Fuel 84 (2005) 1601–1606

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Study on the lubrication properties of biodiesel as fuel lubricity enhancers

Jianbo Hu*, Zexue Du, Changxiu Li, Enze Min
Research Institute of Petroleum Processing, SINOPEC, Beijing 100083, People’s Republic of China.
Received 7 September 2004; received in revised form 5 November 2004; accepted 10 February 2005
Available online 17 March 2005

Abstract

Unrefined biodiesels containing small quantities of monoglycerides, diglycerides, and triglycerides, and refined biodiesels not containing
these glycerides were added to diesel fuel and the resulting lubricity was measured using the High Frequency Reciprocating Rig (HFRR)
method. The unrefined biodiesels showed higher lubricity properties than refined biodiesels. The chemical factors influencing the lubricity
properties of biodiesels were investigated. Methyl esters and monoglycerides are the main compositions that determine the lubricity of
biodiesels that meet international standards. Free fatty acids and diglycerides can also affect the lubricity of biodiesel, but not so much as
monoglycerides. Triglycerides almost have no effects on the lubricity of biodiesel.
q 2005 Elsevier Ltd. All rights reserved.

Keywords: Biodiesel; Lubricity; Vegetable oil; HFRR; Fatty acid methyl esters

1. Introduction fuel additive. They found that the type of alcohol

Biodiesel, which is defined as the monoalkyl esters,
mainly methyl esters (FAME), of long-chain fatty acids
derived from renewable biological sources, such as
vegetable oils or animal fats, is considered as a possible
substitute or extender of conventional diesel fuel. Because
of its good lubrication properties, biodiesel is also used
as an additive to improve the lubricity of petroleum fuels
[1,2]. Much research has been done to evaluate the impact
of biodiesels prepared from different vegetable oils such
as rapeseed oil, canola oil, soy oil, sunflower oil, etc. and
different alcohols such as methyl, ethyl, propyl and butyl
alcohols, on the lubricity of low-sulfur diesel [3–10]. Jon
H. Van Gerpen et al. [3] tested and compared the lubricity
properties of soybean oil and biodiesel derived from it
when used as lubricity additives. The results showed that
biodiesel appeared to be slightly more effective than
soybean oil for equal treatment rates. D.C. Drown et al.
[4] determined the effects of type of alcohol (methanol
and ethanol) and fatty acid profile of vegetable oil on the
lubricity properties of biodiesels when used as jet turbine
* Corresponding author. Tel.: C86 106 232 7551 ext8153.
E-mail address: hujb@ripp-sinopec.com (J.B. Hu).
0016-2361/$ - see front matter q 2005 Elsevier Ltd. All rights reserved.
doi:10.1016/j.fuel.2005.02.009
influenced the lubrication properties of biodiesel, but
fatty acid profile did not. A.K. Dalai et al. [5] used
‘Munson ROCLE’ bench test developed at the University
of Saskatchewan to evaluate the lubricity of biodiesels
derived from different vegetable oils. They also used
methyl, ethyl, butyl and 2-propyl alcohols to make
biodiesels and tested their lubricating properties in a
base diesel. Statistical analyses indicated strong effects of
fatty acid compositions and alcohols on the lubricity of
biodiesels [6]. The results of Dr Drown and Dr Dalai are
not completely in accordance with each other. More
recently, Daniel P. Geller and John W. Goodrum studied
the effects of specific fatty acid methyl esters on diesel
fuel lubricity [10]. They found that the individual fatty
acid esters did not have as dramatic an effect on lubricity
as did methyl esters derived from vegetable oils composed
of a mixture of several fatty acids.
In the literatures referred above, there implies a
hypothesis that the monoalkyl esters are the only main
composition that influences the lubricating properties of
biodiesel, so the effects of type of alcohol and fatty acid
profile of the vegetable oil on the lubricity properties of
biodiesel can be compared. However, biodiesel is not 100
percent monoalkyl esters, because it also contains small
quantities of monoglycerides (MG), diglycerides (DG),
triglycerides (TG) and free fatty acids (FFA), etc. These
compounds may also influence the lubricating properties of
1602 J.B. Hu et al. / Fuel 84 (2005) 1601–1606

biodiesel, but no research has been done on them by this Finally, part of the unrefined biodiesel was refined by
time. distillation at reduced pressure (less than 5000 Pa) and high
In this research, a series of fatty acid methyl esters (i.e. temperature (higher than 250 8C) until about 80% distillate
biodiesel) were synthesized from methanol and four by volume of the biodiesel was obtained.
different vegetable oils, and then refined by distillation at
reduced pressure and high temperature to obtain relatively 2.3. Analytical methods
pure methyl esters. The lubrication properties of unrefined
and refined biodiesels were evaluated and compared by The composition of biodiesel was analyzed by gas
adding the biodiesels to a base diesel and measuring the chromatography (GC) in HP6890 employing a 5 m!
High Frequency Reciprocating Rig wear area diameter 0.53 mm, 0.15 mm film thickness Ultra-ALLOY capillary
(WSD). The effects of MG, DG, TG and FFA on the column (Frontier Laboratories Ltd.). Data collection and
lubricity properties of biodiesel were also examined. analysis was performed with Hewlett–Packard Chemstation
software. N-pentadecane (NC15) was used as an internal
standard. A stock solution of acetone with a known amount
2. Materials and methods of N-pentadecane was prepared a priori and used for
analysis. Samples were prepared for analysis by adding
2.1. Materials approximately 0.1 g oil phase to 2 g acetone. The mixture
was put into GC auto sampler vials. One microliter of the
The vegetable oils, including sunflower oil, corn oil, sample was injected into the column. The oven temperature
canola oil, and soybean oil were food-grade. 1-monoolein program consisted of: start at 50 8C, ramp at 8 8C/min to
(O99%), 1,3-diolein (approx. 99%) and triolein (O99%) 380 8C. Methyl ester of oleic acid, 1-monoolein, 1,3-diolein
were supplied by Fluka and Sigma. Methanol, potassium and triolein were used as standard samples to determine the
hydroxide and oleic acid are of analytical grade. Base diesel retention times of FAME, MG, DG and TG. The fatty acid
was from Refinery, Beijing Yanshan Petrochemical Co., profile was determined by using an HP5890 with a FID and
Ltd., SINOPEC. The properties of base diesel are shown in a 30 m!0.25 mm!0.20 mm PEG capillary column. Acid
Table 1. value was measured according to GB/T 264 [14]. Lubricity
testing was done according to the HFRR method [15] with
2.2. Transesterification addition of biodiesel at 2.0% by weight of base diesel. The
HFRR operating conditions used are as follows: fluid
The biodiesel was made by a transesterification reaction volume (mL), 2G0.2; applied load (g), 200G1; speed (Hz),
carried out at 60 8C and atmospheric pressure for 2 hours. 50G1; duration (min), 75G0.1; fluid temperature (8C),
Potassium hydroxide was used as a catalyst at a concen- 60G2; stroke (mm), 1.0G0.02; batch surface area (mm2),
tration of 1% by weight of vegetable oil. 100% excess 600G100; repeatability (mm), 63; the relative humidity was
methanol (6 mol) was used to obtain high conversion of oil kept between 40 and 60%, while the ambient temperature
into esters. The crude ester was separated and washed with was between 24 and 26 8C. The wear scars quoted are
distilled water to remove the catalyst and unreacted corrected to give the WSD values at a pressure of 1.4 kPa
methanol until the pH value of the water used was less (denoted WS1.4).
than 7. The water present in biodiesel was eliminated by
distillation at reduced pressure and 100 8C for 30 min. The
content of water in the unrefined biodiesel as prepared is 3. Results and discussion
about 40 ppm according to SH/T 0246-92 method [13].
3.1. Composition and fatty acid profile analyses
Table 1
Base fuel properties A typical chromatogram of biodiesel is shown in Fig. 1.
Property Method Base diesel It can be seen that FAME, MG, DG and TG were efficiently
Density (20 8C, kg/L) ASTM D4052 0.7911 separated and trace residual glycerides were readily
Viscosity (20 8C) ASTM D445 1.928 detected in the biodiesel. The results of GC are shown in
Sulfur (mg/L) SH/T 0253–92 [11] 166 Table 2. The contents of methyl esters in unrefined
Nitrogen (mg/L) SH/T 0657–1998 [12] 2.6 biodiesels were not more than 97% w/w, and small
HFRR (mm) 735
quantities of MG, DG and TG were detected, while only
Distillation (8C for ASTM D86
percentage off) methyl esters were detected in the refined biodiesels.
Initial 188 This analytical method cannot distinguish free fatty acid
10% 198 from FAME. In order to analyze the purity of biodiesels,
50% 208 acid value was measured. The results are presented in
90% 218
Table 2. The acid value of unrefined biodiesel is about
End point 231
0.2 mg KOH/g biodiesel, i.e. about 0.1% w/w FFA
 J.B. Hu et al. / Fuel 84 (2005) 1601–1606 1603

Fig. 1. Typical chromatogram of biodiesel.

(oleic acid as typical fatty acid) in biodiesel, while that of
refined biodiesel is higher. The composition of refined
biodiesel is mainly FAME containing little amount of FFA.
The fatty acid profiles of the biodiesels are shown in
Table 3. As expected, similar fatty acid profile was observed
in unrefined and refined biodiesels derived from the same
vegetable oil.
The content of methanol and free glycerol were also
determined by injecting the biodiesels into HP 5890 (OV1
capillary column) directly. No methanol and free glycerol
were detected, which means the contents are below the
lower detection limit of 0.05% w/w. The low contents of
methanol and free glycerol are due to washing and
distillation.
3.2. Lubricity testing
3.2.1. Lubricity properties of the unrefined and refined
biodiesels
The results of the lubricity tests are shown in Table 4. All
the biodiesels, including unrefined and refined biodiesels,
improved the lubricity of base diesel distinctly. When
unrefined biodiesels were used as lubricity enhancers, the
WSD value of diesel decreased significantly, from 735 to
351–429 mm, and were lower than the acceptable limit of
460 mm of EN590. When refined biodiesels were used, the
WSD value decreased to 528w567 mm, but were still over
the acceptable limit of 460 mm. It can be obviously seen that
all the unrefined biodiesels showed improved lubricity
properties over all the refined biodiesels.
Obviously, the lubricity enhancing properties of unre-
fined biodiesels are different from those of refined
biodiesels. The fatty acid profile of unrefined and refined
biodiesels derived from the same vegetable oil was similar,
so it is not the different fatty acid profile that influences the
lubricity properties. The acid value of refined biodiesel is
higher than that of unrefined biodiesel. As fatty acid can
increase the lubricity of diesel [16], the decreasing lubricity
properties of refined biodiesel to unrefined biodiesel are not
contributed to FFA. In the meantime, methanol and free
glycerol were very little (not detected) in biodiesels, which
means the lubricity difference is not due to methanol and
free glycerol. Therefore, MG, DG, and TG are the most
probable compounds that influence the lubricity properties
of them.
To determine whether one kind or all kinds of the
glycerides influence the lubricity, some typical compounds
were used, i.e. 1-monoolein used as monoglycerides, 1,3-
diolein used as diglycerides, and triolein and canola oil used
as triglycerides. Refined biodiesel derived from canola oil

Table 2
Composition and acid value of biodiesels

Biodiesels Sunflower Corn Canola Soybean Refined sun- Refined canola Refined soybean
biodiesel biodiesel biodiesel biodiesel flower biodiesel biodiesel biodiesel
Methyl esters 96.46 94.88 96.19 96.70 98.48 98.00
(w/w%)
Monoglycerides 0.34 0.27 0.35 0.49 ND ND
(w/w%)
Diglycerides 0.46 0.37 0.20 1.10 ND ND
(w/w%)
Triglycerides 0.44 1.64 0.78 ND ND ND
(w/w%)
Acid value 0.14 0.21 0.20 0.18 0.30 0.38
(mg KOH/g)

ND, not detected.

1604 J.B. Hu et al. / Fuel 84 (2005) 1601–1606

Table 3
Fatty acid profiles of biodiesels

Biodiesels Fatty acid (% w/w)

Palmitic Stearic Oleic Linoleic Linolenic Arachidic Eicosenoic Behenic Erucic
C16:0 C18:0 C18:1 C18:2 C18:3 C20:0 C20:1 C22:0 C22:1
Sunflower biodiesel 5.79 5.68 20.43 66.02 – 0.58 – 1.01 –
Corn biodiesel 12.31 2.01 29.79 54.72 0.53 0.64 – – –
Canola biodiesel 4.58 2.01 60.00 21.66 7.92 0.78 1.52 0.33 0.79
Soybean biodiesel 10.32 3.99 22.42 53.48 7.82 0.54 0.30 0.56 –
Refined sunflower biodiesel 6.15 5.53 20.61 67.09 – 0.22 – 0.34 –
Refined corn biodiesel 12.71 1.93 28.96 54.8 0.71 0.53 0.24 – –
Refined canola biodiesel 5.82 2.04 59.08 23.24 7.34 0.51 0.91 – 0.26
Refined soybean biodiesel 14.15 3.67 22.14 52.57 6.91 0.31 – – –

Table 4
WSD values of base diesel blended with 2% w/w unrefined and refined biodiesels

Biodiesels Sunflower Corn Canola Soybean Refined sun- Refined corn Refined canola Refined soybean
biodiesel biodiesel biodiesel biodiesel flower biodiesel biodiesel biodiesel biodiesel
WS1.4(mm) 429 366 351 375 528 567 543 540

(RCME) was employed as base biodiesel. And in this 3.2.3. Effects of diglycerides on the lubricity properties
research, oleic acid was also used to test the effect of free of biodiesel
fatty acid on the lubricity properties of biodiesel. Biodiesels containing about 1.0–2.0% and 0.4–0.8% w/w
diolein were prepared and the lubricity properties were
evaluated by using them as diesel lubricity enhancers The
3.2.2. Effects of monoglycerides on the lubricity properties
WSD value of diesel blended with 2% w/w RCME
of biodiesel
containing 0.4–0.8% w/w diolein is 470 mm, while if
1-monoolein was used as typical monoglyceride and
RCME contained 1.0–2.0% w/w diolein, the WSD value
added to RCME with the addition of 0.25, 0.5, 0.8, and 2.0%
of diesel is 453 mm. The lubricity properties of RCME
w/w each. Then RCME containing different amounts of
changed slightly due to the addition of diolein. If less than
monoolein was added to base diesel by 2% w/w and HFRR
0.4% w/w diolein was added to RCME, the WSD value of
wear scar diameter was measured. Fig. 2 illustrates the
diesel is expected to approach 543 mm, which is the WSD
lubricity improvement due to the addition of monoolein to
value of diesel blended with RCME. The results show that
RCME. Only 0.25% w/w monoolein can greatly enhance
diglycerides have impact on the lubricity properties of
the lubricity properties of refined canola oil methyl esters. If
biodiesel, but not as significantly as monoglycerides.
0.25% w/w monoolein was added to RCME and then the
RCME was added to base diesel by 2% w/w, which means
only 50 ppm monoolein was added to RCME, the WSD
value decreased from 735 to 425 mm, while no monoolein
was added to RCME, the WSD value only decreased to
543 mm. That is to say, 50 ppm monoolein can change the
WSD of diesel (blended with 2% biodiesel) with a decrease
of 21.7%. It has been reported that when 125 ppm
monoglycerides (92%, derived from rapeseed oil) was
added to a base diesel, the WSD decreased from 630 to
366 mm, about 41.9% [17]. Obviously, monoglycerides are
good lubricity enhancers and have much more lubricity
enhancing properties than pure biodiesel (FAME). When
0.5, 0.8, and 2.0% w/w monoolein were added to RCME,
the WSD value of diesel with the additives decreased to 358,
274, and 199 mm each. Undoubtedly, the lubricity properties
of biodiesel are significantly influenced by the concentration Fig. 2. Wear performance of RCME with different content of monoolein in
of monoglycerides in it. base diesel.
 J.B. Hu et al. / Fuel 84 (2005) 1601–1606 1605

not affect the lubricity enhancing properties of biodiesel

when the content is not too high.

3.2.5. Effects of free fatty acids on the lubricity properties

Fig. 3. Wear performance of RCME with different content of oleic acid in
base diesel (dashed is the regression fit line between WS1.4 mm of diesel
and oleic acid content in RCME).
3.2.4. Effects of triglycerides on the lubricity properties
of biodiesel
Triolein was used as typical compound to evaluate the
effects of triglycerides on the lubricity enhancing properties
of biodiesel 2.0% w/w triolein and 0.8% w/w triolein were
added to RCME in turn and then the biodiesel was added to
base diesel by 2.0% w/w. The HFRR wear scar diameter
data were 545 mm and 528 mm each, very close to 543 mm.
So it can be concluded that triglycerides may not influence
the lubrication properties of biodiesel if their concentration
is not too high.
In this research, food-grade canola oil was also used as
triglycerides. Generally speaking, food-grade canola oil
contains purified triglycerides (more than 96% w/w). The
composition of food-grade canola oil was measured by GC
method. A little amount of diglycerides was detected while
no monoglycerides were detected. Little amount of
diglycerides did not affect the lubricity of biodiesel when
canola oil was added to RCME by 2% w/w.
When RCME was blended with 2.0% w/w canola oil and
then added to base diesel, the WSD value of diesel was
536 mm, approximately 543 mm. No matter which triglycer-
ides source was used, the result is the same: triglycerides do
Table 5
International biodiesel standards
of biodiesel
Four samples were prepared by adding 0.2, 0.5, 0.8, and
2.0% w/w oleic acid to RCME each time. Because the
RCME biodiesel still contained little amount of FFA, and
the acid value was 0.30, about 0.15% w/w oleic acid in
RCME, the relatively exact contents of oleic acid in the four
biodiesels as prepared were 0.35, 0.65, 0.95, and 2.15% w/w
each. The decreasing WSD lubricity value of diesel as a
function of FFA in biodiesel is shown in Fig. 3. The
lubricity of diesel with 2% RCME was significantly
improved by adding oleic acid to RCME. The WSD values
of diesel blended with RCME with different content of oleic
acid were 488, 449, 419, and 235 mm in turn, and decreased
almost linearly with the increasing content of oleic acid. If
0.5% w/w oleic acid was added to RCME and then the
RCME was added to base diesel by 2% w/w, which means
only 100 ppm oleic acid was added to RCME, the WSD
value decreased from 735 mm to about 460 mm, the upper
limit of EN590, while no oleic acid was added to RCME, the
WSD value only decreased to 543 mm. FFA has good
lubricity enhancing properties. Other researchers have got
the same results. C. Kajdas et al. [16] reported that when
100 ppm stearic acid (O90%) was added to a base diesel,
the WSD decreased from 691 to 493 mm, about 28.7%.
The results in Fig. 3 show FFA can also influence the
lubricity properties of biodiesel. By comparing the results in
3.2.2–3.2.5, it can be seen that the effects of FFA on the
improvement of lubricity properties of biodiesel are less than
those of MG, but more significant than DG and TG. The
linearity of WSD values versus oleic acid concentrations in
RCME was drawn by a linear fit (dashed in Fig. 3). The WSD
value of diesel blended with non-FFA RCME was obtained
by extending the line to Y-axis, about 552 mm.
3.2.6. Comparing all variables investigated with biodiesel
quality standards
Parts of the requirements of the current world standards
are listed in Table 5 [18]. Some of the maximum contents of

Austria Czech France Germany Italy Sweden USA

Republic
Standard ON CSN 65 Journal DIN E UNI SS ASTM
Specification C1191 6507 Official 51606 10635 155436 PS121–99
Water (mg/kg) – !500 !200 !300 !700 !300 !500
Acid value (mg KOH/g) !0.8 !0.5 !0.5 !0.5 !0.5 !0.6 !0.8
Methanol (% w/w) !0.20 – !0.1 !0.3 !0.2 !0.2 –
Ester content (% w/w) – – O96.5 – O98 O98 –
Monoglycides (% w/w) – – !0.8 !0.8 !0.8 !0.8 –
Diglyceride (% w/w) – – !0.2 !0.4 !0.2 !0.1 –
Triglyceride (% w/w) – – !0.2 !0.4 !0.1 !0.1 –
Free glycerol (% w/w) !0.02 !0.02 !0.02 !0.02 !0.05 !0.02 !0.02
1606 J.B. Hu et al. / Fuel 84 (2005) 1601–1606
different compositions in biodiesel in all the standards are
as follows: MG!0.8% w/w; DG!0.4% w/w; TG!0.4%
w/w; acid value!0.8 mgKOH/g biodiesel, i.e. FFA!0.4%
w/w (oleic acid as typical FFA). Based on the results above,
the lubricity enhancing properties of a biodiesel meeting the
standards are affected not only by the methyl esters, which
are the main composition in biodiesel, but also by the small
quantities of MG, FFA, and DG. The concentrations of FFA
and DG are too low by the standards and just influence the
lubricity properties slightly. However, the concentration of
MG is high enough to greatly affect the properties.
Therefore, the lubricity properties of biodiesels are
determined mainly by methyl esters and monoglycerides.
As the content of methyl esters is very high, exceeding 96%
w/w, the small changes of content do not affect the lubricity,
but because the concentration of MG is very low, less than
0.8% w/w by the standards, and the concentration of MG
influence the lubricity properties markedly, the biodiesels
with different content of MG may have different lubricity
properties. It is not easy to obtain biodiesels with the same
low content of MG in the lab even by the same researchers
using the same reaction conditions, so to compare the effects
of type of alcohol and fatty acid profile of the vegetable oil
on the lubricity enhancing properties of biodiesel is
probably not so exact if the impacts of MG and other
compounds are not excluded.
Based on the research, it can be seen that the lubricity
properties of pure biodiesel, i.e. FAME, is not as good as it
should be. If the compound(s) with the addition amount less
than 1% is not called as additive. Therefore, biodiesel free of
MG, FFA et al. cannot be used as diesel lubricity additive, but
it can be used as diesel blend to improve the lubricity of diesel.
4. Conclusions
In this research, a study on the lubricity enhancing
properties of biodiesels was performed. Unrefined biodiesels
and refined biodiesels derived from vegetable oils were made
and then were added to a base diesel. The WSD values were
measured by HFRR method. Unrefined biodiesels showed
higher lubricity properties than refined biodiesels. The
factors that affected the lubricity of biodiesels were also
studied. Fatty acid methyl esters and monoglycerides were
the main compositions affecting the lubricity properties of
biodiesel if the biodiesel met the international standard, and
free fatty acids and diglycerides affected them slightly, while
triglycerides almost had no effects.
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