D EUTSCHE NORM March 2000

{
Accelerated ageing of rubber
53508
ICS 83.060 Supersedes
October 1993 edition.
Prüfung von Kautschuk und Elastomeren – Künstliche Alterung
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In keeping with current practice in standards published by the International Organization for Standardization
(ISO), a comma has been used throughout as the decimal marker.

Foreword
This standard has been prepared by Technical Committee Prüfung der physikalischen Eigenschaften von
Kautschuk und Elastomeren of the Normenausschuss Materialprüfung (Materials Testing Standards Com-
mittee).
The standard is based on ISO 188, from which it differs in the following points:
– it gives a different flow velocity for the oven with forced air circulation;
– it recommends testing certain properties using type S 2 dumb-bell test pieces;
– it recommends test temperatures and duration;
– it includes formulae for calculating standard deviations, the variation coefficient and confidence
interval.

Amendments
This standard differs from the October 1993 edition in that references have been updated and the standard
has been editorially revised.

Previous editions
DIN DVM 3508 = DIN 53508: 1939-02, 1954-12, 1960-05, 1977-07, 1993-10.

1 Scope
The test methods specified in this standard serve to determine the resistance of rubber to deterioration by
subjecting test pieces to accelerated ageing (either by heating them in air at atmospheric pressure or in
oxygen at an elevated pressure).
Various physical properties are measured at standard laboratory temperature before and after testing, and
the relative or absolute differences are used to estimate the relative service life of the rubber.
The methods described in this standard are not suitable for assessing the effects of light or ozone on the
deterioration of rubber.

Continued on pages 2 to 6.

Translation by DIN-Sprachendienst.
In case of doubt, the German-language original should be consulted as the authoritative text.

© No part of this translation may be reproduced without the prior permission of Ref. No. DIN 53508 : 2000-03
DIN Deutsches Institut für Normung e.V., Berlin. Beuth Verlag GmbH, 10772 Berlin, Germany, English price group 06 Sales No. 0106
has the exclusive right of sale for German Standards (DIN-Normen).
07.00
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DIN 53508 : 2000-03

2 Normative references
This standard incorporates, by dated or undated reference, provisions from other publications. These norma-
tive references are cited at the appropriate places in the text, and the titles of the publications are listed below.
For dated references, subsequent amendments to or revisions of any of these publications apply to this
standard only when incorporated in it by amendment or revision. For undated references, the latest edition of
the publication referred to applies.
DIN 50011-2 Testing of materials, components and equipment – Ovens – Conditioning of test pieces
DIN 50011-12 Artificial climates in technical applications – Air temperature as a climatological quantity
in controlled-atmosphere test installations
DIN 50014 Artificial climates in technical applications – Standard atmospheres
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DIN 50035-1 Concepts relating to the ageing of materials – Basic concepts

DIN 50035-2 Concepts relating to the ageing of materials – Polymer materials
DIN 53504 Determination of tensile stress/strain properties of rubber
DIN 53505 Shore A and D hardness testing of rubber and plastics
DIN 53519-1 Determination of indentation hardness (IRHD) of soft rubber using standard specimens
DIN 53598-1 Statistical evaluation of random samples with examples from tests on elastomers and
plastics
DIN EN ISO 2578 Plastics – Determination of time-temperature limits after prolonged exposure to heat
(ISO 2578 : 1993)
ISO 5725-1 : 1994 Accuracy (trueness and precision) of measurement methods and results – Part 1: General
principles and definitions
ISO 5725-2 : 1994 Accuracy (trueness and precision) of measurement methods and results – Part 2: Basic
method for the determination of repeatability and reproducibility of a standard measure-
ment method
Technische Regeln für Druckbehälter (TRB) (Codes of practice for pressure vessels)
Unfallverhütungsvorschrift Sauerstoff (Accident prevention regulation on the use of oxygen) (VBG 62)
Druckbehälterverordnung (German Pressure Vessels Regulation), BGBl. (German Federal Law Gazette) I, 1989,
No. 20, pp. 843–869

3 Concept
Accelerated ageing is a test method by means of which the expected deterioration of rubber in practical
applications is ascertained by subjecting test pieces to accelerated deteriorating influences (e.g. elevated
temperatures, or, in some cases, elevated oxygen pressures).

4 Test methods
In order to effectively assess its resistance to ageing, the intended service applications of the rubber should
be considered, and test methods and conditions which approximate service conditions should be selected.
Only those properties relevant to application in service shall be determined; in most cases, these will be tensile
strength at break, elongation at break, stress/strain values (see DIN 53504) and hardness (see DIN 53505 or
DIN 53519-1).
Note that test results, especially those obtained from long-term testing, cannot be compared when different
types of ovens (i.e. with either forced or natural air circulation) are used.
Two methods of accelerated ageing are described in this standard.

4.1 Ageing in air at atmospheric pressure in one of the three following oven types, of which the oven described
in subclause 4.1.1 is to be given preference.
4.1.1 Air oven with forced air circulation (air recirculation system with fresh air supply) (see subclause 6.2).
4.1.2 Air oven with natural air circulation (see subclause 6.3).
4.1.3 Cell-type oven (see subclause 6.4).

4.2 Ageing in oxygen at an elevated pressure (see subclause 6.5).

5 Test pieces
Accelerated ageing shall be carried out on test pieces prepared and conditioned as specified in the standards
relevant to the appropriate property tests. The number of test pieces shall also be in accordance with these
standards.
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DIN 53508 : 2000-03

Test pieces shall be measured before testing. Only pieces of identical dimensions shall be compared with each
other.
It is recommended that tests be carried out on type S 2 dumb-bell test pieces which are triple-layered and
(2 t 0,2) mm thick, as specified in DIN 53504.
Marking (e.g. applying gauge lines for measuring elongation) shall be carried out after heating as inks can affect
ageing.

6 Apparatus
6.1 General
In addition to meeting the requirements listed below, ovens shall be designed so that test pieces do not come
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in contact with any parts containing copper or copper alloys, as these materials may accelerate the ageing
process.
It is essential that the temperature tolerances specified in subclause 7.2 be observed and that temperatures
remain constant throughout the oven chamber or cell. Temperatures shall be measured in close proximity to
the test piece.
NOTE: The type of oven to be used will be specified in all relevant test documents.

6.2 Air oven with forced air circulation to DIN 50011-12

Ovens with forced air circulation include a recirculation system with fresh air supply. The air shall be preheated
to operating temperature, shall circulate at not less than thirty changes per hour, and shall flow at a rate between
0,25 m/s and 3 m/s.

6.3 Air oven with natural air circulation to DIN 50011-12

For ovens with natural air circulation, thermostatic control is necessary in order to maintain a constant, evenly
distributed temperature within the specified range throughout the heating period. Aluminium chamber or cell
walls also help achieve temperature consistency. The temperature must nevertheless be monitored at regular
intervals during the ageing period.
The air shall circulate at no less than three and no more than ten changes per hour, with the air velocity being
scarcely measurable (e.g. less than 2 mm/s). Sliding vents shall have no more than a slight effect on this rate.

6.4 Cell-type oven

Cell-type ovens shall comprise one or more unconnected cylindrical, vertical cells having a minimum height of
at least 300 mm in which the temperature can be kept constant and through which the air circulates at not less
than three and not more than ten changes per hour. Cells shall be surrounded by a good heat transfer medium.
NOTE: The flow velocity necessary to maintain the specified air circulation rate can be estimated based on the
number of cells and their volume, and shall be controlled by means of a flowmeter. Air shall circulate
uniformly in all cells.

6.5 Pressure chamber

Pressure chambers shall consist of a vessel made of stainless steel or another suitable material, and shall be
surrounded by a heat transfer medium which does not react with oxygen. The chamber shall meet all safety
requirements specified in the Druckbehälterverordnung, the Technische Regeln für Druckbehälter and the
Unfallverhütungsvorschrift Sauerstoff. It shall be equipped with a bursting disc to prevent the permissible
pressure from being exceeded in the case of an extreme reaction between the test material and oxygen.

7 Procedure
7.1 General
7.1.1 Test pieces shall be conditioned and stored in DIN 50014 – 23/50-2 standard atmosphere.
7.1.2 Test pieces shall be tested no earlier than 16 hours and no later than four weeks after vulcanization. If
this requirement cannot be met, especially when testing finished products, testing shall begin no later than three
months after vulcanization. If this is not possible, or when material is to be tested for which the production date
is unknown, testing shall begin within two months of delivery to the customer.
Once the accelerated ageing process has been completed and before testing, test pieces shall be conditioned
for no less than 16 hours and no more than six days in DIN 50014 – 23/50-2 standard atmosphere.
7.1.3 Ovens shall be brought to test temperature before test pieces are inserted, and the temperature mea-
sured at the location for the test piece. Test pieces shall be free from strain, protected from light, and exposed
to the air and/or oxygen on all sides. The pieces shall be suspended so they are at least 10 mm from each other
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DIN 53508 : 2000-03

and 10 mm (for cell-type ovens and pressure chambers) or 50 mm (for air ovens) from the oven walls. Test pieces
shall occupy no more than 10 % of the oven chamber or cell volume.
Where rubber compounds contain volatile substances, only similar compounds shall be aged simultaneously
in the same oven or cell.

7.2 Test temperatures and duration

Test temperatures and duration are to be selected based on the type of rubber under examination and the
expected service conditions.
7.2.1 Ageing in air as in subclause 4.1
The following test temperatures and periods are recommended:
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(70 t 1) °C for 7 days;

(100 t 1) °C for 3 or 7 days.
In special cases, the following temperatures and periods may be used in any combination:
test temperatures: (85 t 1) °C, (125 t 2) °C, (150 t 2) °C, (175 t 2) °C, (200 t 2) °C, (250 t 3) °C;
test periods: 1, 3, 7, or 10 days, or a multiple of 7 days.
7.2.2 Ageing in oxygen
The following conditions are recommended:
oxygen pressure: (21 t 1) bar;
test temperature: (70 t 1) °C;
test duration: (24 –20 ) hours, or a multiple thereof.

8 Expression of results
Results shall be expressed in accordance with the appropriate standards for each property test.
Calculate the arithmetic mean or median of all single values for each property, E, before ageing, EO, and after
ageing, EA.
Calculate the percentage change, Z r, for each property (except hardness) using equation (1):
EA – EO
Zr = · 100 (1)
EO
The absolute change in hardness, Za , is to be expressed as a difference calculated from equation (2):

Za = E A – E O (2)

The standard deviation for Zr, sZ, shall be calculated from equation (3) (see DIN 53598-1):

EA 2 2
1/2
sZ = ¨vE, A + v E, O ¿ (3)
EO
or, if v E, A R v E, O = v, approximated using equation (4):

EA
sZ = ·v12 (4)
EO
where
EA
are the mean values for each property before and after ageing;
EO
vE, A, vE, O are the coefficients of variation, as a percentage, for property E before and after ageing.

The standard deviation for Za shall be calculated from equation (5):

1/2
2
sZ = ¨sE, + s2E,
A O¿ (5)

or, if sE, A R s E, O = s, approximated using equation (6):

sZ = s 1 2 (6)

where s E, A; s E, O are the standard deviations of single values for property E (hardness) before and after ageing.
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DIN 53508 : 2000-03

The standard deviation can then be used to determine the confidence interval for a confidence level of 95 %,
as well as the coefficient of variation for Z, vZ, (see DIN 53598-1).
NOTE: The percentage changes for each property and the duration of the heating process at several tempera-
tures may be used to determine either the activation energy (using an Arrhenius plot), or the time-tempera-
ture limits (as described in DIN EN ISO 2578).

9 Precision
Repeatability limits and reproducibility limits for the relative changes in selected properties (elongation at break,
tensile strength at break, stress at 100 % strain) after ageing, and the absolute change in Shore A hardness after
ageing are given in table 1. Table 2 gives the characteristic relative repeatability limits and reproducibility limits
(for hardness, the absolute limits) for single values after ageing. In both tables, the arithmetic means for three
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types of vulcanizates are also included (see clause 8).

The difference between two single test results obtained by the same operator using the same equipment on
identical test material within a short period of time will not normally exceed the repeatability limit, r, more than
once in 20 cases.
The difference between two single and independent test results obtained by two operators working in different
laboratories on identical test material will not normally exceed the reproducibility limit, R, more than once in
20 cases.
The data relating to precision were obtained in a national interlaboratory test which was carried out in 1989 and
involved 17 rubber industry laboratories. Three types of vulcanizates were tested in ovens with forced air
circulation over periods of three and seven days at two different temperatures each (NR and NBR at 70 °C and
100 °C, EPDM at 100 °C and 125 °C). Elongation at break, tensile strength at break, stress at 100 % strain and
Shore A hardness were measured before and after ageing. Hardness was measured on 36 mm diameter discs,
as well as on type S 2 dumb-bell test pieces (2 mm thick, triple-layered). No significant difference between the
test results for each test piece type was reported. The test was organized and evaluated as specified in
ISO 5725-2.

10 Test report
The test report shall refer to this standard and include the following details:
a) type and designation of rubber tested;
b) time between vulcanization and testing;
c) type and dimensions of test pieces;
d) position of test pieces in the product;
e) ageing method and type of oven or pressure chamber used;
f) temperature and duration of ageing process;
g) values for each property before and after ageing (either 1: mean and standard deviation or single value
and mean, or 2: median, range and number of single values or single values and median);
h) relative or absolute changes, Z, for each property as described in clause 8 (including the confidence
interval for a confidence level of 95 %, as per DIN 53598-1);
i) any other visible changes, such as brittleness, glassiness, tackiness, deformation, discoloration, etc.;
j) any deviations from the specifications given in this standard;
k) testing date.
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DIN 53508 : 2000-03

Table 1: Repeatability limits and reproducibility limits for relative (or absolute) changes, Zr and Za,
after ageing

Type of rubber/
Property Z r and Za r R
Mean (m)

Elongation at
break, DeR /eR
m
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Tensile strength at
break, DsR /sR
m

Stress at 100 %
strain, Ds100 /s100
m

Shore A hardness

Table 2: Relative (or absolute) repeatability limits and reproducibility limits for single values after
ageing, EA

Type of rubber/
Property Zr and Za (r r) (R r)
Mean (m)

Elongation at
break
eR
m

Tensile strength at
break
sR
m

Stress at 100 %
strain
s100
m

r R

Shore A hardness