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INTERNATIONAL ISO

STANDARD 1817

Fifth edition
2011-09-15

Rubber, vulcanized or thermoplastic —


Determination of the effect of liquids
Caoutchouc vulcanisé ou thermoplastique — Détermination de l'action
des liquides
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Reference number
ISO 1817:2011(E)

© ISO 2011
ISO 1817:2011(E)
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COPYRIGHT PROTECTED DOCUMENT


© ISO 2011
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form or by any means,
electronic or mechanical, including photocopying and microfilm, without permission in writing from either ISO at the address below or
ISO's member body in the country of the requester.
ISO copyright office
Case postale 56  CH-1211 Geneva 20
Tel. + 41 22 749 01 11
Fax + 41 22 749 09 47
E-mail copyright@iso.org
Web www.iso.org
Published in Switzerland

ii © ISO 2011 – All rights reserved


ISO 1817:2011(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 ............................................................................................................................................ 4
6.3 Time interval between vulcanization and testing ............................................................................... 4
6.4 Conditioning .......................................................................................................................................... 4
7 Immersion in the test liquid .................................................................................................................. 5
7.1 Temperature ........................................................................................................................................... 5
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
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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 Test report ............................................................................................................................................ 11
Annex A (normative) Reference liquids.......................................................................................................... 12
Annex B (normative) Calibration schedule .................................................................................................... 15

© ISO 2011 – All rights reserved iii


ISO 1817:2011(E)

Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards bodies
(ISO member bodies). The work of preparing International Standards is normally carried out through ISO
technical committees. Each member body interested in a subject for which a technical committee has been
established has the right to be represented on that committee. International organizations, governmental and
non-governmental, in liaison with ISO, also take part in the work. ISO collaborates closely with the
International Electrotechnical Commission (IEC) on all matters of electrotechnical standardization.

International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.

The main task of technical committees is to prepare International Standards. Draft International Standards
adopted by the technical committees are circulated to the member bodies for voting. Publication as an
International Standard requires approval by at least 75 % of the member bodies casting a vote.

Attention is drawn to the possibility that some of the elements of this document may be the subject of patent
rights. ISO shall not be held responsible for identifying any or all such patent rights.

ISO 1817 was prepared by Technical Committee ISO/TC 45, Rubber and rubber products, Subcommittee
SC 2, Testing and analysis.

This fifth edition cancels and replaces the fourth edition (ISO 1817:2005), which has been technically revised
principally to update the clause on reference oils (Clause A.2) and to include a calibration schedule for the
apparatus used (see Annex B).
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iv © ISO 2011 – All rights reserved


ISO 1817:2011(E)

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 or 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
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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.

© ISO 2011 – All rights reserved v


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INTERNATIONAL STANDARD ISO 1817:2011(E)

Rubber, vulcanized or thermoplastic — Determination of the


effect of liquids

WARNING — Persons using this International Standard should be familiar with normal laboratory
practice. This standard does not purport to address all of the safety problems, if any, associated with
its use. It is the responsibility of the user to establish appropriate safety and health practices and to
ensure compliance with any national regulatory conditions.

IMPORTANT — Certain procedures specified in this International Standard 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
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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 18899:2004, 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.

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ISO 1817:2011(E)

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.

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
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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 micrometer 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.

2 © ISO 2011 – All rights reserved


ISO 1817:2011(E)

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
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 Annex A, 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
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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.

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ISO 1817:2011(E)

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.

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.
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6.3 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 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. The same temperature shall be used throughout
any test or any series of tests intended to be comparable.

4 © ISO 2011 – All rights reserved


ISO 1817:2011(E)

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.

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 20 h; 72 20 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
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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.

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ISO 1817:2011(E)

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 methanol 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.

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: 1 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.
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Calculate the percentage change in mass m100 as follows:

mi  m 0
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.

6 © ISO 2011 – All rights reserved


ISO 1817:2011(E)

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.

Calculate the percentage change in volume V100 using the following equation:

 mi  mi,w  m s,w 
V100    1  100 (2)
 m0  m0,w  m s,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 as follows:

 1  mi  mi,liq  m s,liq  
V100      1  100 (3)
   m0  m0,w  m s,w 
 

where
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 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 Equation (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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ISO 1817:2011(E)

Calculate the percentage change in length l100 using the following equation:

l l
l100  i 0  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 A100 using the following equation:

l l 
A100   A B  1  100 (5)
l
 abl 

where

la and lb are the lengths of the diagonals before immersion;


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

If required, the percentage volume change V100 may be calculated from the following equation:

 
3/2 
l l
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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ISO 1817:2011(E)

Calculate the change in IRHD hardness H, before and after immersion, using the following equation:

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 X100 as a percentage of the value for un-immersed material using the
following equation:

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.
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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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ISO 1817:2011(E)

Express the change in mass per unit surface area mA, in grams per square metre, using the following
equation:

mi  m 0
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.
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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.

10 © ISO 2011 – All rights reserved


ISO 1817:2011(E)

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 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;


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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.

© ISO 2011 – All rights reserved 11


ISO 1817:2011(E)

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

Content
Liquid Constituents
% (by volume)
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A 2,2,4-Trimethylpentane 100
B 2,2,4-Trimethylpentane 70
Toluene 30
C 2,2,4-Trimethylpentane 50
Toluene 50
D 2,2,4-Trimethylpentane 60
Toluene 40
E Toluene 100
F Straight-chain paraffins (C12 to C18) 80
1-Methylnaphthalene 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.

12 © ISO 2011 – All rights reserved


ISO 1817:2011(E)

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

Content
Liquid Constituents
% (by volume)
1 2,2,4-Trimethylpentane 30
Toluene 50
2,2,4-Trimethyl-1-pentene 15
Ethanol 5

2 2,2,4-Trimethylpentane 25,35a
Toluene 42,25a
2,2,4-Trimethyl-1-pentene 12,68a
Ethanol 4,22a
Methanol 15,00
Water 0,50

3 2,2,4-Trimethylpentane 45
Toluene 45
Ethanol 7
Methanol 3

4 2,2,4-Trimethylpentane 42,5
Toluene 42,5
Methanol 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.
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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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ISO 1817:2011(E)

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 21,54a 31,9 to 34,3b
Flash point, °C, min. 243 240 163
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 liquids


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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 and 0,5 % (by mass) of phenothiazine.

A.3.2 Liquid 102

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 suitable additive is commercially available.

A.3.3 Liquid 103

Liquid 103 is intended to simulate phosphate-ester hydraulic oils used in aircraft. It is tri-n-butyl phosphate.

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.

14 © ISO 2011 – All rights reserved


ISO 1817:2011(E)

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 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, to another publication or
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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 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;

U in use.

© ISO 2011 – All rights reserved 15


ISO 1817:2011(E)

Table B.1 — Calibration frequency schedule

Verification
Subclause in
Parameter Requirement(s) frequency Notes
ISO 18899:2004
guide

Total immersion apparatus Volume such that test pieces C U


remain completely immersed
and all surfaces are exposed to
liquid
Volume of liquid at least 15 C U
times that of test pieces
Inert to test liquid and rubber C U
Stoppered bottle or tube to be C U For tests at temperatures
used considerably below
boiling point of liquid
Bottle or tube to be fitted with C U For tests at temperatures
reflux condenser or equivalent near boiling point of liquid
Apparatus for testing one As shown in Figure 1 C N
surface only
Balance Accurate to 1 mg 22.1 S
Dial gauge See ISO 23529:2010, method A 15.1, 16.6 S
Instrument for measuring Scale graduated in divisions of 15.1 S Preferably non-contacting
length and width 0,01 mm
Instrument for measuring Scale graduated in divisions of 15.3 S Preferably non-contacting
change in surface area 0,01 mm
Test liquid As specified in Annex A R N
Materials To be used in 8.3 U
distilled water
lintless blotting medium
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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:

 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.

16 © ISO 2011 – All rights reserved


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ICS 83.060
Price based on 16 pages
ISO 1817:2011(E)

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