See discussions, stats, and author profiles for this publication at: https://www.researchgate.

net/publication/339711642

Investigation of Viton O-ring performance for the SABRE dark matter

experiment

Preprint · March 2020

DOI: 10.13140/RG.2.2.22183.91046

CITATIONS READS

0 139

5 authors, including:

Shahinur Rahman Wayne D. Hutchison

UNSW Sydney UNSW Sydney
13 PUBLICATIONS   25 CITATIONS    156 PUBLICATIONS   1,040 CITATIONS   

SEE PROFILE SEE PROFILE

Heiko Timmers
UNSW Sydney
155 PUBLICATIONS   2,710 CITATIONS   

SEE PROFILE

Some of the authors of this publication are also working on these related projects:

Indium Nitride View project

Tribology View project

All content following this page was uploaded by Shahinur Rahman on 05 March 2020.

The user has requested enhancement of the downloaded file.

 Investigation of Viton O-ring performance for the SABRE dark matter
experiment

Md. Shahinur Rahman1, 2*, Wayne D. Hutchison1, Lindsey Bignell2, Gregory Lane2, Heiko
Timmers1
1
School of Science, The University of New South Wales (UNSW), Canberra BC 2610,
Australia
2
Department of Nuclear Physics, Research School of Physics, The Australian National
University (ANU), Acton ACT 2601, Australia
*
Corresponding author email: Shahinur.rahman@student.unsw.edu.au

Abstract:

Viton O-rings will be used for critical seals of the liquid scintillator (LS) veto detector for the
SABRE (Sodium-iodide with Active Background Rejection) dark matter experiment in
Australia. These Viton O-rings have to maintain a leak-free seal under exposure to the LS for
the 3 to 5-years operational life of the experiment.

In this study, the combined effects of elevated temperature plus exposure to air and Linear
Alkyl Benzene (LAB) on the physical properties of Viton O-rings were investigated over time
using compression set measurements and Young’s modulus tests, ATR-FTIR spectroscopy,
and the analysis of solvent induced swelling. While some changes to the mechanical and
surface-chemical properties of the O-rings were observed, our measurements show the
degradation of physical and mechanical properties of the Viton O-rings were found to be more
pronounced under compression set conditions in air for the same temperature compared to
LAB at the same temperatures. Results confirmed both increased values of the compression set
and change in Young’s modulus. The ATR-FTIR results show that the effects of LAB on the
surface composition of the Viton O-rings were not significant. According to solvent swelling
analysis over time, the Viton O-rings are suitable for use with LAB as there was no obvious
physical and chemical property degradations at three different ageing temperatures (22ºC, 35ºC
and 55ºC). Furthermore, the overall conclusion is that the O-rings can be expected function
efficiently for much longer than the expected operating life of the SABRE experiment.

Keywords: Linear Alkyl Benzene (LAB), Viton O-rings, compression set, ageing, SABRE
dark matter

1
1. Introduction

Major portions of fluoroelastomer (FKM) productions are widely used as sealing materials
called ‘O-rings’ in different industrial applications, such as automobile, transportation,
aeronautical, aerospace, oil and gas production, chemical process plant, food and packaging,
pharmaceuticals, semiconductor fabrication technology and nuclear detector development
under different environmental conditions due to their excellent physical, chemical and
mechanical properties (Ref 1–8). Viton is a brand name of FKM, which is categorized under
the ASTM D1418 and ISO 1629 designation of FKM (Ref 1,2,11–19,3–10). In hydraulic and
chemical sealing applications, Viton O-rings are used to inhibit the leakage of gas and fluids.

Viton O-rings will be used as seal to make a liquid scintillator (LS) veto detector for the
SABRE dark matter experiment in Australia (Fig. 1). It will seal at the interface between
flanges and a veto vessel housing 10.5 tons (12 m3) of LS whose main chemical component is
purified Linear Alkyl Benzene (LAB). The SABRE dark matter experiment is planned to
operate for 3 to 5 years, so the Viton O-rings have to remain in good shape with proper
resilience to ensure the required contact pressure to avoid any LAB scintillator leakage from
veto vessel during the operational life of the SABRE experiment (Ref 20,21). Under practical
operating environments, Viton O-rings are exposed to single or combined effects of different
environmental factors such as the chemical medium, mechanical load stress, temperature and
oxidation, etc. (Ref 3,6,8,9,11,12,22). Through the adverse effects of environmental factors on
sealing materials, elastomeric seals gradually degrade over time and eventually bring about a
permanent failure of the seal (Ref 23,24). Therefore, the determination of the influence of the
environmental factors on the degradation mechanism of elastomeric materials is very important
for their practical use in both research and industry.

Studies to investigate the thermal degradation behavior of Viton, HNBR and NBR O-rings such
as accelerated ageing tests have been carried out for many decades (Ref 7,8,14,23,24).
According to Weitao et al. (Ref 23,24), the elastomeric seal degradation can be classified into
two ageing process: physical ageing and chemical ageing. Physical ageing occurs due to the
volatilization and loss of fillers, and loss of additives, and the rearrangement or rupture of
molecular chains. Chemical ageing occurs due to various oxidation reactions including cross-
linking and chain-scission. The change in the molecular network structure of elastomeric seal
is attributed to the competition between cross-linking and chain-scission (Ref 3–5,11–
13,15,23–25). In addition, excessive cross-linking can result in a denser molecular structure of

2
elastomeric materials, which can degrade the mechanical properties of Viton O-ring (Ref
23,24).

Fig. 1: Preliminary design of the liquid scintillation (LS) veto detector for the SABRE
experiment. NaI (Tl) detectors with copper enclosures will be mounted with flanges on holders
inside the LAB (Linear Alkyl Benzene) scintillator. The LS veto detectors will be used to reject
background radiation events to truly detect dark matter (Ref 20,21).

When elastomeric seals are used in hydraulic systems, hydraulic oil or fluid gradually diffuses
into the interior of the used seals that can lead to swelling of the seal network structures (Ref
6,17). In addition, fluid can dissolve or extract antioxidants (soluble components) from the seal
during practical operations, which could reduce oxidation resistance and degrade mechanical
properties of seal materials (Ref 23). To investigate the excellent seal effect under practical
working environments, Viton or other O-rings are subjected to compression stress and kept in
this state for a long period of time. The compression stress of Viton O-rings usually tends to
decrease with exposure time, which is attributed to stress relaxation and oxidation reactions
(Ref 4,23). Both the physical and chemical ageing processes could have an adverse effect on
the dynamic performance of Viton O-rings or other elastomeric seals (Ref 23,24), which could

3
reduce the service lifetime of O-rings and ultimately leads to leakage of fluids or gasses.
Moreover, the compression stress can inhibit thermo-oxidative aging and refrained oxygen
access (Ref 23).

Most of the research over the past few decades has focused on degradation behaviour and
mechanism of various nitrile butadiene, HNBR, EPDM and Viton O-rings in air, hydraulic oil
and chemical media at different temperatures with or without compression stress. In the case
of hydraulic oil or in a chemical medium, elastomeric O-rings are exposed to more severe and
complicated working environments such as working temperature, hydraulic oil and
compression stress, which results in complicated processes of sealing materials degradation
due to the combined effects of working environments (Ref 3–6,8–12,18,23,24,26–29).
Furthermore, the combined effects from two or three environmental factors leading to
elastomeric seals degradation can be more or less problematic compared to a single
environmental factor. On the one hand, compression stress and liquid environment could
inhibit oxygen access in sealing materials and slow down thermal degradation process; which
in contrast, compression stress can induce physical and chemical changes in elastomeric O-
ring materials such as compression stress relaxation, chain scission and rearrangement of
elastomeric molecular network structure, which could lead to significant seal material
properties degradation (Ref 23).

Studies of Viton O-rings subjected to compression stress in Linear Alkyl Benzene (LAB) with
accelerated ageing at elevated temperatures for a long time period are not available. However,
such long-term tests are very important in understanding the service lifetime and possible
changes in physical and chemical properties.

The aim of this project is to determine the Viton O-rings service lifetime with a compression
set experiment under different ageing temperatures (22ᵒC, 35ᵒC and 55ᵒC) in LAB scintillator
and air. To complement the results and interpretation, the physical, chemical and mechanical
properties changes of the Viton O-rings for interaction with LAB scintillator were investigated
with solvent swelling, Young’s modulus and attenuated total reflection- Fourier transform
infrared spectroscopy.

4
2. Experimental method

2.1 O-ring materials and Linear Alkyl Benzene

Black colour Viton O-rings (MET VITO, OR050X5V75) were purchased from M&G
Industrial Supplies, Fyshwick, Australia. The inner diameter and cross section diameter of
Viton O-rings were 50 mm and 5 mm, respectively.

Linear Alkyl Benzene (LAB) was purchased from Jintung Petrochemical Corporation Ltd.,
Nanjing, China for purification by the SABRE collaboration at the Australian National
University. The density of LAB was 0.858 ±0.004 g cm-3 at room temperature (22ᵒC). The
boiling temperature and flash temperature of LAB were specified as 311ᵒC and 147ᵒC,
respectively (Ref 30).

2.2 Compression set test

The compression set test of elastomeric seals under constant deformation gives information
about the reduction in cross-sectional thickness of seals over a time period at certain
experimental conditions as a percentage of the maximum deformation obtained in the
experimental jig (compression simulator). In order to investigate combined effects and service
lifetime in air and LAB for Viton O-rings at different temperatures, compression set tests were
conducted over 185 day periods using home-built compression simulators (Morrell et al. (Ref
25)) as shown in Fig. 2. The spacer dimension was Φ15 mm x 3.80 mm (cross sectional
diameter x height) to get a constant 25% initial compression value of the original seal thickness
followed by the standard test method (ASTM D395 B) for compression set (Ref 25,31). After
that, the O-rings under compression set in compression simulators were exposed to air or
immersed in Linear Alkyl Benzene. Then, the compression simulators loaded with compressed
O-rings were put in air-circulating ovens at 35 ᵒC or 55 ᵒC. The schematic diagram of
compression set tests for Viton O-rings at different ageing temperatures in air and LAB are
shown in Fig. 3. Moreover, three O-rings were used for each compression set test to obtain
reliable results and the averages of ten values measured on different positions on the O-ring
are reported in this research study.

The reduction in cross-sectional thickness of seals was measured at an arbitrary but fixed 30
min after release from the compression simulators (Ref 3,10,11,23,25). Compression set (%)
is calculated using the following equation (Ref 4,23,25):

5
 𝑑0 − 𝑑2
CS (%) = (1)
𝑑0 − 𝑑1

Where CS is the compression set, d0 is the original cross-sectional thickness of seal, d2 is the
final cross-sectional thickness (recovery thickness at 30 min after releasing from compression
simulator) and d1 is the space bar thickness.

Fig. 2: Compression set experimental set up of Viton O-rings with 5 spacers: (a) drawing of
the compression plates and spacers (Ref 25), and (b) photograph of the compression set
experiment with three O-rings being compressed, two O-rings can be seen at the front face.

6
Fig. 3: Schematic diagram of compression set test for Viton O-rings under different conditions:
(a) compression set in air at selected temperatures (22 ᵒC, 35ºC and 55ºC), (b) compression set
in Linear Alkyl Benzene liquid scintillator (LAB) at 22ºC and (c) compression set in LAB at
selected temperatures(35ºC and 55ºC).

2.3 Mass change measurements

Change in mass is the mass gain or mass loss of an elastomer in solvent due to swelling effects
over time. When an elastomeric seal is exposed to test liquid, it tends to undergo a certain
amount of swelling. The amount of swelling is proportional to the level of mutual solubility of
seal and liquid [6], [26], which can be determined via the accompanying mass gain and/or
volume increase observations. This mass gain and/or volume increase are attributed to the
diffusion of test liquid molecules into the seal network. To understand the compatibility
between an elastomeric seal and a liquid, solvent swelling experiment over time is carried out.

The measurement of swelling of the Viton O-rings in LAB with and without ageing over a
time period were conducted according to ASTM D 471 (Ref 32). Mass gain of the Viton O-
rings was measured with an electronic balance, which had a resolution of 0.001g. Three O-
rings were weighed in air separately, recorded mass as “m” for each O-ring individually, and
then immersed three O-rings in each glass jar containing 100 ml LAB scintillator at selected
temperatures (RT- 22ᵒC, 35ᵒC and 55ᵒC) over a certain period of time. After the immersion test
proceeded over a certain period of time, the O-rings were removed from the glass jars and then
placed on lint free tissue for around 60 min at room temperature in air to remove LAB from

7
the O-rings surfaces. To completely remove the LAB from the surface of O-rings, O-rings were
then dipped in acetone at room temperature for 2 minutes and blotted lightly with lint free
tissue. After that, each O-ring were again weighed in air to determine the mass of each O-ring
in air after immersion (M). After weighing the mass of O-rings, O-rings were again immersed
in LAB inside the glass jars to continue the solvent swelling experiments. The percentage
change in mass of Viton O-rings were calculated using the following equation:

𝑀−𝑚
𝑀𝑎𝑠𝑠 (%) = 𝑋 100 (2)
𝑚

Where m is the initial mass (g) of Viton O-ring in air and M is the final mass (g) of Viton O-
ring in air after immersion.

The mass loss of Viton O-rings due to ageing in air at different temperatures (35 ᵒC and 55 ᵒC)
was calculated using the equation 2, where M is the final mass (g) after ageing in air.

2.4 ATR-FTIR analysis

Attenuated total reflection- Fourier transform infrared spectroscopy (ATR-FTIR, Thermo

Nicolet 6700) was used to analyze the chemical structure changes on surfaces of Viton O-rings
under different ageing conditions. The range of spectra was 700 to 3300 cm-1 with a resolution
of 4 cm-1. The ATR-FTIR spectroscopy was carried out on O-ring surfaces with a diamond
crystal to understand the chemical changes. The scans at three different locations on each O-
ring were conducted to identify the functional peaks precisely. In addition, samples of the LAB
at different ageing conditions were also analyzed with ATR-FTIR spectroscopy.

2.5 Young’s modulus measurement

The Young’s modulus of compressed Viton O-rings exposed to different experimental

conditions were measured using a universal testing machine (Autograph AG-X 100 kN,
Shimadzu, Japan) following standard test methods (ASTM D 412) (Ref 31). The applied stress
was 900 N at the strain rate of 50 mm/min to understand the Young’s modulus of Viton O-
rings at different compression set conditions. Three O-rings of each experimental condition
over time were tested and the average values are reported in this paper. The Young’s modulus
was calculated using the following equation:

8
 𝜎
𝐸= (3)
∈

Where E is the Young’s modulus, σ is the applied stress and ∈ is the strain (proportional
deformation).

3. Results and discussion

3.1 Compression set test for Lifetime prediction

Compression set is chosen as the failure property of elastomeric seals for lifetime predictions
(Ref 3,4,11,13,25–27). The end of life of an elastomeric seal is taken to be considered when
compression set value reaches to 50% according to the standard ISO 11346 (Ref 27) or 80%
(Ref 19). The changes in compression set values of Viton O-rings exposed to different
conditions over time are shown in Fig. 4.

Fig. 4: Compression set value of Viton O-rings over time at different conditions: Viton O-rings
in air at 22ᵒC, 35ᵒC and 55˚C, and Viton O-rings in LAB at 22ᵒC, 35˚C and 55˚C.

9
The compression set value for all the O-rings gradually increased with increasing ageing
temperature over time, which could be due to both cross-linking and chain scission reactions
occurred simultaneously (Ref 8,27),(Ref 24). The cross-linking is predominant over chain
scission during compression set of elastomeric seals in the lower temperature range (Ref 24).
The compression set of O-rings in air was higher than in LAB for the same ageing temperature,
which suggests that more degradation occurs in air compression set experiment.

To calculate O-ring lifetime based on compression set tests, the measured compression set data
is usually extrapolated to a reference temperature (room temperature) using the time-
temperature shift, Arrhenius diagram and combination of both (Ref 4,11,19,22,25–27). The
Arrhenius equation is as follows(Ref 22):

𝐸𝐴
ln (aT) = - +C (4)
RT

Where ln (aT ) is the reaction rate for the process, aT is the shift factor, EA is the activation
energy, R is the gas constant, T is absolute temperature and C is a constant.

For time-temperature shift, compression set data obtained at different temperatures is shifted
along the logarithmic time axis until they superimpose to the lowest temperature compression
set data. Time -temperature shift usually gives a master curve for the reference temperature
(lowest temperature) that has not been shifted (Ref 8). Compression set data of Viton O-rings
in air at 35ᵒ and 55ᵒC was shifted in time (shift factor: aT) until the data superimposed on to the
22ᵒC reference temperature data shown in Fig. 5. In order to interpolate between measured
temperatures or extrapolate to other temperatures, the logarithm of the shift factors (ln (aT))
can be plotted versus the inverse temperature (T-1) in an Arrhenius diagram as shown in Fig. 6.
If the resulting graph is a straight line, it can give the shift factor for shifting the compression
set data to the desired temperature (Ref 8,25,27). The activation energy of Viton O-rings under
compression set in air was determined from the slope of Arrhenius diagram shown in Fig. 6
and found to be 50.0 ± 0.292 kJmol-1 , which corresponds well with the literature value (Ref
4). The activation energies basically depend on exact material composition and test method
(Ref 4). The time to reach the 22.33 % compression set value at 22 ᵒC is approximately 2035
days, 5.58 years, as shown in Fig. 5.

10
The master curve of compression set data for Viton O-rings immersed in LAB at 22 ᵒC obtained
from time-temperature shift up to 2090 days is shown in Fig. 7. The corresponding Arrhenius
diagram of shift factors is given in Fig. 8, which is also a straight line. The calculated activation
energy from Fig. 8 is 50.30 ± 0.369 kJmol-1, which is slightly higher than the activation energy
of compression set data in air as the degradation rate is higher for compression set in air. The
time to reach the 17.19 % compression set value at 22 ᵒC in LAB is approximately 2090 days,
5.73 years. In all cases, the compression set value increased with increasing ageing temperature
because the degradation rate increases with increasing the temperature (Ref 11,22,27,33). The
cross-linking reaction rate in O-rings under compression set usually increases with increasing
the ageing temperature , which increases degradation rate in elastomeric seals (Ref 23).

According to the lifetime prediction results shown in Fig. 5 and 7, O-rings used in practical
applications in contact with LAB at 22 ᵒC will function longer than those in air. The
compression set value of Viton O-rings in air and LAB reaches to 22.33% (5.58 years ) and
17.19 % (5.73 years), respectively. However in both cases, the end of seal lifetime is not
reached , because a 50% compression set value is considered as the end of seal lifetime (Ref
4,8,22). The extrapolated end of lifetime of Viton or FKM O-rings in air at 75˚C is 29 years
with 50% compression set value reported by Kommling et al. (Ref 4). Therefore, the Viton O-
rings will have useful lifetime of more than 29 years in LAB at 22 ᵒC in the SABRE dark matter
experiment assuming as the end of lifetime of Viton O-rings to be taken as 50 % compression
set value (Ref 4,8,33).

11
Fig. 5: Compression set (%) data in air time-temperature shifted to the reference temperature
22ºC with Arrhenius plot over 2035 days.

12
Fig. 6: Arrhenius diagram of shift factors (aT) for Viton O-rings compression set in air.

Fig. 7: Compression set (%) data in LAB time-temperature shifted to the reference temperature
22ºC with Arrhenius plot over 2090 days.

13
Fig. 8: Arrhenius diagram of shift factors (aT) for Viton O-rings compression set in LAB.

3.2 Analysis of mass change (%) of Viton O-rings

The mass gains (%) of Viton O-rings at different temperatures immersed in LAB over
time are shown in Fig. 9. The increase in mass (%) for three different swelling
conditions show a similar increasing trend over time. The mass (%) increases sharply
for all the O-rings during the first 6 days and then the mass gains level out over time. In
addition, less mass gain (%) is observed at higher ageing temperature which might be
due to higher stiffness and cross-linking in Viton O-rings (Ref 6,17). A higher ageing
temperature can induce more cross-linking in elastomeric materials which makes the
seal network structure denser and stiff, so less proportion of liquid can permeate into
the seal network (Ref 6,18). In addition, higher cross-linking could degrade the seal
recovery properties due to higher stiffness and denser network as the deformation
recovery behaviour of seal over time could reduce at higher stiffness and for denser
elastomeric network.

14
Fig. 9: Mass gain (%) of the Viton O-rings before and after ageing at different temperatures
in LAB. An increase in temperature presents a decrease in swelling.

According to Schweitzer et al., if elastomeric seals are exposed to heat, some seals will continue
to soften, and some will follow to harden (Ref 6). In addition, some will show an initial
hardening behavior followed by softening, which is dependent on the material of elastomeric
seal (Ref 6). According to the mass swelling (mass gain (%)) experimental results of Fig. 9,
Viton elastomers showed an initial gain in mass (sharp increase up to 6 days) after which their
mass followed plateau trends. Therefore, this can be interpreted as an initial softening following
by hardening prompted by ageing temperature and time. The initial softening behaviour lasting
of around 6 days likely corresponds to chain rupture in the elastomeric material. While the
plateau in mass gain follows sufficient chain re-growth (Ref 6).

A small amount of swelling of a seal in liquid (less than 10%) may actually improve the sealing
performance depending on elastomeric seal and application conditions. However, swelling
higher than 20% could result in seal failure (Ref 18). The highest mass gain (%) around 4.5
after 30 days was observed for Viton O-rings at 22 ᵒC according to the solvent swelling test,

15
which could link to their sealing performance (low level of swelling). Therefore, the
compatibility of Viton O-rings and LAB is found to be good.

In addition, Table 1 is a list of the mass loss (%) for the O-rings aged in air at different
temperature over time. The mass loss (%) of O-rings is comparatively higher for higher ageing
temperature which might reflect increasing volatility of small molecules including volatile
additives and oxidation induced small molecules. Usually, the volatilization rate is faster at
higher ageing temperature (Ref 24). The mass loss of O-rings under ageing in air denote
elastomeric materials property degradation.

Table 1 Mass loss (%) of Viton O-rings after ageing in air at different temperatures.
Time (days) Mass loss (%) at 35ᵒC Mass loss (%) at 55ᵒC

3 -0.037 ± 0.006 -0.0838 ± 0.004

8 -0.035± 0.008 -0.0823 ± 0.005
15 -0.06 ± 0.01 -0.103 ± 0.015
30 -0.07± -0.12

3.3 ATR-FTIR analysis

The ATR-FTIR spectroscopy is a viable technique to determine the chemical structure change
on the surface of elastomers (Ref 34)(Ref 35)(Ref 9). In this study, ATR-FTIR spectroscopic
analysis was carried out on both pristine Viton O-rings and those aged in air or LAB for 35
days to determine the chemical structure change on the surface of Viton O-rings before and
after ageing shown in Fig. 10. The peak assignments for the ATR-FTIR spectra of Viton O-
ring are shown in Table 2. The peak at 877 cm-1 is assigned to the stretching vibration of CF3
(υ (CF3)).

16
Fig. 10: ATR-FTIR spectra of both a pristine Viton O-ring and for those aged in air and LAB
at different temperatures for 35 days. Higher temperature in LAB shows chemical structure
changes on the surface of Viton O-rings.

The peak at 1010 cm-1 (υg (CF2)) was seen to decrease for Viton O-rings aged in LAB at 55ºC
but that peak did not change for the ageing tests in air at all temperatures. This could be
interpreted as a chemical structure change occurs in O-rings with ageing test in LAB due to
the volatilization and migration of additives and/or oxidation products of the aged O-rings, and
for loss of paraffin in LAB for the elevated temperature (Ref 23,24). The peak at 1644 cm-1
(υ(C=C)) disappeared for O-rings’ aged in air and LAB at 35˚C and 55˚C, which can corelate
with curing or oxidation throughout the ageing process (Ref 24). The intensity of peaks at 2845
cm-1, 2920 cm-1 and 2956 cm-1 increased slightly and broadened for ageing tests in LAB
compared to the pristine Viton O-ring and O-rings ageing in air (Fig. 10), which can be
attributed to the chemical reactions occurred between LAB and Viton O-rings.

17
 Table 2 Peak assignments for ATR-FTIR spectra of Viton O-rings.
No of Peaks Wavenumber (cm-1) Functional References
group/vibration

1 877 υ (CF3) (Ref 5,9,36)

2 1010 υg (CF2) (Ref 5,36)
3 1178 υa (CF2) (Ref 5,9)
4 1394 υ (CF) (Ref 5,9)
5 1644 υ (C=C) (Ref 5,9)
6 2845 υg (CH2) (Ref 5,9)
7 2920 υa (CH2) (Ref 5,9)
8 2956 υ(CH) (Ref 5)

Fig. 11 is the ATR-FTIR spectra of both pristine LAB and used LAB after use for Viton O-
rings ageing test at various temperatures for 35 days. The peak assignments of LAB before and
after ageing are shown in Table 3. The peaks at 699 cm-1 and 757 cm-1 are attributed to the
aromatic C-H external plane bending (monosubstituted benzene derivative) and aromatic C-H
bending, respectively. The peaks at 1378 cm-1, 1455 cm-1, 1491 cm-1 and 1550 cm-1 are assigned
to inner plane bending of C-H, bending vibration of -CH2-CH3, aromatic C=C stretching
vibration and aromatic C=C stretching vibration, respectively. The peaks at 2854 cm -1, 2926
cm-1 and 2957 cm-1 belong to asymmetric C-H2 stretching, symmetric C-H2 stretching and
aromatic C-H stretching, respectively. The ATR-FTIR spectra in the range 699 – 1550 cm-1
and 2854 – 2957 cm-1 confirms that the LAB is mainly composed of aromatic hydrocarbons
(benzene derivatives) with different length of carbon chain (Ref 9,23,37).

18
Fig. 11: ATR-FTIR spectra of both pristine LAB (unaged) and LAB after use for Viton O-
rings ageing with different temperatures for 35 days. Oxidation is more severe at higher
temperature which can degrade LAB chemical properties.

In addition, the intensity of absorption peaks at 1378 cm-1, 1455 cm-1, 2854 cm-1, 2926 cm-1
and 2957 cm-1 increased gradually with the increased the ageing temperature, which may be
due to the migration of additives and/or oxidation products of the aged Viton O-rings to the
LAB. This proposed migration of additives and/or oxidation products of aged Viton O-rings
in LAB at elevated temperature is supported by the peak intensity increase at higher ageing
temperature (Ref 23,24). Moreover, the oxidation of LAB is more apparent at higher ageing
temperature, confirmed by the increase in peak intensity of newly formed peak at 3655 cm-1
(-OH stretching) with higher ageing temperature (Ref 23,37).

19
 Table 3 Peak assignments for ATR-FTIR spectra of LAB.
No of Wavenumber (cm-1) Functional groups/vibrations References
Peaks
1 699 Aromatic C-H external plane bending (benzene (Ref 37–39)
derivative)
2 757 Aromatic C-H bending (Ref 37–39)
3 820 C-H bending (Ref 38,39)
4 1378 Inner Plane C-H bending (Ref 38,39)
5 1455 -CH2-CH3 bending (Ref
9,24,38,39)
6 1491 Aromatic C=C stretching (Ref 38,39)
7 1550 Aromatic C=C stretching (Ref 9,37,39)
8 2854 Asymmetric C-H2 stretching (Ref 39)(Ref
9,23,37)
9 2926 Symmetric C-H2 stretching (Ref 39)(Ref
9,23,37)
10 2957 Aromatic C-H stretching (Ref 38,39)
11 3655 -OH stretching (Ref 37)

Finally, it is noted that there were no remarkable changes in the intensity within relevant
spectral peaks of any of all the Viton O-rings (under compression set conditions) to the pristine
Viton O-ring. There are how chemical changes on the surface of Viton O-rings’ even at higher
ageing temperatures under compression set conditions. Indeed, Viton O-rings are very stable
in LAB.

3.4 Young’s modulus analysis

Observed changes in the Young’s modulus of Viton O-rings under compression set conditions
in air and LAB over time with different ageing temperatures are plotted in fig. 12. The Young’s
modulus of all the tested O-rings gradually increases with increasing exposure time and ageing
temperature. The Young’s modulus under compression set in air is higher than for O-rings
under compression set in LAB at same ageing temperature, which can be attributed to higher
cross-linking (Ref 23,24). The trends of Fig. 12 suggest that thermally induced cross-linking
of elastomeric seal in air is higher than cross-linking of elastomeric seal in liquid at the same
ageing condition. In addition, the seal material might be hardened gradually due to higher
cross-linking, which ultimately can degrade the sealing properties (Ref 18,23,24) .

20
Fig. 12: The changes in the Young’s modulus of Viton O-rings over time exposed to different
compression set conditions at different ageing temperature: compression set of Viton O-rings
in air at 22ᵒC (black colour filled squares), compression set of Viton O-rings in air at 35ᵒC (red
colour filled circles), compression set of Viton O-rings in LAB at 22ᵒC (blue colour upward
triangles) and compression set of Viton O-rings in LAB scintillator at 35ᵒC (cyan colour
downward triangles).

The higher Young’s modulus of O-rings under compression set in air compared to LAB
indicates more O-ring degradation occurs under compression set in air, matching the trend
found from the compression set test results.

21
4. Conclusions

The combined effects of ageing temperature, LAB immersion and compressive set tests on the
degradation of Viton O-rings were investigated as a function of time. The degradation in the
physical and mechanical properties of Viton O-rings were higher in air under compression set
conditions for the same temperature compared to the compression set tests in LAB, which is
confirmed from the increased value of compression set and Young’s modulus. The ATR-FTIR
results show that LAB does not affect the surface chemical property of Viton O-rings
remarkably. From the solvent swelling experimental observations, there is no obvious chemical
and physical compatibility issues between Viton O-rings and LAB at the ambient temperature
(22ºC). Elevation of the temperature is the dominant effect on physical property degradations
of Viton O-rings (not LAB exposure). Therefore, it can be concluded that the LAB will not
degrade the Viton O-rings property beyond normal lifetime (more than 29 years) under SABRE
dark matter experiment conditions.

Acknowledgements

Authors acknowledge the financial and intellectual support towards this research project from
the Department of Nuclear Physics, the Australian National University (ANU) and the
University of New South Wales (UNSW).

References

1. H. Schroeder, Fluorocarbon Elastomers, Rubber Technol., 1999, 2(8), p 410–437.

2. A.L. Logothetis, Chemistry of Fluorocarbon Elastomers, Prog. Polym. Sci., 1989,

14(2), p 251–296.

3. A. Kömmling, D. Wolff, and M. Jaunich, Investigation of Long-Term Behaviour of

Elastomeric Seals for Transport and Storage Packages, Ageing Mater. Struct. Towar.
Sci. Solut. Ageing Our Assets, 2017, p 17–25.

4. A. Kömmling, M. Jaunich, P. Pourmand, D. Wolff, and U.W. Gedde, Influence of

Ageing on Sealability of Elastomeric O-Rings, Macromol. Symp., 2017, 373(1), p 1–
10.

22
5. T. Sugama, T. Pyatina, E. Redline, J. Mcelhanon, and D. Blankenship, Evaluation of
the Performance of O-Rings Made with Different Elastomeric Polymers in Simulated
Geothermal Environments at 300°C, 2014,
https://www.bnl.gov/isd/documents/88370.pdf.

6. S. Salehi, C.P. Ezeakacha, G. Kwatia, R. Ahmed, and C. Teodoriu, Performance

Verification of Elastomer Materials in Corrosive Gas and Liquid Conditions, Polym.
Test., Elsevier, 2019, 75(October 2018), p 48–63,
doi:10.1016/j.polymertesting.2019.01.015.

7. T.W. GIANTS, “Vitron B O-Ring Resilience Study.Pdf,” (Los Angeles), 2001,

https://apps.dtic.mil/dtic/tr/fulltext/u2/a402958.pdf.

8. A. Kömmling, M. Jaunich, and D. Wolff, Ageing of HNBR, EPDM and FKM O-

Rings, KGK Kautschuk Gummi Kunststoffe, 2016, 69(4), p 36–42.

9. S. Mitra, A. Ghanbari-Siahkali, P. Kingshott, K. Almdal, H.K. Rehmeier, and A.G.

Christensen, Chemical Degradation of Fluoroelastomer in an Alkaline Environment,
Polym. Degrad. Stab., 2004, 83(2), p 195–206.

10. Y.-H. Qian, H.-Z. Xiao, M.-H. Nie, Y.-H. Zhao, Y.-B. Luo, and S.-L. Gong, Lifetime
Prediction of Nitrile Rubber under Compression Stress in Transformer Oil, 2016,
(Icmia), p 189–194.

11. C.S. Woo and H.S. Park, Useful Lifetime Prediction of Rubber Component, Eng. Fail.
Anal., Elsevier Ltd, 2011, 18(7), p 1645–1651, doi:10.1016/j.engfailanal.2011.01.003.

12. R.D. Stevens, Permeation and Stress Relaxation Resistance of Elastomeric Fuel Seal
Materials, SAE Tech. Pap. Ser., 2010, 1(724).

13. M. Jaunich, W. Stark, and D. Wolff, Comparison of Low Temperature Properties of

Different Elastomer Materials Investigated by a New Method for Compression Set
Measurement, Polym. Test., Elsevier Ltd, 2012, 31(8), p 987–992,
doi:10.1016/j.polymertesting.2012.07.016.

14. L. Lukács and E. Cséfalvay, Compatibility Study of Viton, NBR 70 and EPDM O-
Rings with Selected Solvents, Period. Polytech. Chem. Eng., 2017, 61(2), p 67–72.

15. N.G. Shimpi, A.D. Mali, and S. Mishra, Property Investigation of Surface-Modified
MMT on Mechanical and Photo-Oxidative Degradation of Viton Rubber Composites,

23
 Polym. Bull., Springer Berlin Heidelberg, 2016, 73(11), p 3033–3048.

16. G. Item, K. Words, and E. Date, “Acceptance Criteria Acceptance Criteria,” 2007.

17. M.D. Kass, S.J. Pawel, T.J. Theiss, and C.J. Janke, “Compatibility Study for Plastic,
Elastomeric, and Metallic Fueling Infrastructure Materials Exposed to Aggressive
Formulations of Ethanol-Blended Gasoline,” 2012, doi:10.2172/1039968.

18. J.G. Drobny, Compounds for O-Rings and Molded Goods, Fluoroelastomers
Handbook, 2nd editio, Elsevier, 2016, p 439–470, doi:10.1016/B978-0-323-39480-
2.00012-9.

19. A.K. and D.W. M. Jaunich, Investigations of Elastomeric Seals—Low-Temperature

Performance and Ageing Behaviour, 2017, 24(Chapter 30), p 1341–1354.

20. P. Montini, Dark Matter Search with the SABRE Experiment, Instrum. Detect., 2018,
p 5–8, doi:DOI: 10.1088/1742-6596/1342/1/012060.

21. M. Antonello, E. Barberio, T. Baroncelli, J. Benziger, L.J. Bignell, I. Bolognino, F.

Calaprice, S. Copello, D. D’Angelo, G. D’Imperio, I. Dafinei, G. Di Carlo, M.
Diemoz, A. Di Ludovico, W. Dix, A.R. Duffy, F. Froborg, G.K. Giovanetti, E. Hoppe,
A. Ianni, L. Ioannucci, S. Krishnan, G.J. Lane, I. Mahmood, A. Mariani, M.
Mastrodicasa, P. Montini, J. Mould, F. Nuti, D. Orlandi, et al., The SABRE Project
and the SABRE Proof-of-Principle, Eur. Phys. J. C, 2019, 79(4).

22. P. Brown, Roger and H. Greenwood, John, “Practical Guide to the Assessment of the
Useful Life of Plastics,” 2002.

23. W. Lou, W. Zhang, T. Jin, X. Liu, and W. Dai, Synergistic Effects of Multiple
Environmental Factors on Degradation of Hydrogenated Nitrile Rubber Seals,
Polymers (Basel)., 2018, 10(8), p 897.

24. W. Lou, W. Zhang, H. Wang, T. Jin, and X. Liu, Influence of Hydraulic Oil on
Degradation Behavior of Nitrile Rubber O-Rings at Elevated Temperature, Eng. Fail.
Anal., Elsevier, 2018, 92(November 2017), p 1–11,
doi:10.1016/j.engfailanal.2018.05.006.

25. P.R. Morrell, M. Patel, and A.R. Skinner, Accelerated Thermal Ageing Studies on
Nitrile Rubber O-Rings, Polym. Test., 2003, 22(6), p 651–656.

24
26. A. Kömmling, M. Jaunich, and D. Wolff, Revealing Effects of Chain Scission during
Ageing of EPDM Rubber Using Relaxation and Recovery Experiment, Polym. Test.,
2016, 56, p 261–268.

27. A. Kömmling, M. Jaunich, and D. Wolff, Effects of Heterogeneous Aging in

Compressed HNBR and EPDM O-Ring Seals, Polym. Degrad. Stab., 2016, 126, p 39–
46.

28. I. Repository, “Study of Stress Relaxation and Strain Recovery in Elastomeric

Compounds Used in Pipe Seals,” A. M. Prabhu, 1991,
doi:https://hdl.handle.net/2134/25928.

29. R. Padakan and S. Radagan, Evaluation of Benzenesulfonyl Hydrazide Concentration

on Mechanical Properties, Swelling and Thermal Conductivity of Thermal Insulation
from Natural Rubber, Agric. Nat. Resour., Elsevier Ltd, 2016, 50(3), p 220–226,
doi:10.1016/j.anres.2016.01.004.

30. J. Joutsenvaara and K. Loo, Analysis of Linear Alkylbenzene Samples with a Camera-
Based Equipment, 2017.

31. ASTM, Standard Test Method for Tensile Properties of Vulcanized Rubber and
Thermoplastic Elastomers—, ASTM D 412-06a, 2018, 598, p 143–152.

32. A. International, Standard Test Method for Rubber Property — Effect of Liquids 1,
Change, 2011, i, p 1–14, doi:10.1520/D0471-16A.

33. M. Jaunich, W. Stark, and D. Wolff, A New Method to Evaluate the Low Temperature
Function of Rubber Sealing Materials, Polym. Test., Elsevier Ltd, 2010, 29(7), p 815–
823, doi:10.1016/j.polymertesting.2010.07.006.

34. M.S. Rahman, U. Shaislamov, J.K. Yang, J.K. Kim, Y.H. Yu, S. Choi, and H.J. Lee,
Effects of Electron Beam Irradiation on Tribological and Physico-Chemical Properties
of Polyoxymethylene Copolymer (POM-C), Nucl. Instruments Methods Phys. Res.
Sect. B Beam Interact. with Mater. Atoms, Elsevier B.V., 2016, 387, p 54–62,
doi:10.1016/j.nimb.2016.10.001.

35. J.A. Hiltz, Characterization of Fluoroelastomers by Various Analytical Techniques

Including Pyrolysis Gas Chromatography/Mass Spectrometry, J. Anal. Appl. Pyrolysis,
Elsevier B.V., 2014, 109, p 283–295.

25
 36. P.B. Wagh, S. V. Ingale, R. Kumar, R.H. Naina, T.C. Kaushik, and S.C. Gupta, Impact
Sensitivity of RDX and Viton Compositions Prepared by Co-Precipitation Method,
Def. Sci. J., 2015, 65(4), p 287–291.

37. D. University of California, “Infrared Spectroscopy Absorption Table - Chemistry

LibreTexts,” 2019,
https://chem.libretexts.org/Ancillary_Materials/Reference/Reference_Tables/Spectrosc
opic_Parameters/Infrared_Spectroscopy_Absorption_Table. Accessed 9 July 2019.

38. S. Zor, B. Yazici, and M. Erbil, Inhibition Effects of LAB and LABS on Iron
Corrosion in Chlorine Solutions at Different Temperatures, Corros. Sci., 2005, 47(11),
p 2700–2710.

39. M.A. Mottaleb, Development of a HPLC Method for Analysis of Linear Alkylbenzene
Sulphonates and Detection by UV and FTIR Spectroscopy Using Thermospray
Interface, Mikrochim. Acta, 1999, 132(1), p 31–39.

26

View publication stats