Energy 54 (2013) 167e173

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Energy
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Wear prevention characteristics of a palm oil-based TMP

(trimethylolpropane) ester as an engine lubricant
N.W.M. Zulkii a, *, M.A. Kalam a, H.H. Masjuki a, M. Shahabuddin a, R. Yunus b
a
b

Department of Mechanical Engineering, University of Malaya, Kuala Lumpur 50603, Malaysia

Institute of Advanced Technology, University Putra Malaysia, 43400 Serdang, Selangor, Malaysia

a r t i c l e i n f o

a b s t r a c t

Article history:
Received 2 September 2012
Received in revised form
9 January 2013
Accepted 14 January 2013
Available online 17 February 2013

This paper presents the experimental results carried out to evaluate wear prevention characteristics of
a palm oil-based TMP (trimethylolpropane) ester using a four-ball machine for different regime of
lubrication. The TMP ester is produced from palm oil, which is biodegradable and has high lubricity
properties such as a higher ash point temperature and VI (viscosity index). Three different regimes of
lubrications are investigated, which hydrodynamic, elasto hydrodynamic and boundary lubrications.
Under these test conditions, the wear and friction characteristics of different TMP samples are measured
and compared. For boundary lubrication, it is found that up to 3% addition of Palm oil-based TMP ester in
OL (ordinary lubricant) decreases the maximum amount of WSD (wear scar diameter) and reduces (COF
coefcient of friction) up to 30%. Highest amount of load (220 kg) carrying capacity was also found from
the contamination of 3% TMP. For hydrodynamic lubrication, addition of 7% of TMP reduces the friction
up to 50%. It is well known that mechanical efciency of machinery component increases with
decreasing COF. The results of this investigation will be used to develop new and efcient lubricant to
substitute the petroleum-based lubricant partially for automotive engine application.
2013 Elsevier Ltd. All rights reserved.

Keywords:
Sliding wear
Biolubricant
Coefcient of friction
Lubrication

1. Introduction
There has been enormous interest in the use of oils from
renewable sources such as animal fats, vegetable oils and biolubricants [1e3]. The uncertainty of the crude oil supply, pollutants
emissions and its higher price give biodegradable biolubricants
more advantages over mineral base oils. However, vegetable oil in
its natural form has limited usage due to its poor oxidation stability
[4] and inferior low temperature properties [5]. The rst biodegradable lubricants were developed for two-stroke outboard
engines in the early 1980s, using neopentylpolyol esters of
branched-chain fatty acids as based uids [6]. Eychenne and
Mouloungui [7] have reviewed the developments in environmentally friendly lubricating oils based on neopentylpolyols such
as neopentyl glycol, pentaerythritol and trimethylolpropane. Other
researches [8,9] have worked on engine oil prepared from a mixture of trimethylolpropane esters having both sufciently high
viscosity and low pour point. Jayadas et al. [10] found that coconut
oil could be a good boundary lubricant as far as the coefcient of

* Corresponding author. Tel.: 60 3 79675204; fax: 60 3 79675317.

E-mail address: nurinmz@um.edu.my (N.W.M. Zulkii).
0360-5442/$ e see front matter 2013 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.energy.2013.01.038

friction is concerned. But the wear rate is higher than ordinary

lubricants, which may not be recommended as an engine oil in the
unmodied form. The major function of engine oil is to decrease the
frictional force, by forming a thin lm between the moving parts in
the engine such as piston and cylinder. Consequently, wear of the
moving parts is reduced and diminished the power loss. Besides,
engine oil also used to cool the engine by carrying away the heat,
inhibits corrosion, cleans and improves sealing. One of the most
important properties of engine oil is viscosity, which should be high
enough to maintain the lubricating lm thickness, and low enough
to make sure the oil can ow through all the engine parts. The TMP
(trimethylolpropane) ester is produced from a palm oil methyl ester
through transesterication. Transesterication eliminates the
hydrogen molecule on the beta carbon position of the palm oil
substrate, thus improving the oxidative and thermal stability of the
TMP ester; an important lubricity property in vegetable oils [11]. In
addition, TMP esters have good friction-reducing properties and
acceptable anti-wear properties [12]. However, in contrast, Waara
et al. [13] found that pure synthetic ester (TMP-Oleate and TMP-C8C10) in a sliding contact resulted in high wear rates and a lot of
abrasive marks on the surface. To understand the lubricity performance, the Stribeck diagram can be seen in Fig. 1. This diagram
shows the coefcient of friction in a rotating bearing, plotted

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N.W.M. Zulkii et al. / Energy 54 (2013) 167e173

Nomenclature
OL
TMP
POME
VI
COF
WSD
HFRR

ordinary lubricant
trimethylolpropane
palm oil methyl esters
viscosity index
coefcient of friction
wear scar diameter
high frequency reciprocating rig

against Stribeck variable (known as the dimensionless Sommereld

number). The Stribeck variable is shown in equation below.

Stribeck variable;

mN

; m viscosity;
P
N rotational speed; P unit load

Lubrication under low values of Stribeck region is known as

boundary lubrication. Low values of Stribeck variable correspond to
low viscosity, low speeds, and high loads. In this case, the surfaces
asperities are actually in contact to each other [14]. Therefore,
extreme pressure and anti wear additives played an important role
to form a boundary lubricating lm [14e16] to protect the surface.
In addition, surface characteristic also plays an important role
contacting two surfaces. There are many locations in the modern
diesel engine where boundary lubrication occurs such as in piston
rings at the top and bottom dead centers, and the fuel-injection
system. Lubricity is the uid property that characterizes friction
and wear phenomenon in boundary lubrication. The lubrication in
the large values of the Stribeck is called hydrodynamic region. Large
values of the Stribeck variable correspond to high viscosity uids,
high rotational speeds, and light loads. Under these conditions, an
oil lm supports the load/carry the load at low friction. In this
condition, uid properties are of greatest signicance for wear and
friction, and the surface characteristics such as surface asperities of
the bearing are not important since the surfaces are not in contact
[17,18]. In an engine, hydrodynamic lubrication occurs in journal
bearing, crankshaft bearing and when the piston rings are moving
[19,20]. It can be highlighted that frictional forces consume about
15e20% of fuel in an internal combustion engine. Only the
development of low coefcient of friction lubricant and surface
development is the solution to reduce this energy consumption.
Hence, in order to have a better understanding of reduction of
frictional forces through the tribological study, a new type of
lubricant substitute TMP is introduced. The effect of TMP ester on

Fig. 2. Synthesis of palm oil-based TMP ester.

different lubrication regime using four-ball machine and HFRR

(high frequency reciprocating machine) wear tests have been
investigated. The output of these experimental results would give
a correlation of actual frictional behavior in internal combustion
engine. The objectives of this study are to investigate the tribological properties under boundary and hydrodynamic lubrication
when added palm-oil based TMP ester in OL (ordinary lubricant).
2. Experimental method
2.1. Lubricant sample preparation
Palm oil-based TMP ester was synthesized by the transesterication of methyl esters as shown in Fig. 2 [21]. The preparation process of palm oil-based TMP ester is shown in Fig. 3. The
trimethylolpropane [2-ethyl-2-(hyhydroxymethyl)-1,3-propanediol] was chosen due to its lower melting point compared to other
polyols. A 200 g volume of palm oil methyl ester and a known
amount of TMP were placed into a 500 ml three-neck reactor and
constantly agitated by a magnetic stirrer. The weight of TMP was
determined based on the required molar ratio and the calculated
mean molecular weight of the POME (palm oil methyl esters). The
mixture was then heated to the reaction temperature in the presence of catalyst. A vacuum was gradually applied to the system until
the desired pressure was reached. This pressure was maintained
until completion of the reaction. The peaks appeared were identied and labeled based on the number of alkyl carbon groups that
attached to TMP backbone. The esters formed are identied by
making comparisons by standard or by using the standard of TG
(triglycerides), DG (diglycerides) and monogliceride (MG) [22].
Fatty acid composition is shown in Table 1.
Both palm oil-based TMP esters were blended with OL using
a stirrer at 110 rpm and heated to 100  C. Detail properties of OL are
shown in Table 2. The blended lubricants consisted of 5%, 10%, 15%,
20% and 100% palm oil TMP esters (volume basis) with OL. Compositions of the lubricant samples are shown in Table 3.

Palm Oil Methyl Ester

Trimethylolpropane

Heating and stirring of mixture Palm Oil

Methyl Ester and Trimethylolpropane

Alkaline catalyst was

added to mixture

A vaccum gradually
applied
Product purification: using vacuum
distillation

Purified palm oil-based TMP ester

Fig. 1. Stribeck curve diagram.

Fig. 3. Preparation of palm oil-based TMP ester.

N.W.M. Zulkii et al. / Energy 54 (2013) 167e173

Table 1
Fatty acid composition of palm oil-based TMP ester.

169

Table 3
Percentages of the palm oil-based TMP ester and OL in each sample.

Fatty acid composition

(%)

Sample

Palm oil-based TMP ester (%)

OL (%)

Monoester
Diester
Triester

5
5
90%

OL
TMP5
TMP10
TMP15
TMP20
TMP100

0
5
10
15
20
100

100
95
90
85
80
0

2.2. Lubricant properties test

Density: Density was measured using a DMA 35 portable density meter. The samples were tested at 15  C. Only 2 ml of each
sample was used per test.
Viscosity index (VI): The viscosity index (VI) was calculated
using ASTM D2270. This method uses the kinematic viscosities
at 40  C and 100  C to determine the VI. The experiments were
carried out using an ISL automatic Houillon viscometer.

2.3. Wear and friction test

2.3.1. Four-ball machine
The four-ball wear test is used to investigate the effect of Palm
oil-based TMP ester under wear preventive test (hydrodynamic
test). The four-ball wear tester is the predominant wear tester used
by the oil industry to study lubricant chemistry. The four-ball wear
tester consists of three balls held stationary in a ball pot plus
a fourth ball held in a rotating spindle as shown in Fig. 4. The balls
used in this study were steel balls, AISI 52-100, 12.7 mm in diameter, with 64e66 Rc hardness. These balls were thoroughly cleaned
with toluene before each experiment. The sample volume required
for each test was 10 ml. The test method used to investigate wear
preventive characteristic was ASTM D4172 [23]. The test conditions
were 40 kg load, operating temperature of 75 C  2  C, rotational
speed of 1200 rpm and operation time of 60 min. For the extreme
pressure test, ASTM 2783 [24] where the load is increased by 20 kg
for every 10 s until the ball is welded. The wear produced on the
three stationary balls is measured under a calibrated microscope
and reported as the WSD (wear scar diameter) or calculated
volume.
2.3.2. HFRR (High frequency reciprocating rig) conguration
The HFRR wear test was used to investigate the effect of Palm
oil-based TMP ester under uid lm lubrication as shown in Fig. 5.
The HFRR test (ASTM D6079) used in this study involves a weighted
cast iron pin cylinder (6 mm length) and a stationary cast iron plat
(15 mm  15 mm), which is completely submerged in a 10 ml of
sample. The ball and disk is tested at room temperature and
brought into contact with each other and the entire apparatus is
vibrated at 10 Hz for 60 min with the load 10 N. The sliding stroke is
maintained at 2 mm. Several blends of Palm oil-based TMP ester
including 1%, 3%, 5%, 7% and 10% are tested and analyzed. Each test
was carried out three times repeatedly to observe any errors need
to be analyzed.

3. Results and discussion

3.1. Physicochemical properties of palm oil-based TMP ester in OL
(ordinary lubricant)
The data were used to evaluate the differences between OL and
to serve as a basis for comparing the blended fuels with palm oilbased TMP esters. The percentage of palm oil-based TMP esters
and OL in each sample is shown in Table 2. All of the lubricant
properties are listed in Table 4.
The VI (viscosity index) of oil is a number that indicates the
effect of temperature changes on its viscosity. A low VI signies
a relatively large change in viscosity with changes in temperature.
In other words, the oil becomes extremely thin at high temperatures and extremely thick at low temperatures. A high VI signies
relatively little change in viscosity over a wide range of temperatures. The ideal oil for most purposes is one that maintains a constant viscosity throughout different temperature changes.
Considering automotive lubricants can easily show the importance
of the VI. The oil having a high VI resists excessive thickening when
the engine is cold and, consequently, promotes rapid starting and
prompt circulation. It also resists excessive thinning when the engines sliding components are hot and thus provides full lubrication
and prevents excessive oil consumption. The VI of oil is determined
based on known viscosities at any two temperatures (here 40  C
and 100  C). It can be seen from Table 3, TMP 1 has the highest
viscosity as 108.75 cSt.
The density of a lubricant uid can provide indications of its
composition and nature. The density of lubricants, mainly hydrocarbons, varies between 0.860 and 0.980 g m3. The densities of OL
and TMP100 were 0.850 and 0.9012, respectively.
3.2. Effect of palm oil-based TMP ester under wear preventive test
(hydrodynamic test)
The WSD results for the different percentages of palm oil-based
TMP ester in OL are shown in Fig. 6. The signicance improvement
in WSD was found for TMP3, which is 30% as compared to OL. This
can be explained that an increase in the number of ester groups
leads to greater binding of the molecules, which provide a greater

Table 2
Properties of ordinary lubricant.
Properties

Ordinary lubricant

Density at 15  C (g/cm3)
Pour point ( C)
Flash point ( C)
TBN (mg KOH/g)

0.867
36
228
8.6

Fig. 4. A schematic of the four-ball test machine.

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N.W.M. Zulkii et al. / Energy 54 (2013) 167e173

Fig. 5. The schematic diagram of HFRR wear test.

resistance to shear forces. However increasing TMP ester more than

3% does not show any improvement on WSD. This can be attributed
to the fact that, more than 3% of Palm oil-based TMP ester could not
form the stronger lubricant lm formation.
This nding is similar to the ndings reported by Yunus et al.
[25], who found the lower wear scar diameter using palm oil-based
TMP ester with compared to ordinary hydraulic uid (not the engine lubricant). In addition, Masjuki et al. [26] also found that palmbased lubricating oil had a better wear performance compared to
mineral oil. Fernandez et al. [27] reported that the addition of
a synthetic TMP ester to a low viscosity polyalphaolen acted as
a wear reducer. According to Havet et al. [28] the length of the fatty
acid chains tends to increase the adsorbed lm thickness, therefore
increasing the surface area protected.
The values of COF (coefcient of friction) for the various lubricant samples are shown in Fig. 6. It has similar trend like WSD. In
general it can be stated that the COF reduces with the addition of
Palm oil-based TMP ester except for TMP100. Based on the value of
COF and WSD it is found that TMP 3 has the best lubricity performance. At TMP 100, WSD is maximum of around 0.78 mm. Based on
Fig. 7, it can be seen that after the operation time of 20 min, the thin
lm layer has started breaking down. This is because of low viscosity in TMP 100, the lubricant lm formed is not able to support
the load throughout the operation time.
The micrographs of the area around the wear scar and the worn
surfaces of the ball specimens for the different percentages of the
Palm oil-based TMP esters are shown in Fig. 8. It can be seen that,
adhesive wear occurs. The load applied to the contacting asperities
that they deform and adhere to each other to form micro-joints.

The continuous rotation of the top ball causes the rupture of the
micro-joints and creates pits and grooves. Surface morphology
shows that adhesive is very minimal for OL as we can see there is
transferred material.
For lubricant added Palm oil-based TMP ester, the appearance of
the worn surfaces seems to present corrosive product of black color
at higher temperature. The higher percentage of palm oil-based
TMP esters added, the black color is darker. This may be
explained from the fact that at higher temperature, lubricant can be
oxidized and thereby produces different types of corrosive acids
that enhance corrosive wear [29,30]. In addition, it is found that this
boundary lubricating lms acts as a sacricial layer. The reaction
products of tribochemistry provide a layer, so instead of the surface
being worn, this layer is removed [31]. It can be seen that, from
Fig. 8(TMP 10), the black color areas have a severe wear compared
to non-black area. Further it can be explained that the existence of
oxygen might accelerate the generation of inorganic oxides like
Fe3O4, Fe2O3, which plays an important role in the formation of
lubrication lm on the rubbing surface [32]. For TMP 100, it seems
like the uid lm of lubricant is completely breakdown. The direct
interaction between two solids that remove material from, while at
the same time producing polished surface on [33]. Based from
Fig. 8(TMP100), material removal in this case occurs as the very
small slabs of surface steel ball being lifted out the surface, probably

Table 4
Properties of the different percentages of the palm oil-based TMP ester in OL.
Sample

Properties
Viscosity


40 C (cSt)
OL
TMP 1
TMP 3
TMP 5
TMP 7
TMP 10
TMP100

101.86
108.75
107.21
101.42
102.15
97.637
40.03









1.53
1.22
1.41
1.30
1.17
1.21
1.32

VI

Density (g/cm3)

146
145
148
153
150
153
221

0.8549
0.8553
0.8558
0.8562
0.8568
0.8583
0.9012

100 C (cSt)
14.46
15.08
15.11
14.89
14.78
14.43
9.15









0.35
0.28
0.21
0.15
0.10
0.11
0.11









0.0174
0.0168
0.0176
0.0191
0.0176
0.0165
0.0171

Fig. 6. Wear scar diameters (WSD) and coefcient of friction (COF) for different percentages of the palm oil-based TMP esters in OL. Maximum error WSD; 0.05 mm,
maximum error COF: 0.005.

N.W.M. Zulkii et al. / Energy 54 (2013) 167e173

171

Fig. 7. Relationship between friction torque and times for different percentages of the
palm oil-based TMP esters in OL. Maximum error of friction torque: 0.01 Nm.

by some form of delamination. The polished wear mechanism occurs here as a result of severe abrasive wear. It can be seen also from
Fig. 8 (TMP100) that, the light reected from real surfaces.
This phenomenon was conrmed with the results of surface
roughness measurement, as shown in Fig. 9. The surface roughness
test was conducted in order to understand the wear scar texture on
the bottom three balls. A stylus prolometry test was performed to
evaluate the surface texture of the worn halo on the rotating ball
and the wear scars on the stationary balls. The prolometry trace
was fed into a microprocessor and the resulting signal was displayed on a chart recorder providing surface roughness graphs. The
prolometer traces were taken perpendicular to the direction of
sliding. Sample TMP 7 showed a comparatively smooth wear pattern compared to the other samples. No signicant difference is
observed among the tested lubricant samples except TMP 100,
which shows the maximum surface roughness of 0.07.
3.3. EP (Extreme pressure) characterization
Under extreme pressure, the wear rate from the rubbing surface
can be minimized by reducing the bearing stress or enhancing the
strength. At extreme pressure the ash temperature is elevated and
the extreme pressure additives decompose to form a chemical reaction lm which tends to increase the bearing area and consequently reduce the contact pressure. The performances of the EP
additives are dependent on three factors, which are: strength of the
tribo-lm, reaction rate between the additives and the rubbing
surface, and nally the compatibility between the base oil and the
additives [34]. To evaluate the friction and wear characteristics of
different biolubricants the extreme pressure characteristics were
investigated for a load range of 20 kg up until the balls specimens
weld with each other, which is dened as the FSL (nal seizure
load). The rotational speed applied was 1200 rpm, the temperature
was 27  7  C and an operation period of 10 s was employed for
each sample.
Fig. 10 shows the variation in the coefcient of friction under
different loads for different TMP ester added lubricant. The magnitude of the coefcient of friction indicates that the lubrication
regime occurring in the rubbing zone were both elasto hydrodynamic and boundary lubrications. Most of the TMP ester presented
a lower coefcient of friction (COF) compared to the OL. It seems
quite clear that the COF for TMP 1, TMP 3, TMP 5 and TMP 7 were
lower as compared to petroleum-based ordinary lubricant while
TMP 10 and TMP 100 showed the higher COF throughout the load
range. The OL, TMP 1 and TMP 3 were found to be more stable in
terms of a FSL (nal seizure load) which is dened as the load at
which lubricants lm totally break down and testing ball materials
become welded. It can also be noted that TMP 1 imparted lowest

Fig. 8. SEM micrograph from the stationary ball of different percentages of the palm
oil-based TMP ester in OL.

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N.W.M. Zulkii et al. / Energy 54 (2013) 167e173

Fig. 9. Surface roughness for the different lubricating oil samples. Error 0.01 mm.

COF upto initial seizure load (ISL) of the load at which a considerable amount of wear is occurred however, after FSL the lowest
COF was found to be using TMP 3. The results of Fig. 10 imply that
the TMP 1 and TMP 3 have the greatest ability to retain its properties upto the load of 220 kg without the lubricating lm breaking
down. This can be attributed to the fact that at higher loads the
lubricating lm thickness becomes thinner than some of the asperities present in the boundary lubrication regime. However,
these asperities are covered by the long chain fatty acid and the
esters of the biolubricants, which are known as surface active
materials. TMP 1 and TMP 3 showed the best performance in terms
of reducing the COF, which can be interpreted as the fatty acid
present in the TMP esters acting as an active surface material which
is adequate for these two lubricants, and above that the fatty acid
does not take part because the rubbing contact surface is fully
covered by the them. Another important fact is that above 3%
addition the TMP adversely affects the quality of the lubricant.
3.4. Effect of palm oil-based TMP ester under uid lm lubrication
According to results presented in Fig. 11, TMP 7 has showed the
lowest friction torque around 0.02 Nm. The OL shows the highest
friction torque because the viscosity is too high and created a thick
lm, which will cause more friction. Addition of Palm oil-based
TMP ester in the OL reduced the viscosity of the lubricant, hence
provides a better thin lm at the surface and thus reduced the
friction. Based on the experimental results, it can be stated that, the
addition of Palm oil-based TMP ester in the base lubricant leads to

Fig. 11. Relationship of friction with time under hydrodynamic lubrication.

Error 0.005 Nm (Reciprocating test).

improve the frictional torque characteristics of the lubricants. In

contrast with boundary lubrication, at low load, TMP 100 still can
maintain the lm lubrication. The weight loss of the cast iron at
plate is very small. It can be assumed almost no wear occur in this
regime lubrication.
4. Conclusion
The experimental results show that Palm oil-based TMP ester
based lubricant improves the wear preventive lubrication properties in terms of COF and WSD. The TMP 3 shows the lowest WSD
and COF with compared to others lubricants analyzed in this study.
In addition, under extreme pressure condition maximum load
bearing capacity of 220 kg was found to be using TMP 3 by retaining
its quality without breakdown. Under the uid lm lubrication
using reciprocating test the TMP 7 shows the best lubricity property
with the lowest friction torque. In order to utilize Palm oil-based
TMP ester as an engine oil, many other properties including oxidative, thermal and hydrolytic stabilities need to be examined.
Palm oil-based TMP ester is environmentally desired to mineral oilbased lubricants, research to investigate the properties of palm oilbased TMP ester to make it technologically competitive as automobile lubricant, and should be encouraged.
Acknowledgments
The authors would like to thank the University of Malaya, which
made this study possible through the research grant FRGS FP020/
2011A, PV070/2011B and high impact research grant no UM.C/HIR/
MOHE/ENG/07.
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Fig. 10. Variation in coefcient of friction at different load under extreme pressure
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