International Journal of Civil & Environmental Engineering IJCEE-IJENS Vol:10 No:05 1
100905-5252-IJCEE-IJENS © October 2010 IJENS I J E N S
Determination of Structural and Dimensional
Changes of O-ring Polymer/Rubber Seals Immersed
in Oils
A.A. Roslaili1, A.S. Nor Amirah1, S. Mohd. Nazry2, K. Ain Nihla1
1School of Environmental Engineering, Universiti Malaysia Perlis, 02600 Jejawi, Perlis, Malaysia. 2School of Materials Engineering, Universiti Malaysia Perlis, 02600 Jejawi, Perlis, Malaysia.
Email: [email protected]
Abstract-- The purpose of this work is to investigate the
suitability use of vegetable-based oil in hydraulic system and
the compatibility between the rubber seals and lubricant
extracted from vegetable-based oil in hydraulic system. Two
types of o-ring rubber seals were used which are VITON and
NBR. These rubber seals were fully immersed in two different
types of oil, Seri Murni Palm Olein and Pennzoil 68 Hydraulic
Oil for two months. Detailed analysis of the rubber seals mass,
thickness and perimeter, swelling test, SEM and oxidation test
were done during the period in order to investigate the
dimensional and structural changes of rubber seals. The
viscosities of immersed oil were also tested to analyze its
impact and influence on the physical changes of seals. The
analysis was done using the ASTM standard method. Result
shows that the Seri Murni Palm Olein has the potential to be
used as hydraulic fluid especially when using with VITON seal.
However, some of physical and its chemical properties need to
be enhanced first such adding additives to the olein in order to
improve the effectiveness of the vegetable-based oil as
hydraulic fluid.
Index Term-- VITON, NBR, palm olein and mineral-based
hydraulic oil.
1. INTRODUCTION
Hydraulic fluids or hydraulic liquids are the
medium by which power is transferred in hydraulic
machinery. Examples of equipment that might use hydraulic
fluids include excavators, brakes, power steering systems,
transmissions, backhoes, garbage trucks, aircraft flight
control systems and industrial machinery. Reports indicated
that nearly 38 million metric tonnes of lubricants were used
globally in 2005, with a projected increase of 1.2 percent
over the next decade (Kline, 2004–2014). Approximately
85% of lubricants being used around the world are
petroleum-based oils (Loredana, 2008). Use of hydraulics is
expanding, and consumption of hydraulic fluids today
constitutes a significant part of the world’s total
consumption of defined mineral oils, approximately 1
million tonnes per annum or around 10%. Continuing efforts
to achieve improved efficiency resulted in development of
fluids with higher quality, displaying longer life and
providing better protection for hydraulic components under
operating conditions (Shashidhara & Jayaram 2009). Plus,
stronger environmental concerns and growing regulations
over contamination and pollution will increase the need for
renewable and biodegradable lubricants.
Vegetable oils, especially palm oil was considered the
most likely candidate for a fully biodegradable hydraulic
fluid. Plant oil is a natural resource available in abundance.
Vegetable oils have already been considered as potential
industrial fluids as early as the 1900s (Oommen &
Claiborne,1999). Vegetable oils with high oleic content are
considered to be potential candidates as substitutes for
conventional mineral oil-based lubricating oils and synthetic
esters (Randles and Wright, 1992; Asadauskas et al., 1996).
The use of vegetable oils as hydraulic fluid would help to
minimize hazardous pollution caused by accidental spillage,
lower disposal costs of the used fluid, and help the user
industry to comply with environmental safety regulations
(Nik et al., 2005). Due to the advance of petrochemical
industry development, the readily available of petroleum
oils replaced vegetable oils for reasons of lubricity, stability,
and economics. Recently, environmentally related issues
that include biodegradability, toxicity, occupational health
and safety, and emissions have created important issues to
be revealed and reconsidered especially the use of mineral
oils in environmental sensitive areas.
There are many factors can reduce the service life of
hydraulic components. An elastomeric o-ring is one of the
most widely used sealing components in mechanical
systems. It is the most critical elements in a hydraulic
system and are typically manufactured from PTFE,
polyurethane or an elastomer (Frank et al., 2006). The seal
functions to prevent leakage of hydraulic fluid into the
surroundings and to exclude contaminants. It is the unique
characteristics of the elastomer material used in o-rings that
makes the o-ring such a good seal. The special
characteristics of o-ring include the circular cross section
provides minimum surface area, which enhances resistance
to abrasion, fluids, adverse environments, and arid
mechanical damage and it will fit into confined spaces
without the need for bulky, adjustable, or expensive support
structures The elastomer, a highly viscous, incompressible
fluid with high surface tension, has a capacity for
remembering its original shape for a long time (George et
al., 2004). Therefore, in order to ensure successful long-term
operation of a hydraulic system the seal components should
be manufactured for maximum compatibility. Thus, the
approach of this study is to evaluate the relationship
between the seal and the potential lubricant from vegetable
oil, as both elements are important mechanisms in a
hydraulic system.
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2.0 SAMPLE PREPARATION
Two types of o-ring seal investigated are Fluoroelastomers
(VITON) and Acrylonitrile-Butadiene Rubber (NBR).While
for oil samples, two types of oils were used which are Seri
Murni Palm Olein and Pennzoil 68 Hydraulic Oil. The oils
were filled in the boiling tube about 50 mL and immersed in
an oil bath at 70oC and pressure at 1 atm. VITON and NBR
were centred cut, tied with the black threads, labelled, and
put into boiling tube containing oil samples according to the
labels (as explained in Table I) for about two months. The
dimensional changes tests were carried out for every two
weeks.
Table I
Label of Rubber Seals and Oils
Label of Boiling Tube Types of Rubber Seal Types of Oil
VIT 1 VITON Seri Murni Palm Olein
VIT 2 VITON Seri Murni Palm Olein
VIT 3 VITON Pennzoil 68 Hydraulic Oil
VIT 4 VITON Pennzoil 68 Hydraulic Oil
NBR 1 NBR Seri Murni Palm Olein
NBR 2 NBR Seri Murni Palm Olein
NBR 3 NBR Pennzoil 68 Hydraulic Oil
NBR 4 NBR Pennzoil 68 Hydraulic Oil
Fig. 1. Schematic Diagram of Boiling Tubes in Oil Bath
3.0 TEST EQUIPMENT AND PROCEDURE
3.1 Dimensional Changes of Seal (VITON and NBR)
Test
The rubber seals dimension was measured using Vernier
Caliper. Dimensional changes of the seals were measured
based on its perimeter and width of the seals, as according to
the ASTM D471: Liquid Immersed Properties Test to
measure the changes in weight and dimension (depth and
perimeter) of materials immersed. Readings for the seals
dimension were taken four times in every two weeks
3.2 Changes in Mass Test
The mass of seals rubber were weighed using Digital
Analytical Balance after taking out from the boiling tube
containing oil samples. Before weighing, the seals were
cleaned with dilution water and dried properly using filter
paper. All the measurement was recorded and changes in
mass were determined four times along the immersion
period.
3.3 Swelling Test
Swelling test was performed according to ASTM D3616:
Swelling Test by immersing the rubber seals in those oils at
25ºC for 72 hours. The rubber seals were weighted before
and after removed from the oils.
The swelling ratio (Q) was calculated according to the
following equation:
Where;
Wd = Seals weight before swelling
A6
Stainless Steel
Tube Rack
Test
Boiling Tube
Q = 1+ (Ws-Wd)ρp
Wd (ρs)
A1
A8 A7 A2
A6 A5 A4 A3
A1
000
0
A9 A10
A1
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Ws = Seals weight after swelling
ρs = is the density of the solvent,
ρp = is the seal density.
3.4 Viscosity Test
A Brookfield (Viscometer model DV-I+) rotational type
viscometer was used to measure the viscosity of oil samples.
S61 spindle has chosen and was operated at different speeds
between 10 and 100 rpm. For both oil samples the viscosity
and percentage of torque were manually recorded when the
viscosity reading reached apparent equilibrium (appears
relatively constant for reasonable time).
3.5 Oxidation Test
The oxidation performance of test oils is when the test oils
are aged for three days in beaker at temperature of 95 C
while ambient air is introduced and a copper wire is
immersed periodically. At the end of the test viscosity of
test oils is tested and the viscosity increase by oxidation
must not exceed 20%.
3.6 Scanning Electron Microscope (SEM) Test
The scanning electron microscope (SEM) model was used to
observe the morphology of VITON and NBR before and
after the immersion test.
4.0 RESULTS AND DISCUSSION
a) Structural and Dimensional Changes of Rubber Analysis.
Figure 2 shows the seal deformation before and after immersion process. Both of seals NBR and VITON tend to swollen and
shrunken after immersion in both oils.
(a) VITON Before Immersion (b) VITON Minor Changes After Immersion
(a) NBR Before Immersion (b) NBR Harden After Immersion
Fig. 2. Seal Deformation After and Before Immersion
VIT 1
VIT 4
111
VIT 2
111
VIT 3
NBR 1
NBR 4
NBR 3 NBR 2
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Fig. 3. Changes in Mass with Time
Figure 3 shows changes in mass of VITON and NBR o-ring
seals before and after immersed in oil bath with different
types of oil. It shows the mass of VIT 1 & 2 (immersed in
Seri Murni Palm Olein Oil) were significantly increased
with increasing time. The results of VIT 1 & 2 was started
with increased of mass value from range 0.05 g up to 0.3 g
and raised until 0.4 g. Same thing goes happened to VIT 3 &
4 which were immersed in Pennzoil 68 Hydraulic Oil. The
results value at the beginning of experiment was 0.05 g then
increased to the 0.3 g and rose up until 0.3 g. However,
results of NBR 1 & NBR 2, which immersed in vegetable
oil shows the fluctuation reading. The mass of both seals
were first begin to increase but then decreased and rose
again. It shows that the NBR 1 & 2 was shrunken at the
beginning of the experiment conducted due to the mass
value which indicates negative sign (-0.07 g decreased to -
0.08 g) and tend to swollen at the final stage up to 0.21 g).
While NBR 3 & NBR 4 (immersed in Pennzoil 68
Hydraulic Oil) shows the result were quite fluctuated but
unobvious. There is not much different values for NBR 3 &
4 which were swollen ( -0.01g to -0.04 g) and increased for
about 0.16 g at the final experiment. This proven that
VITON is more compatible to be use with vegetable oil.
The effect of increased of mass on their physical
properties deserves careful consideration. The enhancement
of rubber properties with increased molecular weight has
been known for many years but development has been
limited, because of the difficulty of processing these high
molecular weight rubbers. However, for high pressure and
high temperature sealing applications, as in the oil industry,
only high molecular weight rubbers are suitable, since they
possess low compression set along with other desirable
functional properties.
Figure 4 and 5 shows the results of thickness and perimeter
changes of the seals. The thickness and perimeter of seals
were not consistent where the readings were fluctuated. For
widthness changes, it clearly shown that NBR 3 & 4
undergone the most reduction of width started from 0.4 mm,
decreased to 0.2 mm and then sink to 0.02 mm. Based from
the results obtained, shows that when the reading of the
mass and dimensional changes is decreased, those
elastomers were shrunk as well. Based from results obtained
it can concluded that a few factors results in changes in
mass, structural and dimensional in VITON and NBR.
VITON well known for its excellent heat resistant which is
200°C.It offers excellent resistance to aggressive fuels and
chemicals (Du Pont 2009) and it shows small changes when
expose to oil and fuel. While NBR is good oil resistant, its
physical and chemical properties vary depending on the
polymer’s composition of nitrile the more nitrile within the
polymer, the higher the resistance to oils but the lower the
flexibility of the material (Du Pont, 2009). There also few
factors influencing the capability of elastomers such as
oxygen attack, effect of liquid, cross linking of polymers,
and degradation of mineral oil.
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Fig. 4. Changes in Width with Time
Fig. 5. Changes in Perimeter with Time
The more serious cause of deterioration in rubbers is its
reaction with atmospheric oxygen. This is possible because
rubber is a diene polymer and some; NBR and VITON
have olefinic double bonds in their structure. Oxidative
degradation of unvulcanized elastomeric, is resistant in
storage or in service as their aging behaviours.
Unvulcanized elastomer compound has to be vulcanized in
order to produce usable products. The nature of the cross-
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link produced varies considerably, and this can affect the
balance of chemical and particularly of physical properties
of the vulcanizates.O-Ring surfaces contains many flaws,
where cracks can be initiated via ozone attack. Increasing
stress will increase the number of flaws, which leads to a
larger number of cracks. The depth of the cracks is
inversely related to their number, and so, low stresses that
produce long deep cracks are more damaging to elastomer
seals than high stresses.
Furthermore, low molecular weight compounds (non-
polar) have sharply defined maximum levels that will
dissolve in oil. Elastomer on the other hand, first swells,
absorbing the fluid without true solvation occurring. An
increasing amount of fluid is absorbed, leading first to the
formation of a gel and finally a true solution (Abu Abdeen
& Elamer, 2009). Firstly, a rapid uptake of fluids occurs,
reaching a fairly well defined equilibrium state, and then
secondly fluid is absorbed slowly at an approximately
constant rate. This second stage does not take place in the
absence of air, and it is therefore assumed that it is related
to irreversible breakdown of the rubber.
Cross linking is a process of forming a three-
dimensional network structure from a linear polymer by a
chemical and physical method a cross linking process can
be classified into addition, substitution, and elimination
reactions, or it can involve two or even all of these.
Elastomers can degrade in chemical seal environments
through reactions with the polymer backbone and crosslink
system, or by reactions with the filler system. Presence of
the polar side-groups in the backbone chain increases the
oil resistance of the polymer (Patil & Coolbaugh, 2005).
Cross linking also limits the degree of polymer swelling by
providing tie-points (constrains) that limit the amount of
solvent that can be absorbed into the polymer (Hoffman,
2001 ). NBR is a copolymer of acrylonitrile and butadiene.
NBR is a low-cost elastomer with good mechanical
properties. The concentration of acrylonitrile in the
copolymer has a considerable influence on the polarity and
swell resistance of the vulcanizates in non-polar solvents.
The greater the acrylonitrile content, the lesst he swell in
motor fuels, oils, fats and other (Hoffman, 2001) However,
the elasticity and low temperature flexibility also become
poorer. NBR seals in both oils remain almost unchanged
compared to VITON seals. This added by the cross-linking
of polymers in VITON seals (which are synthetic seal) that
reduced the capability of the elastomer in palm olein. This
may be influenced by the higher fat content in palm olein.
b) Swelling Analysis
Swelling ratio of NBR and VITON shows VITON is relatively
good in term of swelling for both different oils compared with
NBR immersed in Seri Murni Palm Olein was relatively high
(1.63) compared to NBR immersed in Pennzoil 68 Hydraulic Oil
(0.431).The analysis of swelling is represented in Table II. This
phenomenon is referred as swelling, which normally takes place as
liquid is absorbed. The diffusion rate of liquid into a seal test will
determine the time taken to reach equilibrium. After that, the rate
of absorption of liquid slows. The lower the viscosity of the liquid,
the higher the diffusion rate. (Challapa Chandsekaran ,2010).
The major changes of volume noticed after immersion of a NBR in
a vegetable oil for a specified period. This shows that NBR seals
absorbed more vegetable oil rather than mineral oil.
Table II
Swelling Ratios of NBR and VITON
O-Ring Seals Oil Swelling Ratio
VITON Pennzoil 68 Hydraulic Oil 1.0058
Seri Murni Olein Palm Oil 0.9750
NBR Pennzoil 68 Hydraulic Oil 0.4319
Seri Murni Olein Palm Oil 1.6300
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Fig. 6. SEM images VITON and NBR
SEM images of NBR (a) before immersing in oil, followed
by after immersion in Seri Murni Olein Oil (b) and (c) in
Pennzoil 68 Hydraulic Oil. SEM images of VITON before
immersion (d ) followed by immersion in Seri Murni Olein
Oil (e) and in Pennzoil 68 Hydraulic Oil (f) shows in Figure
6.NBR relatively undergone a huge cracking effect and it’s
swollen drastically after immersed in Seri Murni Palm
Olein. VITON however shows small cracking and
unobvious swelling effects when immersed in palm olein.
The seals deteriorates because of oxidation at an elevated
temperature; as it tooks up large quantity of oxygen. This
led to the increase in weight of seals. Oxidation of rubber
may take place in three ways; (i) deterioration throughout
the rubber, (ii) formation of a film on the surface of the
rubber, and (iii) ozone cracking. Ozone cracking is
considered unlikely to be happened but because only very
small traces of gas are needed to initiate the cracking, have
succumbed to the problem. Ozone attack will occurs at the
most sensitive zones in a seal, especially the sharp corners
where the strain is greatest when the seal is flexing in use.
The corners represent stress concentrations, so the tension is
at a maximum when the diaphragm of the seal is bent under
air pressure (Asadauskas, 2007).
In an atmosphere, stretched samples of VITON and NBR
has developed surface cracks which grows in length and
depth until they eventually breakdown the test piece. Even
when they are quite small, they can cause a serious
reduction in strength and fatigue life (Gent, 2005). The
aging of rubber is caused by oxidative degradation in the
physical and mechanical properties of vulcanized rubbers
(Li-Gui & Koenig, 2005). This has be seen the SEM images
clearly proved through the SEM images where that, VITON
is suitable to be used with vegetable oil due to the minor
deteriorations.
c) Viscosity Analysis Figure 7,8,9,10,11 and 12 shows the results of viscosities for both
oils. In this study the speed used were 10 RPM, 20 RPM, 50 RPM
and 100 RPM. As speed increase, the velocity will decrease. The
velocity of Pennzoil 68 Hydraulic Oil is higher than Seri Murni
Palm Olein Oil. The viscosity was decreased with increasing time.
It happens for both samples Pennzoil 68 Hydraulic Oil and Seri
Murni Palm Olein.
30X 500X
(a) (b) (c)
500X
30X 500X 500X
(d) (e) (f)
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Fig. 7. Viscosity of Pennzoil 68 Hydraulic Oil at Speed 10 RPM
Fig. 8. Viscosity Seri Murni Palm Olein versus Time at 10 RPM
Fig. 9. Viscosity Pennzoil 68 Hydraulic Oil versus Time at 10 RPM
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Fig. 10. Viscosity Seri Murni Olein Palm Oil versus Time at 20 RPM
Fig. 11. Viscosity Pennzoil 68 Hydraulic Oil versus Time at 20 RPM
Fig. 12. Viscosity Seri Murni Palm Olein versus Time at 50 RPM
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Fig. 13. Viscosity Pennzoil 68 Hydraulic Oil versus Time at 50 RPM
Fig. 14. Viscosity Seri
Murni Palm Olein versus Time at 100 RPM
Fig. 15. Viscosity Pennzoil 68 Hydraulic Oil versus Time at 100 RPM
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The range of viscosity is unstable especially when the
speed is lower. At lower speed of 10 RPM, A4 and A8
shows the lowest reduction of viscosity. The results varied
from 33 cP to 62 cP and from 44 cP to 115 cP. Viscosity is
tending to increase at speed of 50 RPM and above and
achieved the highest stability at 100 RPM. This can be seen
when NBR seals immersed in both oils they shows the
viscosity of the oils were much higher and reduced unstable
at lower speed compared to when immersed with VITON.
At lower speed of 10 RPM, the lowest reduction viscosities
were shown by A5 and A7 where the results ranged from 40
cP to 67 cP and from 54 cP to 113. At speed of 20 RPM, A4
shows the lowest reading for vegetable oil (33 cP to 62 cP)
while A8 shows the lowest reading for Pennzoil oil (43 cP
to 114 cP).
The viscosity also affected by immersion of seals in
both oils. Viscosities tend to be stable at speed of 50 RPM
and above and achieved the highest stability at 100 RPM.
A3 and A8 at speed of 50 RPM show the highest reduction
result of viscosities. A3 (NBR immersed in vegetable oil)
shows the viscosity range from 26 cP to 58 cP .While for A8
(NBR immersed in Pennzoil Oil) shows the results from 29
cP to 109 cP . The highest stability was of achieved at speed
of 100 RPM which performed by A5 and A9, that are
VITON immersed in both samples. Both show the best
performance of all by undergone the smallest reduction
reading of viscosities. Final stage of oxidation resulted in
more changes that are significant in viscosity. Thus, we can
see the different ranges of viscosity at initial and after
completing the experiment.
Moreover, the changes of viscosity can be seen in their
colour .At the beginning of study the colour of the oil was
thick and more viscous. After two months, the colours seem
to be lighter and less viscous. Figure 16 represents the
colour of the oils at beginning of the project and after two
months. This is because oils will decay during the lifetime
of the lubricant either; in storage or during the application.
The physical and chemical changes that occur within the oil
during oxidation are likely to have an impact on the
lubrication performance, which shows on the colour changes
of both oils. Moreover the viscosities for both oils also
being affected by oxidation of the seals and oil. Heat is one
of the factors of oxidation, which for every 8ºC of
increasing temperature, the rate of oxidation will be twice.
Oxidation will attack the elastomers and this has lead to
“dehydrofluorination” and the degradation of the seal itself.
Vegetable oils also show poor corrosion protection (Ohkawa
et al., 1995). The presence of ester functionality renders
these oils susceptible to hydrolytic breakdown (Rhodes et
al., 1999).
Fig. 16. Colour Changes of the Oils:
(A) At the Beginning of the Project and, (B) After Two Months Project Completed
5.0 CONCLUSIOS
It can be concluded that Seri Murni Palm Olein is actually
has a big potential to be used as hydraulic fluid. There are
few unique characteristics and advantages of palm olein, as
such it is a potential candidate to replace the function of
conventional mineral-based lubricating oil. Moreover, palm
olein is highly non-toxic and exhibits a ready
biodegradability, good lubricity and cause fewer health
problems (Vizintin et al., 2002). It even possible to provide
satisfactory high performance as a functional fluid due to its
good resistance to oxidation and formation of breakdown
products at high temperatures and longer shelf life of
finished products. Moreover, products derived from them
are generally environmentally friendly (Gryglewicz et al.,
2003). Meanwhile VITON shows minimum changes of
structural and dimensional in both oils and successfully to
be applying together with vegetable-based hydraulic oil. Its
synthetic characteristics are more compatible with Seri
Murni Palm Olein, as it is easily oxidized and quickly react
compared to NBR seals. However due to some constraints
during their usages in hydraulic system such as oxygen,
water, air pressure and heat, suitable additives should be
added in order to improve the effectiveness of the palm
olein as hydraulic fluid. Seals’ durability also can be
enhanced by different additives, as example antioxidants
from phenolic and aminic as they offer flex fatigue and
ozone protection as well.
6.0 RECOMMENDATIONS
For structural and dimensional changes test, they should be
carried out in longer period of times and in a few interval of
time thus the changes can be regularly monitored.While for
o-ring seals, perhaps elastomers seals need not be cut down
to prevent and retain the origin formation of seals. The
cross section of the o-ring itself should be manipulated so
that we can see the consistency of the changes with
different diameters of seals. Plus, in order to improve on the
properties of vegetable oils, the glycerine molecule of the
vegetable oil can be substituted with a hindered alcohol.
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This improves the thermal, oxidative andhydrolytic stability
of the oil significantly without affecting much on the
biodegradability.
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