2 By weighing the dried test piece

Dry the test piece, after immersion, under an absolute air pressure of approximately 20 kPa at
approximately 40 °C to constant mass, i.e. until the difference between successive weighings at 30 min
intervals does not exceed 1 mg.
The extractable-matter content is taken as the difference between the original mass of the test piece and
its mass after immersion and drying, expressed as a percentage of the original mass of the test piece.

8.9.3 By evaporating the test liquid

Transfer the liquid in which the test piece was immersed to a suitable container and wash the test piece
with 25 ml of fresh liquid, collecting the washings in the same container. Evaporate the liquid and dry
the residue to constant mass under an absolute air pressure of approximately 20 kPa at approximately
40 °C.

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Carry out a blank test to estimate the solids content in a volume of the test liquid equal to that used for
the immersion plus that used for washing.
The extractable-matter content is taken as the mass of the dried residue, corrected for the result of the
blank test, expressed as a percentage of the original mass of the test piece.

9 Precision
Precision results of an interlaboratory test programme (ITP) are given in Annex C.

10 Test report
The test report shall include the following information:
a) sample details:
1) a full description of the sample and its origin,
2) the method of preparation of test pieces from the sample, for example whether moulded or cut;
b) a reference to this International Standard;
c) test method and test details:
1) the method(s) used,
2) the type(s) of test piece used (dimensions),
3) the standard laboratory temperature used,
4) details of conditioning,
5) the period and temperature of immersion,
6) any deviation from the specified procedure;
d) test results:
1) the results, expressed in the form stated in the relevant subclause,
2) the appearance of the test piece (for example cracking, delamination), if appropriate,
3) the appearance of the test liquid (for example discoloration, sedimentation), if appropriate;
e) the date of the test.

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Annex A
(normative)

Reference liquids

WARNING — Appropriate safety precautions should be taken when preparing and handling test
liquids, especially those known to be toxic, corrosive or flammable. Products giving off fumes
should be handled only under an efficiently ventilated hood, corrosive products should not be
allowed to come into contact with the skin or ordinary clothing, and flammable products should
be kept away from any source of ignition.

A.1 Standard simulated fuels

Commercial fuels vary widely in composition even within the same grade (i.e. knock-rating) and from the
same source. There are hydrocarbon-based fuels with and without oxygen compounds as well as alcohol-
based fuels. The grade of gasoline is improved by adding aromatic or oxygen-containing compounds, but
these additives increase the effect of fuels on normally fuel-resistant rubbers. The composition varies
with the situation on the gasoline market and with the geographical area and can change rapidly. Hence,
several test liquids which are used in practice are recommended in Tables A.1 and A.2 to cover the range
of different compositions. They can also serve as guidelines for the formulation of other suitable test
liquids. Analytical reagent quality materials shall be used in making up the test liquids. Test liquids
containing alcohol shall not be used if the fuels involved are known to be free of alcohol.

Table A.1 — Standard simulated fuels without oxygen compounds

CAS Registry Content
Liquid Constituents Number
% (by volume)
A 2,2,4-Trimethylpentane 540–84–1 100
B 2,2,4-Trimethylpentane 540–84–1 70
Toluene 108–88–3 30
C 2,2,4-Trimethylpentane 540–84–1 50
Toluene 108–88–3 50
D 2,2,4-Trimethylpentane 540–84–1 60
Toluene 108–88–3 40
E Toluene 108–88–3 100
F Straight-chain paraffins (C12 to C18) 68476–34–6 80
1-Methylnaphthalene 90–12–0 20
NOTE Liquids B, C and D simulate petroleum-derived fuels without oxygen compounds. Liquid F is intended to simulate
diesel fuel, domestic heating oils and similar light furnace oils.

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Table A.2 — Standard simulated fuels containing oxygen compounds (alcohols)

CAS Registry Num- Content
Liquid Constituents ber
% (by volume)
1 2,2,4-Trimethylpentane 540–84–1 30
Toluene 108–88–3 50
Di-isobutylene 25167–70–8 15
Ethanol 64–17–5 5

2 2,2,4-Trimethylpentane 540–84–1 25,35a

Toluene 108–88–3 42,25a
Di-isobutylene 25167–70–8 12,68a
Ethanol 64–17–5 4,22a
Methanol 67–56–1 15,00
Water 7732–18–5 0,50

3 2,2,4-Trimethylpentane 540–84–1 45
Toluene 108–88–3 45
Ethanol 64–17–5 7
Methanol 67–56–1 3

4 2,2,4-Trimethylpentane 540–84–1 42,5

Toluene 108–88–3 42,5
Methanol 67–56–1 15
a Together, these four constituents are equivalent to 84,5 % (by volume) of liquid 1 above.

A.2 Reference oils

A.2.1 General descriptions
Oil No. 1 (IRM 901) is a “low volume increase” oil, oil No. 2 (IRM 902) is a “medium volume increase” oil
and oil No. 3 (IRM 903) is a “high volume increase” oil.
These reference oils are representative of low-additive mineral oils.

A.2.2 Requirements
The oils shall have the properties specified in ASTM D5964 and shown in Table A.3. The properties given
in Table A.4 are typical of the oils but cannot be guaranteed by suppliers.
When these reference oils are required as test liquids, only those obtained from recognized suppliers
shall be used for referee purposes and they shall be available for general use. However, in the event
that they are not available, alternative oils may be used, but for routine testing only, provided that they
comply with the requirements of Table A.3 and also have been shown to give results similar to those
obtained with the reference oils when testing rubbers of the same type of composition as those on which
the routine tests are to be carried out.

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Table A.3 — Specifications of reference oils

Requirements
Property
Oil No. 1 Oil No. 2 Oil No. 3
Aniline point, °C 124 ± 1 93 ± 3 70 ± 1
Kinematic viscosity, m2/s ( × 10−6) 18,12 to 20,34a 19,2 to 21,5a 31,9 to 34,1b
Flash point, °C, min. 243 232 163
API gravity at 16 °C 27,8 to 29,8 19,0 to 21,0 21,0 to 23,0
Viscosity-gravity constant 0,790 to 0,805 0,860 to 0,870 0,875 to 0,885
Naphthenics content, cN, % 27 (average) 35, min. 40, min.
Paraffinics content, cP, % 65, min. 50, max. 45, max.
a Measured at 99 °C.
b Measured at 37,8 °C.

Table A.4 — Typical properties of reference oils

Requirements
Property
Oil No. 1 Oil No. 2 Oil No. 3
Pour point, °C −12 −12 −31
ASTM colour L3.5 L2.5 L0.5
Refractive index at 20 °C 1,484 8 1,510 5 1,502 6
UV absorbance at 260 nm 0,8 4,0 2,2
Aromatics content, cA , % 3 12 14

A.3 Simulated service liquid

NOTE Liquid 102 has been removed from the present edition of this International Standard because no
supplier can be found. For information, the composition of the liquid is given below.

Liquid 102 is intended to simulate certain high pressure hydraulic oils. It is a blend comprising 95 % (by mass)
of oil No. 1 and 5 % (by mass) of a hydrocarbon-compound oil additive containing 29,5 % (by mass) to 33 % (by
mass) of sulfur, 1,5 % to 2 % (by mass) of phosphorus and 0,7 % (by mass) of nitrogen.

A.3.1 Liquid 101

Liquid 101 is intended to simulate synthetic diester-type lubricating oils. It is a blend comprising
99,5 % (by mass) of di 2 ethylhexyl sebacate (CAS Registry Number: 122-62-3) and 0,5 % (by mass) of
phenothiazine (CAS Registry Number: 92-84-2).

A.3.2 Liquid 103

Liquid 103 is intended to simulate phosphate-ester hydraulic oils used in aircraft. It is tri-n-butyl
phosphate (CAS Registry Number: 126-73-8).

A.4 Chemical reagents

Tests with chemical reagents shall be carried out using the same chemicals at the same concentrations as
those to be encountered in the intended use of the product. For general purposes, where no specification
is known, the list of chemical reagents given in ISO 175 can be useful.

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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 in any calibration report or certificate. It shall be reported whether calibration
is carried out in the “as-received” condition or after rectification of any abnormality or fault.
It shall be ascertained that the apparatus is generally 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 mandatory part of this International Standard. However,
the frequency of calibration and the procedures used are, unless otherwise stated, at the discretion of
the individual laboratory, using ISO 18899:2013 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, to 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 18899:2013, to another
publication or to a procedure particular to the test method which is detailed (whenever a calibration
procedure which is more specific or detailed than that in ISO 18899:2013 is available, it shall be used in
preference).
The verification frequency for each parameter is given by a code-letter. The code-letters used in the
calibration schedule are:
R use of certified reference material;
C requirement to be confirmed, but no measurement;
N initial verification only;
S standard interval as given in ISO 18899:2013;
U in use.

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Table B.1 — Calibration frequency schedule

Verification
Subclause in
Parameter Requirement(s) frequency Notes
ISO 18899:2013
guide
Total immersion apparatus Volume such that test 15.8, 19.1 U
pieces remain completely
immersed and all surfaces
are exposed to liquid
Volume of liquid at least 15.8, 19.1 U
15 times that of test
pieces
Inert to test liquid and 15.8, 19.1 U
rubber
Stoppered bottle or tube 19.1 U For tests at tempera-
to be used tures considerably
below boiling point of
liquid
Bottle or tube to be fitted 19.1 U For tests at tempera-
with reflux condenser or tures near boiling
equivalent point of liquid
Apparatus for testing one As shown in Figure 1 - N
surface only
Balance Accurate to 1 mg 22.1 S
Dial gauge See ISO 23529:2010, 15.1, 16.6 S
method A
Instrument for measuring Scale graduated in divi- 15.1 S Preferably non-con-
length and width sions of 0,01 mm tacting
Instrument for measuring Scale graduated in divi- 15.3 S Preferably non-con-
change in surface area sions of 0,01 mm tacting
Test liquid As specified in Annex A - N
Materials To be used in 8.3 - U
    distilled water
    lintless blotting medium

In addition to the items listed in Table B.1, use of the following is implied, all of which need calibrating in
accordance with ISO 18899:2013:
— a timer;
— a thermometer for monitoring the conditioning and test temperatures;
— a hygrometer for monitoring the conditioning and test humidities;
— apparatus for measuring selected physical properties.

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Annex C
(informative)

Precision results from an interlaboratory test programme

C.1 General
The following interlaboratory test programme (ITP) was initially carried out in 2011.
All calculations to provide repeatability and reproducibility values were performed in accordance with
ISO/TR 9272[1]. Precision concepts and nomenclature are also given in ISO/TR 9272.

C.2 Precision results from the ITP

C.2.1 Programme details
The ITP was organized and conducted by Bundesanstalt für Materialforschung (Germany) in 2011.
Cured test pieces were prepared in one laboratory and sent to all 12 participating laboratories.
A total of four compounds were used in the test. The samples were designated as Compounds A, B, C and
D. For the details of the compounding of the materials and their vulcanization, see Table C.1.

Table C.1 — Compounding

Ingredient Number of parts by mass

Compound A Compound B i Compound C j Compound D k
NR (TSR L) 100
NBR (ACN content 28 %) 100
HNBR (ACN content 39 %) 100
FKM (VDF/HDF copolymer) 100
HAF carbon black (N 330) 30
HAF carbon black (N 550) 65 50
HAF carbon black (N 990) 25
Zinc oxide 3 5 2
Magnesium oxide 2 3
a N’-Isopropyl-N’-phenyl-p-phenylendiamine
b Polymerized 2,2,4-trimethyl-1,2-dihydroquinoline
c Benzothiazyl disulfide
d Tetramethylthiuram disulfide
e N-Cyclohexylbenzothiazyl-2-sulfenamide
f organic phosphonium salt, e.g. triphenylbenzyl-phosphonium chloride
g 1,3-bis(t-butylperoxyisopropyl)-benzene
h 2,2-bis(4-hydroxyphenyl)-hexafluoropropane
i Compound B is in conformance with ISO 13226[2] SRE-NBR 28/SX
j Compound C is in conformance with ISO 13226[2] SRE-HNBR/1X
k Compound D is in conformance with ISO 13226[2] SRE-FKM/2X

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Table C.1 (continued)

Ingredient Number of parts by mass
Compound A Compound B i Compound C j Compound D k
Calcium hydroxide 2
Stearic acid 1
Antioxidant (IPPD) a 1
Antioxidant (TMQ) b 2
Antioxidant Diphenylamine, sty-
1
renated
Accelerator (MBTS) c 1,7
Accelerator (TMTD) d 2,5
Accelerator (CBS) e 1,5
Accelerator f 0,44
Triallyl isocyanurate 1,5
Sulfur 2,5 0,2
Peroxide (40 % by mass) g 7,5
Bisphenol h 1,35
Total 138,2 177,2 164,0 131,79
Press cure 150°C 160 °C 180°C 180°C + 220 °C
18 min 20 min 10 min 7 min + 16 h
a N’-Isopropyl-N’-phenyl-p-phenylendiamine
b Polymerized 2,2,4-trimethyl-1,2-dihydroquinoline
c Benzothiazyl disulfide
d Tetramethylthiuram disulfide
e N-Cyclohexylbenzothiazyl-2-sulfenamide
f organic phosphonium salt, e.g. triphenylbenzyl-phosphonium chloride
g 1,3-bis(t-butylperoxyisopropyl)-benzene
h 2,2-bis(4-hydroxyphenyl)-hexafluoropropane
i Compound B is in conformance with ISO 13226[2] SRE-NBR 28/SX
j Compound C is in conformance with ISO 13226[2] SRE-HNBR/1X
k Compound D is in conformance with ISO 13226[2] SRE-FKM/2X

The influence of liquids during storage was determined for the following properties:
— change in mass
— change in volume
— change in dimensions
— change in hardness
— change in tensile stress-strain properties.
The test pieces were provided as disks with a diameter of 36,6 mm and type 2 dumb-bells.
The test pieces were stored in the liquids at standard laboratory temperature and also at 70 °C; the
details of the storage are given in Table C.2. Each participating laboratory used its own test liquids.

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Table C.2 — Overview of the test program

Compound Temperature Duration of Liquid a Method
exposure
A standard laboratory 2h+6h B mass
A standard laboratory 24 h B mass; thickness; hardness
B standard laboratory 2h+6h B mass
B standard laboratory 24 h B mass; volume; thickness; hardness
C standard laboratory 24 h B mass; volume; tensile test
D standard laboratory 24 h E mass; volume; tensile test
C 70 °C 7d Oil No. 3 mass; volume; hardness; tensile
test
a See Annex A.

The number of laboratories on which precision data for each property is based is given in the tables of
precision results (Tables C.3 to C.15). The number of participating laboratories as noted in these tables
is the final number after identifying certain laboratory values as outliers (for each of the five properties).
The ITP testing was conducted over a period of four sequential weeks. On a specified day in each of these
four weeks, five individual measurements were performed on all four materials. The test result of each
week is the median of the five individual measurements. All analysis was conducted on the basis of these
test results.
The participating laboratories were encouraged to use two equally competent operators (if available)
for this ITP: Operator 1 for test weeks 1 and 2 and Operator 2 for test weeks 3 and 4. The aim of the use of
different test pieces and different operators and the repetition over four test weeks was to include such
normal variation sources in the final or pooled combined database. Thus, the precision values represent
more reliable and realistic values compared to the usual ITP results which constitute a “single point in
time” estimate of precision.

C.2.2 Precision results

The precision results are listed in Tables C.3 to C.15.
The precision results as determined by this ITP should not be applied to acceptance or rejection
testing for any group of materials or products without documentation that the results of this precision
evaluation actually apply to the products or materials tested.
Explanation of symbols for Tables C.3, C.4, C.5, C.6, C.7, C.8, C.9, C.10, C.11, C.12, C.13, C.14 and C.15:
sr = within-laboratory standard deviation (in measurement units);
r = repeatability (in measurement units);
(r) = repeatability (in percent of mean level);
sR = between-laboratory standard deviation (for total between-laboratory variation in measurement
units);
R = reproducibility (in measurement units);
(R) = reproducibility (in percent of mean level).

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Table C.3 — Precision data for change in mass

No. of
Compound Mean level sr r (r) sR R (R)
laboratoriesa
A 120,53 2,78 7,77 6,45 3,81 10,68 8,86 9
B 10,31 0,76 2,13 20,65 0,86 2,40 23,32 9
Average b 1,77 4,95 13,55 2,34 6,54 16,09
NOTE   Duration of exposure: 2 h; standard laboratory temperature; Liquid B.
a Number of laboratories after outliers deleted (total number of laboratories in ITP: 12).
b Simple averages calculated.

Table C.4 — Precision data for change in mass

No. of
Compound Mean level sr r (r) sR R (R)
laboratoriesa
A 157,31 1,91 5,35 3,40 3,19 8,92 5,67 10
B 18,77 0,99 2,77 14,74 1,02 2,87 15,27 8
Average b 1,45 4,06 9,07 2,10 5,89 10,47
NOTE   Duration of exposure: 6 h; standard laboratory temperature; Liquid B.
a Number of laboratories after outliers deleted (total number of laboratories in ITP: 12).
b Simple averages calculated.

Table C.5 — Precision data for change in mass

No. of
Compound Mean level sr r (r) sR R (R)
laboratoriesa
A 160,93 1,63 4,55 2,83 2,76 7,73 4,80 10
B 27,17 0,78 2,20 8,09 1,69 4,74 17,44 9
C 21,55 1,12 3,15 14,61 1,74 4,86 22,55 10
D 3,26 0,09 0,24 7,47 0,39 1,10 33,64 9
Average b 0,92 2,57 8,40 1,43 4,00 17,41
NOTE   Duration of exposure: 24 h; standard laboratory temperature; Liquid B – Compound A, B, C; Liquid E – Compound D.
a Number of laboratories after outliers deleted (total number of laboratories in ITP: 12).
b Simple averages calculated.

Table C.6 — Precision data for change in mass

No. of
Compound Mean level sr r (r) sR R (R)
laboratoriesa
C 5,99 0,12 0,35 5,84 0,72 2,01 33,64 9
NOTE   Duration of exposure: 7days; 70 °C; Oil No. 3.
a Number of laboratories after outliers deleted (total number of laboratories in ITP: 12).

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Table C.7 — Precision data for change in volume

No. of
Compound Mean level sr r (r) sR R (R)
laboratoriesa
B 40,37 1,24 3,47 8,61 1,27 3,57 8,84 8
C 30,37 2,19 6,14 20,20 2,73 7,64 25,16 9
D 7,39 0,43 1,21 16,42 0,95 2,67 36,11 9
Average b 1,29 3,61 15,08 1,65 4,63 23,37
NOTE   Duration of exposure: 24 h; standard laboratory temperature; Liquid B – Compound B, C; Liquid E – Compound D.
a Number of laboratories after outliers deleted (total number of laboratories in ITP: 12).
b Simple averages calculated.

Table C.8 — Precision data for change in volume

No. of
Compound Mean level sr r (r) sR R (R)
laboratoriesa
C 7,31 0,24 0,66 9,03 1,20 3,35 45,89 8
NOTE   Duration of exposure: 7days; 70 °C; Oil No. 3.
a Number of laboratories after outliers deleted (total number of laboratories in ITP: 12).

Table C.9 — Precision data for change in dimensions (thickness)

No. of
Compound Mean level sr r (r) sR R (R)
laboratoriesa
A 54,46 0,86 2,40 4,40 2,00 5,59 10,26 7
B 14,08 0,52 1,46 10,35 0,71 2,00 14,17 8
Average b 0,69 1,93 7,38 1,35 3,79 12,22
NOTE   Duration of exposure: 24 h; standard laboratory temperature; Liquid B.
a Number of laboratories after outliers deleted (total number of laboratories in ITP: 12).
b Simple averages calculated.

Table C.10 — Precision data for change in hardness

No. of
Compound Mean level sr r (r) sR R (R)
laboratoriesa
A −21,93 0,55 1,53 6,98 2,35 6,57 29,98 9
B −18,40 0,24 0,67 3,63 0,64 1,78 9,70 7
Average b 0,39 1,10 5,31 1,49 4,18 19,84
NOTE   Duration of exposure: 24 h; standard laboratory temperature; Liquid B.
a Number of laboratories after outliers deleted (total number of laboratories in ITP: 12).
b Simple averages calculated.

Table C.11 — Precision data for change in hardness

No. of
Compound Mean level sr r (r) sR R (R)
laboratoriesa
C −3,68 0,93 2,60 70,63 1,36 3,80 103,06 10
NOTE   Duration of exposure: 7days; 70 °C; Oil No. 3.
a Number of laboratories after outliers deleted (total number of laboratories in ITP: 12).

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Table C.12 — Precision data for change in tensile stress-strain properties — Tensile strength
No. of
Compound Mean level sr r (r) sR R (R)
laboratoriesa
C −43,77 1,94 5,43 12,40 4,16 11,65 26,62 10
D −17,88 1,46 4,09 22,87 3,53 9,89 55,34 10
Average b 1,70 4,76 17,63 3,85 10,77 40,98
NOTE   Duration of exposure: 24 h; standard laboratory temperature; Liquid B – Compound C; Liquid E – Compound D.
a Number of laboratories after outliers deleted (total number of laboratories in ITP: 12).
b Simple averages calculated.

Table C.13 — Precision data for change in tensile stress-strain properties — Tensile strength
No. of
Compound Mean level sr r (r) sR R (R)
laboratoriesa
C −1,39 2,83 7,91 570,92 3,50 9,79 706,39 9
NOTE   Duration of exposure: 7days; 70 °C; Oil No. 3.
a Number of laboratories after outliers deleted (total number of laboratories in ITP: 12).

Table C.14 — Precision data for change in tensile stress-strain properties — Elongation
No. of
Compound Mean level sr r (r) sR R (R)
laboratoriesa
C −42,68 3,05 8,55 20,03 3,93 11,01 25,80 10
D −7,88 1,95 5,45 69,18 2,21 6,19 78,57 10
Average b 2,50 7,00 44,61 3,07 8,60 52,18
NOTE   Duration of exposure: 24 h; standard laboratory temperature; Liquid B – Compound C; Liquid E – Compound D.
a Number of laboratories after outliers deleted (total number of laboratories in ITP: 12).
b Simple averages calculated.

Table C.15 — Precision data for change in tensile stress-strain properties — Elongation
No. of
Compound Mean level sr r (r) sR R (R)
laboratoriesa
C −2,38 3,91 10,93 458,52 4,70 13,17 552,21 8
NOTE   Duration of exposure: 7days; 70 °C; Oil No. 3.
a Number of laboratories after outliers deleted (total number of laboratories in ITP: 12).

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Bibliography

[1] ISO/TR 9272, Rubber and rubber products — Determination of precision for test method standards
[2] ISO 13226, Rubber — Standard reference elastomers (SREs) for characterizing the effect of liquids
on vulcanized rubbers

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