Energy Education Science and Technology Part A: Energy Science and Research

2012 Volume (issues) 30(1): 123-136

Tribological characteristics
of amine phosphate and
octylated/butylated diphenylamine
additives infused bio-lubricant
M. A. Kalam, H. H. Masjuki, M. Shahabuddin*, M. Mofijur
University of Malaya, Department of Mechanical Engineering, 50603 Kuala Lumpur, Malaysia

Received: 27 August 2011; accepted: 31 October 2011

Abstract

This paper presents the experimental results of normal lubricant, additives added lubricants and waste
vegetable oil (WVO) contaminated bio-lubricants to evaluate the tribological properties such that friction
and wear characteristics. The test was conducted using a four-ball tribotester with standard test method IP-
239. The balls used in four-ball tribotester were based on carbon-chromium steel ball bearings. To
evaluate friction and wear characteristics, coefficient of friction (μ), wear scar diameter (WSD), flash
temperature parameter (FTP), viscosity index (VI) and total acid number (TAN) were investigated. Each
test was conducted for five different loads from 50 kg to 90 kg at an interval of 10 kg. The lubricant was
contaminated with WVO from 1% to 5%. The normal lubricant (as sample A) was used for comparison
purposes. The test results showed that WVO contaminated lubricants with suitable anti-wear additive
(amine phosphate) can reduce friction and wear coefficient substantially. The objective of this
investigation is to develop a new lubricant based on waste palm oil (such as WVO).

Keywords: Waste vegetable oil (WVO); wear scar diameter (WSD); Four-ball tribotester
©Sila Science. All Rights Reserved.

1. Introduction

Lubricant, fuel and engine materials are closely related to each other. The conventional
mineral oil based lubricant was developed based on fossil fuel (such as gasoline and diesel fuels)

___________
*
Corresponding author: Tel: +601-6241-8438; fax: +603-7967.5317.
E-mail address: shahabuddin.suzan@yahoo.com (M. Shahabuddin).
124 M. Shahabuddin / EEST Part A: Energy Science and Research 30 (2012) 123-136

which is not suitable for biodiesel fueled engine as it degrades lube oil quality and increases the
wear rate of the engine components [1]. Vegetable oils have numerous advantages over mineral
lubricant which are renewability, environmental friendly, less toxicity, more biodegradability and
higher stearic acid [2-5]. Therefore, vegetable oil has the potential to substitute petroleum based
lubricating oil as well as the interest in the use of animal fats and vegetable oils derived lubricant
is increasing precipitously [6-8]. In addition, the rapid depletion of the crude oil and higher price
has drawn the attention to use bio-lubricants instead of petroleum based lubricant. Most of the
biodiesel contain large proportion of unsaturated free fatty acid which is defined as the ratio and
position of carbon-carbon double bond, one two and three double bonds of carbon chain is named
as anoleic, linoleic, and linolenic fatty acid components respectively [9]. Both boundary and
hydrodynamic lubrication can be obtained from the bio lubricant due to its long chain free catty
acid and polar groups of the natural plant oil [10, 11]. Since bio lubricant possess double bonded
unsaturated fatty acid thus it exhibit poor oxidation stability, poor cold flow properties, poor
corrosion characteristics and other tribochemical degradations [12-20]. To improve these
limitations, several investigations have been undertaken and will continue in future [21-23]. The
lubricating oil undergoes various unfavorable conditions such as extreme pressure, temperature,
share stress etc. During several tribochemical processes, lubricating oils should have adequate
ability to maintain its properties. The Triacylglycerol molecules of the bio lubricant having polar
end formed a mono or multi molecular layer [24, 25]. Study result shown that storing the
vegetable oil at -100Cundergoes cloudiness, poor flow and solidification [26]. The properties of
the vegetable oil do not with stand at a storage temperature over 80°C also. However, the use of
appropriate antioxidant as an additive can be played a significant role to resist the degradation of
the lube oil quality [27]. Even, it is also investigated that vegetable oil without additives
performed better, as compared to mineral oil in terms of friction and wear [28, 29], scuffing load
capacity [30], which are also good agreement with other authors [31-33].They stated that
vegetable oil showed lower coefficient of friction, resistance to pitting wear, equivalent scuffing
load capacity, though poor oxidation and thermal stabilities are the limitations. Independent
approaches are taken by the several researchers to improve the oxidation and thermal stabilities
of vegetable oil [34, 15, 35]. However, for improving the overall properties of the vegetable oil,
more generalized approaches are needed [36]. Lubricating oil quality is degraded especially in
the piston-cylinder friction zone due to mixing fuel with lubricant. Hsu et al. [37] stated that
hydrodynamic effect of the lubricating oil does not affect surface wear significantly while, the
interaction between the contact surfaces and between the contact surfaces and the lubricating oil
with or without additive influences the tribological properties. Different feedstock is used, to
formulate the vegetable oil in the different part of the world. In Europe mostly rape seed oil is
used as the source of lubricating oil which showed excellent tribological properties and
compatibility with the equipment seal and the elastomers as well as environment adaptability
[27]. Whereas, in Malaysia mostly palm oil is used as the source of bio lubricant and
investigations are still in progress on other sources including infusing additives with the bio
lubricants. In this investigation, waste palm oil (as WVO) contaminated lubricant has been
developed as a biodegradable lubricant to be used for biodiesel fuelled engines. Based on four
ball tribo-testing results, WVO contaminated lubricant with the presence of suitable anti-wear
additive shows promising result as compared to conventional lubricant. This is mainly due to
better thermal and oxidative properties of WVO consisting of long chain saturated fatty acids
that leads to inferior
 M. Shahabuddin / EEST Part A: Energy Science and Research 30 (2012) 123-136 125
cold flow behavior [38]. The results of this study have presented an indication for the formulation
of a new lubricant.
2. Experimental details
2. 1. Equipment
Four-ball tribotester machine was used with standard test method of IP-239. This machine is
simple to use for testing friction and wear of lubricating oils. Three balls are located in a (Fig.1)
cup below a fourth ball which is connected to a rotating shaft via a chuck. Different loads are
applied to the balls by weights on load lever. The frictional torque exerted on the three lower
balls can be measured by a calibrated arm, which is connected to the spring of a friction
recording device. The extension of the spring in resisting the frictional torque is transmitted
through a link mechanism, to a pen which records its travel on a drum at 1 revolution in 60-75s.

Fig. 1. Schematic diagram of the four-ball tribo-tester.

2. 2. Ball materials
The tested ball‟s material was carbon-chromium steel (SKF), 12.7 mm in diameter with a
surface roughness of 0.1μm C.L.A. The chemical composition of ball material was scanned by
Energy Dispersion X-Ray Spectrometer (EDS) as shown in Table 1. Before starting a test, all the
balls were cleaned using spirit alcohol and dried with dry air. Before starting a test, the four-ball
tribotester machine was operated without any load for a period of 15 min, all the approximate
parts of the machine were clean by solvent, dry with a clean soft lint-free cloth or clean dry air.

Table 1. Chemical composition (wt. %) of carbon-chromium steel ball material

Element C Si P S Cr Mn Fe Ni Total
wt. % 10.2 0.45 0.12 0.07 1.46 0.42 87.21 0.06 100

2. 3. Lubricant samples

Three samples were explicitly prepared such as (1) Sample A-normal lubricant as SAE40 grade.
It can stated that sample A is the reference lubricant, (2) Sample B- consists of sample A
126 M. Shahabuddin / EEST Part A: Energy Science and Research 30 (2012) 123-136

with 0.5% Amine phosphate additive, and (3) Sample C- consists of sample A with 0.5%
Octylated/butylated diphenylamine additive. It can be stated that sample B and sample C are
prepared with two different types of anti-wear additives. The sample B and sample C can be
referred to as base lubricants with respect to contaminated lubricant by WVO. The sample B and
sample C were contaminated with WVO from 1% to 5%. Details of lubricant compositions can
be seen in Table 2. Details properties of anti-wear additives can be seen in Table 3.

Table 2. Lubricant sample compositions

Samples Lubricant compositions
A Normal lubricant as SAE 40 grade
B Sample A with 0.5% Amine phosphate additive
Sample A with 0.5% Octylated/butylated diphenylamine additive plus 1% to 5% waste palm oil
C
with base lubricant
D Sample B with 1% to 5% waste palm oil with base lubricant
E Sample C with 1% to 5% waste palm oil with base lubricant

Table 3. Properties of anti-wear additives

Octylated/butylated
Chemical description Amine phosphate
diphenylamine
Treat level/range (%) 0.1 – 1.0 0.3 – 1.0
Viscosity at 40°C 220 (mm2/s) 280 (mm2/s)
Melting point <10°C <10°C
Density at 20°C (g/m3) 0.92 0.98
Phosphorus (%) 4.8 -
Nitrogen (%) 2.7 4.5
Flash point (°C) 135 185
Solubility limits at 5°C (wt. %)
 Mineral oil 3 5
 Ester >5 5
 water <0.01 <0.01

2. 4. Test procedure

At the beginning of the experiment, lubricant sample is placed on the erected plate where
three balls are held position into a cup (at the end of the motor spindle) with the clamping ring
and assembly secured by tightening the locknut. The fourth ball is then fitted on the upper balls
chuck. Mounting disks are placed between the thrust bearing and the cup. The desired loads are
then placed on the load lever to be tested at. The conducted test method is standard IP-239.

2. 5. Friction evaluation

The coefficient of friction is calculated by multiplication of the mean friction torque and
spring constant [39].The friction torque on the lower balls may be expressed thus;

  3W  r T 6
T    (1)
6 3W  r
 M. Shahabuddin / EEST Part A: Energy Science and Research 30 (2012) 123-136 127

where, μ : coefficient of friction

T : frictional torque in kg/mm
W : applied load in kg
r : distance from the center of the contact surfaces on the lower balls to the axis of
rotation, which is 3.67mm.

2. 6. Wear test

The test run was carried out at loads (50, 60, 70, 80 and 90 in kg) and at 1500 rev min-1 with
test duration of 60 minutes. The wear scar diameter (WSD) was measured and analyzed by
“ducom software” with installed image acquisition system.

2.7. Flash temperature parameter

A single number is used to express the critical flash temperature above which a lubricant will
fail under given conditions. For conditions existing in the four-ball test, the following formula is
used [40].

W
FTP  1.4
(2)
d
where, W: load in kg
d: mean wear scar diameter in mm.

2. 8. Kinematics viscosity analysis

The ISL Automatic HOUILLON Viscometer is used to measure the viscosity of the
lubricating oil using ASTM Method D-455 with two controlled bath temperatures such as 40°C
and 100°C. Before measuring the viscosity of the lube oil, the viscometer tubes are calibrated by
standard sample lube oil. The lube oil is warmed to the desired temperature and allowed to flow
through the calibrated region to be measured. The lube oil‟s viscosity (in cSt) is the flow time (in
second) multiplied by the apparatus constant.

3. Results and discussion

All the samples preparation and test are conducted at Engine Tribology Laboratory,
Department of Mechanical Engineering, and University of Malaya. All the test results can be
discussed as follow:

3.1. Coefficient of friction (COF) analysis

Under high sliding contact and load, the polar functional group of the triacylglycerol molecule
undergoes a physical as well as chemical interaction with the metallic surface [41]. The
coefficient of friction of the bio-lubricant is largely depends on the mixing ratios of the vegetable
128 M. Shahabuddin / EEST Part A: Energy Science and Research 30 (2012) 123-136

oil and the mineral oil [36]. As the consequence of unsaturated free fatty acid and the palmitic
acid the corrosive wear of the palm based vegetable oil results the higher friction co efficient
friction (μ) as compared to mineral oil [42]. The coefficient of friction versus applied loads on
four-ball testing is shown in Fig. 2. The sample A is the reference lubricant as SAE40 grade. The
sample B and sample C are the anti-wear additive added lubricants with sample A. Fig. 2 shows
how the different types of anti-wear additives affect on coefficient of friction. It is found that
sample C increases COF from 0.8 to 0.24 for increasing loads from 50 kg to 90 kg. However, the
sample B shows lower COF than reference lubricant as lubricant A. It is clearly evident that the
additive (0.5% Octylated/butylated diphenylamine based additive) in sample C has an adverse
effect on COF with reference lubricant A. The lowest COF was found from sample B followed
by sample A and sample C. The sample B consists of 0.5% Amine phosphate additive with
sample A. Hence, Amine phosphate additive is effective in reducing friction and enabled to keep
consistency throughout the load range.

Fig. 2. Coefficient of friction (μ) vs. loads for sample A, B and C (Table 2).

Fig. 3. Coefficient of friction (μ) vs. percentage (%) of palm oil in samples D & E (Table 2) at
constant 70 kg.

Fig. 3 shows comparison of coefficient of friction (μ) for sample A, D and E at 70 kg applied
load. The medium load as 70 kg was chosen for comparison purposes. It can be stated that
samples D and E are palm oil contaminated lubricant which are obtained from base lubricants B
 M. Shahabuddin / EEST Part A: Energy Science and Research 30 (2012) 123-136 129

and C respectively (Table 2). In addition, sample A is always a reference lubricant as neither anti-
wear additive nor palm oil have been added in it. The sample E which consists of
octylated/butylated diphenylamine as anti-wear agent and palm oil shows adverse result. The
friction coefficient for Sample E is found within 0.14 to 0.15 and sample A and D are found
within 0.04 to 0.06 only. This indicates that, octylated/butylated diphenylamine is not a suitable
anti-wear additive to reduce friction. Although its detailed chemical structure is unknown,
changes in its physical properties such as viscosity can be observed [43]. Furthermore, the best
performance is obtained when percentage combination of WVO is at maximum 4% of palm oil.
However, above 4% of palm oil mixture drops friction coefficient. As the consequence of
unsaturated free acid and the palmitic acid thus corrosive wear of the palm oil based vegetable oil
result the higher friction co efficient friction (μ) as compared to mineral oil based bio lubricant.
3. 2. Wear scar diameter (WSD) analysis
Fig. 4 shows WSD for samples A, B and C and Fig. 5 showsWSD for samples A, D and E.
Referring to Fig.4, it is found that sample C produces higher level WSD followed by sample A
and sample B. Sample B shows the best performance (a reduction of 20% of WSD as compared
to sample A) which means that amine phosphate is effective in palm oil contaminated lubricant.
It can be explained that the friction and wear resistance mechanism of anti-wear additive in palm
oil contaminated lubricant causes from complex chemical transformation on the metal surface.
The amine phosphate has the general structure represented (below) by: R = mostly aliphatic
groups (2-ethylhexyl, hexyl and n-octyl); amines have tert-alkyl group with 10-24 carbon atoms
[43].

Fig. 4. Wear scar diameter (WSD) vs. loads for sample A, B and C (Table 2).

Fig.5. Wear scar diameter WSD) vs. percentage (%) of palm oil in samples D & E (Table 2).
130 M. Shahabuddin / EEST Part A: Energy Science and Research 30 (2012) 123-136

Fig. 5 shows that sample D reduces WSD with maximum 4% palm oil contaminated lubricant
with amine phosphate additive. However above 4% palm oil contaminated lubricant, the film
thickness might be broken due to increasing palm oil percentage. The presence of up to 4% of
palm oil makes the sample D more effective than other combination (as sample E). The
breakdown of WVO (waste palm oil) molecule during tribo-chemical process results in the
formation of fatty acids which can react with the phosphorus containing group from amine
phosphate. These fatty phosphates function as effective friction modifiers and anti-wear agent in
the presence of WVO. The long hydrocarbon chain of the fatty acid provide an excellent
molecular barrier while the polar group coordinate with iron to form a protective film on the
metal surface. Sample C shows the WSD between 0.70 -0.80 mm up to 4% palm oil combination
which is 50% higher than sample B. This can be caused by the high friction in contact surfaces
by using a composition containing octylated/butylated diphenylamine additive as anti-wear agent.
It can be realized that the octylated/butylated diphenylamine additive works as anti-oxidant rather
than anti-wear agent while added with palm oil contaminated lubricant. This additive and the
waste palm oil neutralize each other at high temperature that causes adverse effect on the metal
surface. Hence, surface wear increases. A similar phenomenon was also found by Maleque et al.
[44] and Adhvaryu et al [36].

3. 3. Flash temperature parameter analysis

The maximum flash temperature parameter (FTP) can be defined as a number used to express
critical temperature above which a lubricant film thickness will be breakdown under given
conditions. The value of FTP has been calculated using equation 2. From the equation it can be
seen that FTP value depends on applied load and WSD. According to Fig. 6 and Fig. 7, it can be
said that amine phosphate based lubricants such as sample B (Fig.6) and sample D (Fig.7) show
higher level of FTP number which means greater lubricant stability. Meanwhile, samples C and E
show lower FTP value that indicate breakdown of lubricant film thickness, hence WSD increases.
However, above 4% palm oil contaminated lubricant, the FTP value drops as shown in Fig.7.

at constant 70 kg load

Fig. 6. Flash temperature parameter (FTP) vs. loads for sample A, B and C (Table 2).

3. 4. Total acid number (TAN) analysis

Usually the TAN values of the vegetable oil are in the range of 0.18-0.37 mg KOH/g and in
M. Shahabuddin / EEST Part A: Energy Science and Research 30 (2012) 123-136 131

Fig. 7. Flash temperature parameter (FTP) vs. percentage (%) of palm oil in samples D & E
(Table 2) at constant 70 kg load.

the absence of additives this range is increased to 2.0-3.0 mgKOH/g after 28 days [17]. The TAN
test results are shown in Fig. 8 and Fig. 9. According to Fig.8, the lowest TAN value is found
from sample B (1.60 mgKOH/g) followed by sample A (1.70 mgKOH/g) and sample C (2.30
mgKOH/g). It can be found that sample E produces higher level of TAN followed by sample D
and sample A. It is evident that the octylated/butylated diphenylamine additive is not suitable in
both the normal lubricant (sample A) and WVO (waste palm oil) contaminated lubricant (sample
E). This is mainly due to the chemical properties of octylated/butylated diphenylamine additive
that does not suit with sample A and sample E. Whereas, the amine phosphate anti-wear additive
shows higher TAN value (Fig. 9) as compared to normal lubricant (sample A) when the
percentage of WVO is increased. This is mainly due to the high fatty acid in WVO. However, the
TAN value may also increase due to effect of oxygen in WVO, and at higher temperature, the
fatty acid molecules or other organic acids can be decomposed during operation.

Fig. 8. Total acid number (TAN) vs. loads for sample A, B and C (Table 2).

3. 5. Viscosity index (VI) analysis

Viscosity is the property used for identification of individual grades of lube oil and for
monitoring the changes occurring in the lube oil while in service. Higher viscosity indicates that
132 M. Shahabuddin / EEST Part A: Energy Science and Research 30 (2012) 123-136

Fig. 9. Total acid number (TAN) vs. percentage (%) of palm oil in samples D & E (Table 2) at
constant 70 kg load.

the lubricant is being deteriorated by either oxidation or contamination, while a decrease usually
indicates dilution by lower viscosity oil or by fuel [44-47]. One of the main drawbacks of
vegetable based bio lubricants is its limited range of available viscosities [29]. Fig. 10 and Fig. 11
show viscosity at 40oC and Fig. 12 and Fig. 13 show viscosity at 100 oC. According to Fig. 10 to
Fig. 13, it can be seen that amine phosphate increases viscosity (as sample B in Fig.10 and Fig.
12). However, the same additive such as amine phosphate decreases viscosity with palm oil
(Fig.11 and Fig13) as compared to original sample A, but this change is usually within the useful
range in the both the temperature ranges such as at 40oC and 100oC.

Fig. 10. Viscosity (at 40oC) vs. loads for sample A, B and C (Table 2)

Fig.11. Viscosity (at 40oC) vs. percentage (%) of palm oil in samples D & E (Table 2) at constant
70 kg load.
 M. Shahabuddin / EEST Part A: Energy Science and Research 30 (2012) 123-136 133

Fig. 12. Viscosity (at 100oC) vs. loads for sample A, B and C (Table 2).

Fig. 13. Viscosity (at 100oC) vs. percentage (%) of palm oil in samples D & E (Table 2) at
constant 70 kg load.

Sample D shows viscosity decrease from 120 cSt to 100 cSt as WVO increased from 1% to
5%, indicating suitability for machinery operations. Normally at 40oC, the lower limit of engine
oil should be 80 cSt and below this value indicates that the oil has decreased its quality. The
applicable range of engine oil/lubricating oil at 40oC and 100oC are „80 cSt to 150 cSt‟ and „12
cSt to 20 cSt‟ respectively. However, the sample C and sample E show higher decreasing trend as
compared to sample B and sample D. Hence, the sample C and E will increase components wear
through degrading oil quality.

4. Conclusions

The following conclusions may be drawn from present study:

1. Amine phosphate as an anti-wear additive shows better result with normal lubricant (SAE
grade 40), whereby it reduces coefficient of friction (COF), WSD and TAN value while,
increases FTP, and viscosity as compared to octylated/butylated diphenylamine additive.
2. Combination of amine phosphate, normal lubricant and palm oil (up to 4%) show better
results such as reduces coefficient of friction (COF), WSD and TAN value while, increases FTP,
and viscosity as compared to octylated/butylated diphenylamine additive as like as the sample
made with the combination of amine phosphate and normal lubricant only.
134 M. Shahabuddin / EEST Part A: Energy Science and Research 30 (2012) 123-136

Hence, it can be stated that waste palm oil can be used as lubricant substitute (maximum 4%)
with normal lubricant and amine phosphate additive. However, Palm oil based lubricant still
shows higher TAN value, which will be further investigated [48].

Acknowledgment

The authors would like to acknowledge the Department of Mechanical Engineering,

University of Malaya, and Ministry of Higher Education (MOHE) of Malaysia for HIR grant
(Grant No. UM.C/HIR/MOHE/ENG/07) which made this study possible.

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