Tribology International 92 (2015) 301306

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Tribology International
journal homepage: www.elsevier.com/locate/triboint

Studies on biodegradability of bio-based lubricants

F. Murilo T. Luna a, Jefferson B. Cavalcante a, F. Ordelei N. Silva b,1, Clio L. Cavalcante Jr.a,n
a
Universidade Federal do Cear, Departamento de Engenharia Qumica, Grupo de Pesquisa em Separaes por Adsoro GPSA, Campus do Pici, Bl. 709,
Fortaleza, CE 60455-900, Brazil
b
Universidade Federal do Cear, Departamento de Qumica Orgnica e Inorgnica, Laboratrio de Bioinorgnica, Campus do Pici, Bl. 735, Fortaleza,
CE 60455-900, Brazil

art ic l e i nf o

a b s t r a c t

Article history:
Received 17 March 2015
Received in revised form
6 July 2015
Accepted 8 July 2015
Available online 16 July 2015

Vegetable or synthetic lubricants, also called biolubricants, are less harmful to the environment. In order
to quantify their biodegradability, some tests are able to predict how long oil/lubricants will take to be
degraded in the environment. This study proposes to evaluate the biodegradability of bio-based
lubricants using a bio-kinetic model (without microorganisms), comparing their performances with
fresh vegetable oil and mineral oil. The results are presented through an Effective Composition for
Biodegradation (ECB), half-lives and biodegradation time prole. The synthesized biolubricants showed
ECB values closer to vegetable oil than mineral oil. Half-life times are approximately 12 days for fresh
vegetable oil, around 2030 days for the biolubricants, and over 200 days for the mineral oil.
& 2015 Elsevier Ltd. All rights reserved.

Keywords:
Biodegradability
Bio-based lubricant
Basestock oil

1. Introduction
Biodegradability is an important characteristic for the majority
of today's chemical industry products, and represents a way of
measuring the risk level of decomposition presented by these
products when deployed to the environment. Biodegradation is a
natural process caused by the action of microorganisms, in the
presence of oxygen, nitrogen and minerals.
In the process of formulating lubricant oils, biodegradability is
strongly dependent on the oil used. Basestock oils and nished
lubricants are products with a potential risk of being in direct
contact with the environment, which may happen in their
production, distribution, services usage or even in disposal after
their utilization. Therefore, environmental authorities have been
increasingly demanding less toxicity in these products, so they will
cause less harm to the nature [13].
The impacts on the environment caused by inappropriate
disposal of the wastes are huge. Lubricants, when in intentional
or accidental contact with the soil, make it useless for farming and
civil construction, killing the vegetation and the microorganisms
[4,5]. Brazilian Environmental National Council (CONAMA) determine that the best environmental management for used or
contaminated oils is re-rening and, for that, there are many
companies properly registered in this Council that are able to
perform this activity [6].

Corresponding author. Tel.: 55 85 3366 9611; fax: 55 85 3366 9601.

E-mail address: celio@gpsa.ufc.br (C.L. Cavalcante Jr.).
1
Present address: Universidade Federal do Rio Grande do Norte, Instituto de
Qumica, Av. Salgado Filho, Lagoa Nova, Natal, RN 59.072970, Brazil.
http://dx.doi.org/10.1016/j.triboint.2015.07.007
0301-679X/& 2015 Elsevier Ltd. All rights reserved.

Some kinds of lubricants are more risky to be in contact with

the environment and because of that they must be preferably
formulated with less environmentally toxic and more biodegradable products. Some pathways are already being explored such as:
chainsaw oil, drilling uids and lubricants for the train line. Other
applications of highly biodegradable lubricants are in services that
may contain leaking risks, like forest and mining equipment and in
very sensible areas like platforms, agricultural equipment and
hydroelectric power plants. However, environmental agencies
have been trying to put more restrictions to all the products with
low biodegradation rate, whether they are used for risky applications or not. The intention is that when these products get in touch
with the environment, accidentally or not, they may be quickly
isolated and treated [79].
Nowadays, there are plenty of evaluation methods of biodegradability. Most of them use microorganisms to obtain the data,
even though they are difcultly adjusted and long time methods.
The analysis methods of biodegradability without using microorganisms are relatively recent and were based on the oils
components and their degradation reactions [10]. However, it is
still not clear what is the criteria to determine if certain basestock
oil is biodegradable or not, that is, what quantity of sample will
biodegrade and how long it will take, yet the evaluation of the
biodegradability is an important tool of comparison between two
different lubricants.

2. Standard methods
One of the rst methods proposed to evaluate the biodegradability of lubricant oils and fuels was the CEC L-33-T-82,

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F.M.T. Luna et al. / Tribology International 92 (2015) 301306

established by the Co-ordinating European Council (CEC). The

method uses a standard uid of known biodegradability where
both, the standard and the sample are inoculated with microorganisms. The progress of the reaction is accompanied by infrared
throughout a period of 28 days. This was the most used and
known method by biolubricants producing companies in years.
Over the years, this method has not passed through many changes
and was updated to the method CEC L-33-A-94 which stipulated
that a biodegradable sample, by denition, would have to be 80%
consumed in 21 days [11].
Another way of monitoring these reactions is the quantication
of carbon dioxide released from decomposition, since the reactions
of biodegradation form CO2 and water at the end of the process.
This point of view was adopted by American Society for Testing
and Materials (ASTM) with the ASTM D5864-11 [12] method
(Standard Test Method for Determining Aerobic Biodegradation
of Lubricants and Their Components), which simulates a natural
aqueous environment of biodegradation and quanties the production of CO2. According to this method, ASTM labels a sample as
fully biodegradable if 60% of that sample has been completely
converted to CO2 over a period of 28 days [3,13,14]. With this same
concept of monitoring, there were several other methods with
different forms of analysis of CO2 and different criteria for judging
the biodegradability of the sample.
The method developed by the Organization for Economic
Cooperation and Development (OECD) is also based on the CO2
production by the samples biodegradation. The CO2 is captured in
a sodium or barium hydroxide solution which is then titrated and
the amount of CO2 emitted is quantied. A biodegradable sample
must exhibit, in a period of 28 days, a consumption greater than or
equal to 60% of the initial sample. In order to measure the ultimate
stage of the aerobic biodegradation process, the OECD 301 B
method is used in aqueous or soil medium as an ultimate
biodegradation test [15]. Another developed method is the Bartha
Respirometer Method. In this method, the produced CO2 is
captured by a KOH solution. The result of this method is a graph
expressing the quantity of CO2 produced as a function of the
analysis time [3,16].

and synthesized oils, where the method performed well showing a

half-life of 25 days for the synthesized oil, presenting a considerable higher biodegradability when compared to mineral oils. In
this context, Silva et al. (2013) [20] compared the biodegradability
of two lubricant base uids from castor biodiesel esters, using two
different catalysts, tin and sodium methoxide, concluding that the
presence of tin may decrease the oxidative stability and biodegradability of such products.
Beyond the ASTM D7373-12 [18] method, other studies have
reported different ways of measuring biodegradability, for example the use of a lysimeter to follow the migration and progressive
primary biodegradation of lubricants [14]. Another approach is the
use of mathematical models along with experimental data to
predict how different types of oils may affect the parameters in
biodegradation kinetics [21].
This study proposes to evaluate the biodegradability of two
different bio-based lubricants from castor oil and compare their
performances with samples of mineral oil and pure vegetable oil,
using bio-kinetic tests.

2.1. Bio-kinetic method

3.2. Preparation of bio-based lubricants

The difculty of working with microorganisms combined with

the long time taken on the analysis led Rhee (2005) [10] to
develop a method capable of estimating, rapidly and reliably, the
biodegradability of a lubricant sample without the use of
microorganisms.
Although there are many methods for this purpose, few results
were similar to those reported by ASTM D5864-11 [12], adopted as
consistent for this assessment. The use of a bio-kinetic model
(equations for biomass growth, such as Monod details in Ref.
[10]) and the knowledge about the biodegradation process for oils
led them to obtain correlations to estimate half-life and calculate
the cumulative biodegradation consistent with the ASTM D586411 [12] method.
The oil biodegradation depends on its chemical composition.
The saturated chains are easily attacked by microorganisms and
tend to biodegrade. However, aromatic and polymeric chains are
unlikely to be attacked by microorganisms and are more resistant
to biodegradation [10,17].
From the work published by Rhee (2005) [10], it was developed
a standard method to evaluate the biodegradation of base oils and
lubricants without the use of microorganisms (ASTM D7373-12
[18]). Since this is considered a recent method, not many researchers have studied biodegradability using this approach. However,
Luna et al. (2010) [19] reported the use of this bio-kinetic model to
estimate and compare the biodegradability of mineral, vegetable

Two different biolubricants were synthesized and coined as

BLx, where x is related to the alcohol used in the esterication step
(1 for 2-ethyl-1-hexanol; 2 for 1-octanol), as depicted in Figs. 1 and
2. The esterication reactions were conducted with ricinoleic acid
in a batch reactor (200 mL) maintained at 80 1C for 24 h under
inert atmosphere. Acid/alcohol molar ratios were 1:1.2 for 2-ethyl1-hexanol, and 1:2 for 1-octanol. All esterication homogeneous
reactions were catalyzed by boron triuoride diethyl etherate
(0.5 wt%). The acetylation reactions were performed with acetic
anhydride using an alkaline catalyst (KOH, 5 wt%). The reaction
was carried out homogeneously in liquid phase at 90 1C for 12 h
under inert atmosphere and intense stirring. The products were
puried using a Kugelrohr distiller under high vacuum at 110 1C to
remove excess alcohol. After separation, the products were

3. Materials and methods

3.1. Materials
Samples of mineral oil were provided by Petrobras (Brazil) and
the vegetable oil used for this study was commercial castor oil
from Proquinor (Brazil). Physicochemical properties of these
samples are reported in Table 1. Ricinoleic acid ( 498 wt%),
obtained from castor oil, was kindly supplied by MiracemaNuodex (Brazil). Analytical-grade reagents (n-pentane, toluene,
diethyl ether anhydrous, acetic anhydride and ethyl alcohol) were
from J.T. Baker (USA). 2-Ethyl-1-hexanol ( 499.6%), 1-octanol
anhydrous (499%) and boron triuoride diethyl etherate were
from Sigma-Aldrich (USA). Silica gel (70230 mesh) and activated
bauxite (2060 mesh) were supplied by Macherey-Nagel (Germany) and Curimbaba (Brazil), respectively.

Table 1
Physicochemical properties of vegetable and mineral oils.
Samples

Specic gravity Pour

at 20 1C (g/cm) point
(1C)

Castor oil 0.958

0.892
Mineral
basestock oil

 15
 33

Flash
point
(1C)

TAN
(mg
KOH/g)

Viscosity (cSt)

286
162

1.120
0.001

261.3 19.6
19.9 4.8

VI

40 1C 100 1C
84
174

F.M.T. Luna et al. / Tribology International 92 (2015) 301306

303

Fig. 1. Synthesis of BL1 samples.

Fig. 2. Synthesis of BL2 samples.

checked for purity by GC/FID (495 wt%). Physicochemical properties of these samples are reported in Table 2.
3.3. Biodegradability method
The method described by Rhee (2005) [10] was performed to
estimate the biodegradability of lubricants, without using microorganisms. This procedure uses a bio-kinetic model, which was
already validated as a very accurate method when compared to
the standard results obtained using the ASTM D5864-11 [12]
method (which evaluates the biodegradation of lubricants using
aerobic microorganisms) to quickly estimate the biodegradability
of lubricants. This method uses glass chromatographic columns
packed with silica gel and bauxite activated under nitrogen gas
ow, as shown in Fig. 3.
The experiments were performed using initially 2 g of the
samples dissolved in 10 mL of n-pentane. According to the

Table 2
Bio-based lubricants physicochemical properties.
Samples Specic gravity Pour
at 20 1C (g/cm) point
(1C)
BL1
BL2

0.9033
0.9138

 42
 36

Flash
point
(1C)

TAN
(mg
KOH/g)

Viscosity (cSt)

264
258

0.021
0.025

17.6
18.3

VI

40 1C 100 1C
4.31
4.33

159
152

method, if the sample does not dissolve completely in n-pentane

at room temperature, it must be heated up to 40 1C in a water bath.
Cyclohexane may be used if even heated n-pentane is not capable
of dissolving the sample completely.
The dissolved sample was poured in the top of the column to
start the elution procedure with different solvents. In order to
elute the non-aromatic fraction (F1) 35 mL of n-pentane were

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F.M.T. Luna et al. / Tribology International 92 (2015) 301306

4. Calculations
According to Rhee (2005) [10] the Effective Composition for
Biodegradation (ECB) is calculated based on the quantity of nonaromatics and esters fractions, associated with the ECB coefcient
(), as shown in Eq. 1.
ECB U F 1 F 3 =100

where: F1 is the mass fraction of non-aromatics, F3 is the mass

fraction of esters and similar and is the ECB coefcient according
to Table 3.
With the ECB data of many samples, Rhee (2005) [10] correlated the experimental half-life times in order to obtain a relationship between these two parameters. Among the correlated
samples are base mineral oils, hydraulic oils, poly-alpha-olens,
and vegetable oils, amongst others.
The Eq. (2) represents the correlation obtained by Rhee (2005)
[10] which connect the half-life (t1/2) with the determined ECB.
t 1=2 6:8  ECB  2:38

The cumulative biodegradation of all samples was estimated

based on the bio-kinetic model, according to the Eq. (3).
Bt B1

Fig. 3. Packed column with bauxite and silica gel.

Table 3
Coefcients for the ECB calculation (Rhee, 2005
[10]).
Lubricants base

ECB Coef. ()

Mineral
Poly-alpha-olen 2a
Poly-alpha-olen 4a
Poly-alpha-olen 6 or superiora
Natural Esters
Polyol Esters

0.3
0.8
0.6
0.4
1.0
0.8

Poly-alpha-olens viscosity's degree.

added. After the F1 is eluted, the non-polar aromatic fraction (F2)

was eluted using 80 mL of a 50% pentane/toluene mixture. Esters
and similar products (F3) were eluted using 80 mL of diethyl ether.
Finally, the polar aromatics (F4) were eluted using 100 mL of
chloroform and 75 mL of ethyl alcohol.
The solvents from the collected samples were completely
removed using a rotary evaporator and the material left in the
ask was weighted, allowing the determination of the fractions of
non-aromatic, non-polar aromatics, esters, aromatic and polar
compounds. For the rst fraction (non-aromatic products) the
bath was set to 50 1C. For the following fractions, the temperature
was progressively raised until the bath reaches complete evaporation, paying attention not to raise the temperature so high that the
sample may be lost to evaporation.
When all the solvent is evaporated, the ask was weighted and
compared to its initial weight, calculating thus the mass fraction.
After three consecutive weighing and evaporation, it was considered that all the solvent had been eliminated whenever the
difference observed between two consecutive weighing was less
than 20 mg. After all the fractions were determined, their summation would have to be at least 95% of the initial weight of the
sample, if the value of 95% was not reached it would mean there
were loses in the steps of the analysis, therefore the experiment
would need to be repeated.

0:49  lnt
lnt 1=2

where: B(t) is the cumulative biodegradation with time, B(1)

0.01, t is time in days and t1/2 is the half-life in days. According to
Rhee (2005) [10], this method provides an excellent correlation
with the standard biodegradation tests [12,22]. Therefore, this
approach was used to estimate and compare the biodegradability
of biolubricants synthesized in laboratory relating to products
usually biodegradable like vegetable oils and to products of low
biodegradability such as base oils derived from petroleum.

5. Results and discussion

5.1. Physicochemical properties
The evaluated physicochemical parameters were specic mass,
pour point, total acid content, ash point and kinematic viscosity.
The viscosity index (VI) was also calculated in order to indicate the
oil viscosity variation with temperature and is normally used as an
important parameter to evaluate lubricant oils, the higher the
viscosity index, the lower is the viscosity variation with temperature. These measurements were performed to evaluate the differences in results obtained with the bio-based lubricants when
compared with two extreme behaviors (pure vegetable or petroleum based oil).
Analyzing the values from Table 1, we see a lower pour point in
the mineral basestock oil whereas the castor oil has a higher ash
point. The vegetable oil viscosity is also higher for 40 and 100 1C.
The total acid number (TAN) shows a much higher value for the
castor oil, indicating it has a larger amount of acidic components.
Viscosity index analysis showed a high value for the vegetable oil
and a very high value for the mineral oil, which means the
basestock oil, has a lower viscosity variation with temperature.
The bio-based lubricants BL1 and BL2 present very similar
properties, except for the pour point value, in which BL2 (obtained
from 1-octanol) show a slightly higher value than BL1 (obtained
from 2-ethyl-1-hexanol). This may be due to the branching of the
alcohol used to obtain BL1, as previously reported by other authors
[23]. When compared to the physicochemical properties of the
pure castor oil and the mineral oil, we notice that most properties
of the biolubricants obtained for this study have values closer to
the mineral oil basestock, except for the ash point values.

F.M.T. Luna et al. / Tribology International 92 (2015) 301306

305

According to the Brazilian National Petroleum Agency (ANP),

synthetic basestock oils must have VI values higher than 120
[24], thus biolubricants BL1 and BL2 satisfy this requirement.
However, the specic application of a given lubricant oil is also
related to the viscosity value. It may be observed that the biobased samples obtained from castor oil have viscosities that are
much lower than the values for castor oil. This can be related to
the smaller chain length of the molecules of BL1 and BL2 when
compared to vegetable oil triglyceride molecule, as also observed
in previous studies [2527].

5.2. Biodegradability
The biolubricants biodegradability was estimated using the
bio-kinetic model. Before carrying out the tests with the biolubricants, biodegradability analysis of samples from vegetable
castor oil was performed to assess the results of a typical
biodegradable product. The results from this method are the
Effective Composition for Biodegradation (ECB), the half-life and
the estimation of the percentage of biodegradation as a function of
time. The values found for three runs with the same sample of
pure castor oil are shown in Table 4. The results indicate that
vegetable oil shows values of ECB and half-life close to those
reported by Rhee (2005) [10] for canola oil (t  9 days).
For the bio-based lubricant samples evaluated, it was observed
that BL1 and BL2 showed half-lives of about 26 and 20 days,
respectively. In Figs. 4 and 5, cumulative biodegradation estimates
as a function of time are presented for three experimental runs for
BL1 and BL2, respectively, showing average ECB of 0.57 for BL1 and
0.64 for BL2.
The estimated cumulative biodegradation for the naphthenic
mineral oil samples is shown in Fig. 6. Good reproducibility for
three replicates can be observed as previously seen for the other
samples. According to Rhee (2005) [10], for mineral lubricants, ECB
values range from 0.22 to 0.36 and half-lives from 114 to 231 days.
The ECB values and half-lives obtained for the samples of mineral
oil evaluated in this study are thus within the range reported above.
It may be observed that the biodegradability of the mineral
naphthenic oil is lower than what was observed for the biolubricant samples (average ECB of 0.23 and half-life of  225 days). For
mineral base oils, several authors have reported biodegradability
studies relating their results with chemical and physical properties
[28,29] or their chemical composition [17]. In general, the biodegradability of basestock mineral oils is strongly related to the
presence of aromatic and naphthenic compounds in their composition (the higher the content of these compounds the lower the
biodegradability). The bio-based lubricants in this study, obtained
from castor oil, would be likely to present higher biodegradability
than mineral basestock oils.
A comparison between the biodegradation proles for the
biolubricant samples with those for castor vegetable oil and for
the mineral oil samples is presented in Fig. 7. As mentioned before,
the biodegradability of the biolubricant samples are clearly higher
when compared to mineral oil. On the other hand, some loss in
biodegradability is observed for the biolubricant samples when
compared to the fresh castor vegetable oil, which was expected
Table 4
Effective composition of biodegradation (ECB) and halflife (t) for three runs with pure castor oil.
Run

ECB

1
2
3

0.774
0.802
0.780

 12 days

Fig. 4. Estimated biodegradation proles for the BL1 biolubricant. () Exp. 1; (  )

Exp. 2; and () Exp. 3.

Fig. 5. Estimated biodegradation proles for the BL2 biolubricant. () Exp. 1; (  )

Exp. 2; and () Exp. 3.

Fig. 6. Estimated biodegradation proles for the mineral basestock oil. () Exp. 1;
(  ) Exp. 2; and () Exp. 3.

since castor oil is a natural triglyceride. However, there are several

limitations to the use of castor oil as direct lubricant related to
thermal, oxidative and hydrolytic stability properties [4,23,30].
The synthesized biolubricant samples presented physicochemical
properties that are interesting for applications as lubricants (high
viscosity index and low pour point) with biodegradability properties somewhat closer to those of vegetable oils (in this case, castor
oil) than to the properties of mineral petroleum oils.

F.M.T. Luna et al. / Tribology International 92 (2015) 301306

Biodegradation (%)

306

100
90
80
70
60
50
40
30
20
10
0
0

20

40

60

80 100 120 140 160

Time (days)

Fig. 7. Estimated biodegradation proles for castor oil (), BL1 (  ), BL2 ( ) and
mineral oil (). Half-life times are 12, 26, 20 and 225 days, respectively.

6. Conclusions
This study estimates the biodegradability of different oils
(vegetable, synthesized and mineral), using experiments without
microorganisms. Two different synthesized biolubricants (BL1 and
BL2) were evaluated along with a mineral and a vegetable oil
(castor oil), using this method as a form of comparison. As
expected, the castor oil presented the highest ECB value (0.78)
whilst the mineral oil showed the lowest (0.23), which means a
very high half-life for the mineral oil and the opposite for the
vegetable oil. Nonetheless, the vegetable oil is not the best choice
to be used as a direct lubricant especially because of its limitations
in thermal and oxidative stability. In the other hand, the synthesized biolubricants have high viscosity index and low pour point,
which makes them an appropriate lubricant option, especially
because of the good half-lives they presented, around 26 days for
BL1 and 20 days for BL2. Very little difference may be identied
when comparing the half-lives of BL1 and BL2, meaning there is no
considerable change in using 2-ethylhexyl or octyl ricinoleates as a
bio-based lubricant. Furthermore, a huge difference can be spotted
when comparing the biodegradation as a function of time of the
synthesized lubricants with that of the mineral oil.
Acknowledgments
The authors wish to thank nancial and logistic support
provided by PETROBRAS (Petrleo Brasileiro S.A.) and CNPq (Conselho Nacional de Pesquisa e Desenvolvimento Cientco).
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