Proceedings of the ASME 2018
Pressure Vessels and Piping Conference
LONG-TERM PERFORMANCE OF ELASTOMER SEALS - FROM AGING TESTS TO
LIFETIME ESTIMATIONS
Matthias Jaunich
Bundesanstalt für Materialforschung und -prüfung
(BAM)
12200 Berlin, Germany
Jutta Horn
Bundesanstalt für
Materialforschung und -prüfung Materialforschung und -prüfung
(BAM)
12200 Berlin, Germany 12200 Berlin, Germany
ABSTRACT
Elastomers show a high versatility which makes them
ideal materials for sealing applications in various fields.
Especially under changing application conditions the high
recovery potential of this class of material is beneficial to
compensate temperature or pressure fluctuation, and
geometrical changes resulting from mechanical loads in e.g.
accident conditions. Out of these reasons elastomers are also
used in containers for low and intermediate level radioactive
waste and for spent fuel transportation casks. In casks designed
for low and intermediate level waste elastomer seals can act as
primary seal responsible for the containment function whereas
in spent fuel storage and transportation casks (dual purpose
casks (DPC)) elastomer seals are used as auxiliary seals to
allow leakage rate measurements of metal barrier seals. An
inherent prerequisite for this kind of application is the long
time-scale of operation without or with limited possibility of
seal replacement. In Germany an interim storage license for
DPC`s is typically issued for 40 years, a timeframe which might
increase in the future due to challenges of the final repository
siting procedure. For low and intermediate level waste, also
long time periods are required before final disposal can be
achieved. Therefore, the performance of elastomer seals over
extended time periods is, as for other applications, of high
importance.
A typical approach to ensure long-term functionality is to
perform accelerated aging tests to calculate an estimated
lifetime by assuming e.g. Arrhenius like equations for the time-
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PVP2018
July 15-20, 2018, Prague, Czech Republic
PVP2018-84631
Anja Kömmling
Bundesanstalt für Materialforschung und -prüfung
(BAM)
12200 Berlin, Germany
Holger Völzke Dietmar Wolff
Bundesanstalt für Bundesanstalt für
Materialforschung und -prüfung
(BAM) (BAM)
12200 Berlin, Germany
temperature relationship. This approach requires a suitable end
of life criterion considering the application of interest. This
often can represent a challenge on its own.
As BAM is involved in most of the cask licensing procedures
and especially responsible for the evaluation of cask-related
long-term safety issues we initiated several test programs for
investigating the behavior of elastomer seals. Experiments
concerning the low temperature performance down to -40 °C
and the influence of gamma irradiation have been started first.
Currently the thermal aging behavior of elastomer seals, which
is the topic of this contribution, is examined.
For our aging investigations we use a broad approach to first
determine the property changes in different elastomer materials
due to thermo-oxidative aging at elevated temperatures and
secondly, we test how the typical methods of lifetime
extrapolation can be applied to these results. This approach
enables us to detect and exclude undesired side effects which
very often influence lifetime estimations. In this contribution,
our recent results are extended. The results show that lifetime
estimation based on single material properties can be
misleading and therefore a combination of several methods is
recommended.
NOMENCLATURE
DPCs dual purpose casks, i.e. casks used as well for
transportation as for storage of radioactive
waste
EPDM ethylene propylene diene rubber
1 Copyright © 2018 ASME
 FKM fluorocarbon rubber
HNBR hydrogenated nitrile rubber
phr parts per hundred parts rubber
INTRODUCTION
Elastomers show a high versatility which makes them
ideal materials for sealing applications in various fields [1].
Especially under changing application conditions, the high
recovery potential of this class of material is beneficial to
compensate temperature or pressure fluctuation, and
geometrical changes resulting from mechanical loads in e.g.
accident conditions. Due to these reasons elastomers are also
used in containers for low and intermediate level radioactive
waste and for spent fuel storage and transportation casks (dual
purpose casks (DPCs)). In casks designed for low and
intermediate level waste elastomer seals can act as primary seal
responsible for the containment function whereas in DPCs
elastomer seals are used as auxiliary seals to allow leakage rate
measurements of metal barrier seals. An inherent prerequisite
for this kind of application is the long time scale of operation
without or with limited possibility of seal replacement. In
Germany interim storage licenses for DPCs are typically issued
for 40 years, a time frame which might increase in future due to
challenges of the final repository siting procedure. For low and
intermediate level waste, also long time periods are required
before final disposal can be achieved. Therefore, the
performance of elastomer seals over extended time periods is,
as for other applications, of high importance.
A typical approach to ensure long-term functionality is to
perform accelerated aging tests to estimate a lifetime by
assuming e.g. Arrhenius or Williams-Landel-Ferry (WLF) like
equations for the time-temperature relationship [2-5]. This
approach requires a suitable end of life criterion considering the
application of interest, which can be challenging. Various
lifetime criteria are used but a defined single set of parameters
which is really related to the seal performance is difficult to
establish [6].
As BAM is involved in most of the cask licensing procedures
and especially responsible for the evaluation of cask-related
long-term safety issues we initiated several test programs for
investigating the behavior of elastomer seals. Experiments
concerning the low temperature performance down to -40 °C
and the influence of gamma irradiation have been started first
[7-10]. A focus of these investigations was the seal performance
under static conditions but also tests performed after rapid
partial release of the seals were conducted [11, 12].
Currently, the thermal aging behavior of elastomer seals, which
is the topic of this contribution, is examined. In parallel
numerical description of the behavior of elastomer seals is
investigated [13].
For the aging experiments we focus on three different rubbers
namely ethylene propylene diene rubber (EPDM), fluorocarbon
rubber (FKM) and hydrogenated nitrile rubber (HNBR). These
rubbers are typically used for seals for different applications.
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FKM and EPDM are in use for the sealing of containers for
radioactive materials and HNBR is mainly used for applications
in contact with mineral oil. This selection is based on our
intention to compare materials which have different expected
lifetimes. In our case it is expected that the lifetime increases in
the following order: HNBR, EPDM and FKM.
In the following section an overview of our aging program is
given.
OVERVIEW OF ONGOING RESEARCH PROJECT
Our approach for the investigation of aging of different
elastomer seals is described in [14]. Therefore, here only a brief
overview is provided.
The tested materials are EPDM, FKM and HNBR. The EPDM
contained a base polymer with 48 wt.% ethylene, 4.1 wt.% of
diene ethylidene norbornene and the compound contains 90 phr
of carbon black filler. The HNBR base polymer has an
acrylonitrile content of 36 wt.% and an iodine number of 11.
The compound contains 80 phr of filler (mostly carbon black)
and 5 phr of plasticizer. FKM contains a polymer with 66 wt.%
fluorine content and 70 phr of silica/silica-chalk filler.
For aging we use a threefold approach consisting of component
tests performed on seals (inner diameter 180 mm and a cord
diameter of 10 mm) compressed between two flanges,
characterization of material stored at 25 % compression
between two metal plates and uncompressed material. Aging
was performed at temperatures ranging from 75 °C to 150 °C in
circulating ovens with air atmosphere. As samples O-ring seals
and 2 mm thick test plates were used. The dimensions of the
O-rings were 10 mm cord diameter and an inner diameter of
190 mm. Aging duration is planned from 1 day up to 5 years
and currently samples aged up to 2.5 years are investigated.
The combination of component test and material tests allows
correlating seal performance with changes in material properties
which is required to determine a suitable end of life criterion.
For our aging investigations we determine property changes of
the different elastomer materials due to thermo-oxidative aging
at elevated temperatures and test how typical methods of
lifetime extrapolation can be applied to these results [14, 15].
This approach enables us to detect and exclude undesired side
effects which very often influence lifetime estimations [16-20].
In the following text of this paragraph an overview of our so far
published results is given to set the framework for the additional
investigations presented in the main part of this contribution:
In [20] an in depth investigation of heterogeneous aging effects
was presented which focused on EPDM and HNBR samples
with an aging time of up to 180 days. The investigated
properties comprised compression set (CS), hardness,
compression stress relaxation and permeability. Based on these
results it was concluded that heterogeneously aged samples
should be excluded from lifetime estimations as they can falsify
the results if the conditions which led to the heterogeneous
aging are not expected during real service conditions.
Unfortunately, this is often the case if high acceleration of the
aging process is desired.
 In [21] results of the three rubbers aged for up to one year were
presented focusing on hardness and CS measurements. The
effect of aging on the glass rubber transition was shown and
first results from component tests using samples after 98 days
and 180 days aging at 150 °C were presented. After 98 days the
leakage rate of the tested samples remained very low and
therefore full functionality was shown despite the fact that e.g.
CS after 100 days showed already a very strong increase. After
180 days EPDM seals showed increased leakage which
correlates well with the CS increasing over 100 % which
indicates that the sample showed shrinkage in comparison to the
initial state and therefore a leakage path was formed. By use of
a hardness profile the heterogeneously aged samples were
identified and excluded from the performed lifetime estimation
based on CS data.
Overall, it could be concluded that the static leakage rate
measurements represent the ultimate performance criteria for
seals but are not sensitive to the observed changes of material
properties. The investigated seals showed constant (some even
improving) seal performance and then suddenly a complete
failure.
In [15] a method to differentiate the effect of chain scission and
additional crosslinking was presented. By combination of a
stress relaxation and a subsequent recovery measurement
performed on aged samples a deeper understanding of the
contribution of chain scission and crosslinking on the overall
observed changes of the material properties can be generated. It
was shown, as already known from the literature [22, 23], that
both effects are present in EPDM but that chain scission plays
an important role for the overall mechanical behavior of the
aged material.
In [24] heterogeneous aging was again addressed but with a
higher spatial resolution using indenter modulus measurements.
Additionally, CS data was used to perform a time estimation to
reach a CS of 50 % at 60 °C. The criterion was used as at that
time the highest CS values that were not DLO affected were
around 50 % CS. The extrapolation procedure used a combined
approach of time temperature superposition and Arrhenius
approach. As a result, 1.2 years for HNBR, 17 years for EPDM
and 29 years for FKM were determined to reach the defined
value of 50 % CS.
In this contribution, our results of changes in sample mass,
density and viscoelastic properties are presented. The
evaluation is performed on basis of these results and our
findings briefly described above. The aim is to show that the
use of a single material property to evaluate aging of a seal is
not sufficient and an in-depth analysis requires a combination of
different methods to understand the aging behavior, exclude
samples from aging conditions which caused heterogenous
aging and perform a conservative lifetime estimation which is
oriented on the real application conditions.
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EXPERIMENTAL
The samples used in this investigation are part of our
ongoing aging project and therefore the description given above
is applicable.
Sample weight
For monitoring of the sample weight specific samples
were aged uncompressed and repeatedly their weight was
determined by use of a lab balance with a resolution of 1 mg.
For comparison the weight was normalized to the initial weight
of the respective sample.
Density
Density measurements were performed at 23 °C using
the immersion method in water according to DIN EN ISO 1183
(A) with an analytical balance having a resolution of 0.1 mg.
Three samples from one O-ring of each material aged in
compression were tested and the average and standard deviation
is given.
Dynamic Mechanical Analysis
Dynamic Mechanical Analysis (DMA) is a scientific
thermal analysis method which uses a (small) sinusoidal stress
acting on the sample The sample deformation is analyzed in
dependence of temperature and frequency. From the ratio of
stress to strain the complex modulus is calculated. As polymers
show viscoelastic material behavior, a phase shift between
stress and strain is observed which is used to split the complex
modulus into two components, the storage modulus and the loss
modulus. The storage modulus is understood as a measure of
the purely elastic (Hookean) behavior and the loss modulus is a
measure for the part of energy which is converted into heat.
From the characteristic shape of these curves the temperature
range of transitions can be deduced.
Measurements were performed on cylindrical samples (diameter
2.5 mm) at 3.2 Hz in compression mode on a GABO Eplexor®
500 N device. The temperature was changed stepwise between
-50 °C and 50 °C.
Leakage rate after rapid partial release
Besides static pressure rise tests which were described
e.g. in [24], the pressure rise during rapid partial release was
measured using a device constructed in our department that is
described in detail in [11]. The device was designed for testing
the low temperature leak tightness, but can also be applied for
aged samples. It enables a release of the O-ring by approx.
0.2 mm from 25 % to 23 % compression in less than one second
during the pressure rise measurement. If the resilience of the
seal has decreased passing a certain point, the seal cannot
follow the decompression fast enough and a leak can open up.
One flange system containing an EPDM seal was tested by first
measuring the static pressure rise, then evacuating the inside of
the flange system again, and measuring the pressure rise during
partial release. One data point per second was recorded during
the static test, and one point every 0.4 seconds in the dynamic
test which is sufficient to detect a pressure increase and its time
dependency. After evacuation, data recording is activated. Then
the valve to the pump is closed, starting the pressure rise
 measurement. Subsequently, the partial release is applied and
the pressure is recorded for up to 45 min. If the seal remained
leak tight, i.e. showed no step like pressure increase due to the
partial release, it was recompressed to 25 % and aging was
continued.

RESULTS AND DISCUSSION

The mass change of the rubber materials with aging is
of interest for the evaluation of the seal performance as it can
indicate a change in the chemical of the material composition
(loss of volatile components and formation and subsequent loss
of volatile species) and additionally a potential volume loss
which could lead to formation of a leakage path. If the seal is
considered as a solid object blocking the gas transport it is
necessary that this object is able to keep the groove closed even
during aging. When aging leads to mass loss, this could have an
influence on the dimensions of the seal due to the
proportionality between mass and cross-sectional diameter.
Occurrence of a seal failure just by mass loss under the given
assumptions would require a mass loss of about 44 % for the
used degree of compression of 25 %.
The results are given in Figure 1.
EPDM and HNBR show a strong mass loss at an aging
temperature of 150 °C, whereas FKM shows only a slight mass
loss. At 125 °C only for HNBR a slight mass loss can be
observed. For lower temperatures none of the samples showed a
change in sample mass for the applied aging times.
The reason for the mass loss is assumed to depend on limited
evaporation of volatile compound components and the
formation of volatile species due to chemical aging.
As the chemical reactions caused by thermo-oxidative aging
include chain scission and crosslinking reactions [25], this
could also have an influence on the density of the materials. An
increase in density leads to size reduction of the seal and is
therefore also relevant for the discussion of seal performance.
The results are given in Figure 2. The error bars given in the
figure indicate standard deviation of the measurement results. In
several cases the deviation is very small and therefore the bars
are smaller than the symbols.

Figure 1: Mass loss over aging time for a) EPDM, b) FKM, c)

HNBR

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 Reasons for the increase in density are that due to aging
primarily the polymer chains are degraded and possibly broken
into volatile species which reduces the relative amount of
polymer in the compound or increases the relative content of
fillers which have a higher density [26]. Additionally,
crosslinking reactions create chemical bonds between polymer
chains which are therefore coming closer together which also
increases density [27, 28].
Taking into account a combination of both effects mass loss and
density increase of e.g. EPDM aged at 150 °C for 1 year (mass
loss of 13 %, increase in density of 8 %) a reduction in seal
cord diameter of about 10 % may result. This alone would not
affect the sealing function as the seal was initially compressed
by 25 %. But these changes also affect other material properties
as can be seen e.g. by DMA or CS [24]. As described in the
reference the EPDM seals aged at 150 °C showed increased
leakage after 180 days which shows that not a single but several
factors are responsible for the overall seal performance.
An example for material behavior changes with aging is given
in Figure 3 showing the results of DMA measurements on
HNBR aged at 125 °C.

Figure 3: Storage modulus over temperature of HNBR samples

aged at 125 °C for different aging times measured at 3.2 Hz.

For the unaged sample the storage modulus shows a typical

rubber curve. At low temperatures the material is in the glassy
state and has a rather high stiffness which shows a slight
decrease with increasing temperature. Starting at about -30 °C
the storage modulus shows a steep decrease from the GPa range
down to values below 100 MPa which represents the rubbery
region where the material shows its typical elastomeric
Figure 2: Normalized density over aging time for a) EPDM, b)
properties. This process is called glass-rubber transition.
FKM, c) HNBR
With increasing aging time the glass-rubber transition shifts to
higher temperatures and the storage modulus increases for
For aging at 150 °C the normalized density shows a similar
temperatures higher than the glass-rubber transition region.
trend as the mass loss. At 125 °C the aging effect is stronger for
Additionally, the transition becomes broader. This correlates
EPDM and HNBR and at temperatures of 100 °C and below
well with our previous results which showed e.g. increased
only a slight increase in density is observed.

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 hardness and a strong increase of compression set [15, 20, 21].
The storage modulus values of the sample aged for 1 year at
125 °C show that the material is no longer behaving like a
rubber. At room temperature the materials modulus is in the
GPa range and even above glass-rubber transition the material
is more comparable to plastics.
As it has been shown that the static leakage rate has only limited
sensitivity for the degradation of the seal material, other ways to
evaluate seal performance were sought. Moreover, seals can
remain leak tight even with only very low remaining sealing
force [2, 29]. However, this applies only to purely static
measurements with no margin for mechanical vibrations,
pressure cycling or thermal shrinkage during service [9, 30].
Therefore, a modified leakage test with quick partial release of
the seal was applied for testing the leak tightness under more
demanding conditions. In this dynamic test, the seal was
released from 25 % to 23 % compression in less than one
second during the pressure rise measurement. This measurement
was performed on an EPDM O-ring that had been aged at
150 °C. Figure 4a shows the pressure rise under static
conditions measured before each partial release.
Figure 4. Pressure rise leakage rate measurements for an EPDM
seal aged at 150 °C under (a) static and (b) dynamic test
conditions.
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It can be seen that the pressure rise is very small (indicating a
low leakage rate) and hardly changes when the seal ages up to
80 days at 150 °C. This agrees well with the other results of
leakage rate measurements. When subjected to the quick partial
release (Figure 4b), the sealing system remained leak tight after
up to 70 days of aging. However, after 80 days of aging an
enormous pressure increase (past the effective range of the
pressure sensor) was observed, meaning that a leak path had
opened up. The fact that the seal becomes untight after about
half a minute and not immediately (see Figure 4b) is due to the
manual operation of the system (delay between activation of
data recording, closing the valve to the pump, and applying the
partial release). Thus the time of the strong pressure increase
corresponds to the time at which the seal was partially released.
As the seal that was aged for 80 days at 150 °C failed the
dynamic test, the aging state of 70 days at 150 °C, which was
the last investigated aging state at which the seal remained leak
tight even in the dynamic test, was chosen for the end-of-
lifetime criterion. This criterion is not fully representative as
only two O-rings could be tested. However, as the chosen
criterion is conservative in several ways, variations between
different O-rings should be covered. For instance, the seal was
still fully functional after 70 days of aging at 150 °C, which
means that the actual failure occurs later. Furthermore, the
dynamic test might be more demanding than the actual (mainly
static) conditions during normal operation. For most designs,
possible vibrations are expected to be much smaller than the
decompression by 2 %, and changes in the O-ring dimensions
due to e.g. thermal variations would occur slower, giving the
elastomer more time to follow. Finally, O-rings are not freely
exposed to oxygen in many applications, but oxygen access is
restricted to one or both sides, leading to slower oxidative
degradation. Thus, the chosen criterion contains a safety margin
that is considered to cover the safety relevant aspects. For the
tested EPDM material and O-ring geometry, the aging state
after 70 days at 150 °C corresponds to a CS of 83 %, a decrease
of elongation at break by 90 % (relative), a density increase by
4.6 % and a decrease of the maximum loss factor by 48 % [31].
As CS values can contain an error of up to ± 3 % CS, 80 % CS
is chosen as a more conservative criterion. CS values around
80 % have already been mentioned as end-of-lifetime criteria
for O-ring seals [2, 32-34], but so far without supporting
experimental data. However, the obtained criterion is specific
for this EPDM material and geometry. Due to different aging
stabilities and degradation mechanisms, different materials
(even different EPDMs) would give different results. Therefore,
for determining the criterion for other materials (such as the
investigated HNBR), the test has to be performed with an O-
ring made of this material. But, as DLO effects have to be
avoided, aging of the HNBR O-ring would have to be
performed at 100 °C [20]. At this temperature, it would take a
long time to reach leakage failure, which is why no criterion
could be determined yet for HNBR. Furthermore, the formation
of a leak path depends on the geometry of O-ring and flange
 system, which is why the obtained result is valid only for the
tested O-ring and compression geometry.
Nevertheless, for a first approach in [31] a CS of 80 % was
proposed as lifetime criterion and based on this assumption a
lifetime of 48 years for the EPDM at a temperature of 60 °C
was estimated. By use of the same criterion for the HNBR
sample a lifetime of 3.6 years was estimated. As the FKM so far
has not reached a CS of 80 % for the lifetime estimation a
criterion of 65% was used which resulted in an estimated
lifetime at 75 °C of 40 years.
As pointed out above the investigations have to be extended to
test whether this criterion is also applicable for the other
materials but it can be concluded that for dynamic events a
certain spontaneous recovery of the seal is required. When
aging leads to changes that prevent this fast recovery, a leakage
path will be generated.
CONCLUSION
In this contribution we give an overview of our
ongoing aging investigation of EPDM, FKM and HNBR seals.
Already published results are summarized and extended by
some new results for different methods. The additional results
show that changes of a single material property might be small
if they were used as the only criterion to discuss seal
performance due to aging. The question how this property
relates with the real seal performance is often not easily to be
answered and therefore component tests are a useful extension
for the evaluation of the aging behavior.
The combination of different methods allows to achieve a better
understanding of the aging state and therefore perform more
realistic lifetime estimations. An important factor is to select
suitable aging conditions to avoid falsifying conditions which
lead e.g to heterogeneous aging. Additionally, a suitable lifetime
criterion is required. In our opinion this should be related to the
seal performance. For example, for a tested EPDM sample the
proposed conservative approach using a fast partial release of
the seal leads to an aging time of 70 days at 150 °C at which the
seal remains functional. The correlation with material properties
showed that for this aging state a CS of about 80 % is reached.
Therefore we used a CS of 80 % as criterion for our lifetime
estimations for this EPDM. Similar criteria were also presented
in the literature but typically without experimental justification.
The ongoing investigation of the influence of thermo-oxidative
aging on material properties and seal performance of the three
materials will be continued for a total aging time of up to
5 years and the additional results will be used to check the so
far performed estimations and to optimize the overall
description.
ACKNOWLEDGMENTS
Parts of the presented project were funded by the
German Federal Ministry of Economic Affairs and Energy
(BMWi, project no. 1501509) on basis of a decision by the
German Bundestag.
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Additionally, the authors want to express their gratitude to Felix
Denecke and Milan Goral from Bundesanstalt für
Materialforschung und -prüfung for performing measurements
and processing of raw data.
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