Determination of Structural and Dimensional Changes of O ...ijens.org/100905-5252...

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.

mailto:[email protected]

http://en.wikipedia.org/wiki/Hydraulic_machinery

http://en.wikipedia.org/wiki/Hydraulic_machinery

http://en.wikipedia.org/wiki/Excavator

http://en.wikipedia.org/wiki/Brake

http://en.wikipedia.org/wiki/Power_steering

http://en.wikipedia.org/wiki/Transmissions

http://en.wikipedia.org/wiki/Backhoe

http://en.wikipedia.org/wiki/Garbage_truck

http://en.wikipedia.org/wiki/Aircraft

http://en.wikipedia.org/wiki/Flight_controls

http://en.wikipedia.org/wiki/Flight_controls



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



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



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.



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-



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



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)



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



Fig. 10. Viscosity Seri Murni Olein Palm Oil versus Time at 20 RPM


Fig. 12. Viscosity Seri Murni Palm Olein versus Time at 50 RPM




Fig. 14. Viscosity Seri

Murni Palm Olein versus Time at 100 RPM




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.



This improves the thermal, oxidative andhydrolytic stability

of the oil significantly without affecting much on the

biodegradability.

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