J Therm Anal Calorim
DOI 10.1007/s10973-017-6291-7
Evaluation of different aging procedures on biodiesel thermal
degradation process
R. S. Leonardo1,2 • M. L. Murta Valle1 • J. Dweck2
Received: 2 December 2016 / Accepted: 6 March 2017
 Akadémiai Kiadó, Budapest, Hungary 2017
Abstract The sediments that form during biodiesel oxi-
dation decrease the ignition quality, damaging the injector
nozzle, the filter and the motor operation system. They may
form in a very fast way, and their correct quantification is
still a problem. The insoluble oxidation products due
mainly to biodiesel degradation in diesel/biodiesel blends
may be characterized by several analytical techniques. The
conventional methods currently used for sediment quan-
tification are gravimetric, but do not present repetitive
results, still presenting a technical challenge to be solved.
In this work, the thermal degradation process of a com-
mercial soybean ethylic biodiesel (BS100) was evaluated
by thermogravimetry, derivative thermogravimetry and by
infrared spectroscopy, after being submitted to different
aging procedures. Analyses of samples aged at 43 C,
110 C and 150 C were compared to the original non-
aged sample. As diesel engines operate under oxidizing
conditions, thermal analyses were performed with synthetic
air and the results were compared with the analyses in
nitrogen.
& R. S. Leonardo
rosangela@coc.ufrj.br
M. L. Murta Valle
murta@eq.ufrj.br
J. Dweck
jodweck@yahoo.com.br
1
Laboratory of Biodiesel Stability Evaluation, Chemical
School, Federal University of Rio de Janeiro, Rio de Janeiro,
RJ CEP: 21 949-900, Brazil
2 less, it has undesirable characteristics such as poor oxida-
Thermal Analysis Laboratory, Chemical School, Federal
University of Rio de Janeiro, Rio de Janeiro,
RJ CEP: 21 949-900, Brazil
Keywords Soybean biodiesel
Thermal stability

Sediments
TG/DTG
IR
Introduction
Among petroleum-based fuels, diesel is one of the most
susceptible to the formation of sediments/gums [1]. The
oxidative stability of diesel is directly influenced by their
chemical composition, especially, by aromatic hydrocar-
bons, olefins and/or by reactive organic compounds con-
taining heteroatom such sulfur, nitrogen and oxygen
content [2–5].
In recent years, more and more countries are adopting
biodiesel as substitute for diesel for environmental and
energy security concerns. Biodiesel is fatty acid esters ethyl
or methyl produced by transesterification process, from
renewable sources, and miscible to conventional diesel fuel
in all proportions. The transesterification process, using
methyl or ethyl alcohol to produce biodiesel, is basically
the same. The alcohol methanol is the most used, due to its
low cost. However, ethanol alcohol that is produced from
renewable materials shows a less toxic effect on the envi-
ronment. As Brazil is a great ethanol producer, ethyl and
methyl biodiesels are commercially produced and used
indistinctly as fuel.
Biodiesel can be used in compression ignition engines
(diesel cycle) without significant modification in the sys-
tem [6, 7]. It is reported from the literature that biodiesel
has higher flashpoint and cetane number than petroleum
diesel. It tends to improve lubricity and has no sulfur and
aromatic compounds in its composition [8–11]. Neverthe-
tion stability, cold flow properties and tendency to the
formation of deposits [12–14].
123

The oxidative degradation products formed during
thermal stressing conditions or long-term storage difficult
the use of diesel and biodiesel fuels. Gum and sediments
that may be formed have a negative effect on biodiesel/
diesel atomization, clogging filters and nozzle injectors,
and can cause corrosion, reducing the engine performance
[15–19]. Using biodiesel or diesel/biodiesel blends fuels,
the knowledge of the mechanisms of gum and sediments
formation, resulting from oxidation processes, is necessary.
Previous studies have shown that as the content of
biodiesel in diesel/biodiesel fuel increases, the degradation
of the blend becomes higher, changing their physical and
chemical properties [20, 21]. These oxidation reaction
products contribute to the increase in acidity and viscosity
of the fuel [13, 22–28]. It is well established in the scien-
tific literature that interaction of the fuel with its environ-
ment, such as air, humidity [11], light [29, 30], higher
temperature [31, 32], microbial growth [33, 34], storage
time [35–38] and their unsaturation degree [39–43], is the
main factors related to this degradation process.
Sediments and gum are formed quickly, and its quan-
tification is difficult. These degradation products in diesel
fuel or diesel/biodiesel blends can be characterized by
various analytical techniques. Traditional methods cur-
rently used to quantify sediment and content in diesel are
the gravimetric ones [44]. These methods do not exhibit
reproductive values, which leads to many non-reliable
results for biodiesel and diesel/biodiesel blends.
The purpose of this study was to evaluate the oxidative
stability of a commercial soybean biodiesel (BS100), pro-
duced by ethylic route (FAEE). Different procedures were
used for accelerated aging, and samples were analyzed by
thermal analysis techniques as thermogravimetry (TG) and
derivative thermogravimetry (DTG), as well as by infrared
spectroscopy (IR). BS100 samples were aged at 43, 110
and 150 C. The results were compared with those of the
original non-aged biodiesel. The results of all samples
oxidized by different procedures were compared in order to
verify the effect of the temperature and the exposition time
on the profile of the degraded products.
Experimental
Materials and methods
In this research, a Brazilian commercial soybean biodiesel
(BS100) produced by ethylic route transesterification pro-
cess was used. The BS100 did not contain antioxidant, and
it was stored in a freezer until the beginning of the
research. In order to evaluate its thermal degradation pro-
cess as a function of temperature, samples were submitted
to different conditions of accelerated aging. Since the
123
R. S. Leonardo et al.
temperature is a determining factor for the degradation of
fuels, the formation of insoluble increases with increasing
temperature, according to Arrhenius’s Law [45, 46]. The
temperatures were selected among the literature range used
to characterize fuel in accelerated aging tests [47–49].
Samples were aged storing them in an oven, during 90 days
at 43 ± 1 and 110 ± 1 C selected from specific literature
data for experiments performed to characterize biodiesel
under accelerated conditions, and also for 2 days at
150 ± 1 C. After being submitted to those conditions, the
samples were analyzed using thermal analysis and infrared
techniques, and the results were compared to those of the
original non-aged biodiesel.
Thermal analysis
Thermal analyzes were performed using a Simultaneous
DSC-TGA equipment, model SDT-Q600 from TA Instru-
ments. Open platinum crucibles were used (110 lL) for the
sample and reference. Calibration runs were performed
according to manufacturer’s recommended procedures.
Samples of 12 mg (±0.3 mg) were employed, at a heating
rate of 10 C min-1, from room temperature to 800 C.
Nitrogen and synthetic air were used as purge gases, at
100 mL min-1 flow rate. The results were analyzed using
the equipment Universal Analysis software. In order to
interpret the results more accurately, DTG curves were
deconvoluted by using the OriginLab 8.5 software, apply-
ing the Gaussian method, and all deconvolution coeffi-
cients presented an R2 value greater than 0.98. These
deconvolutions were used to determine the temperature at
which ends the mass loss of the residual low molecular
components, on aged sample TG curves, as exemplified in
Fig. 1.
4
R2= 0.9962
Deriv.mass/% min–1
2
1
0 End of low molecular components
mass loss
125 250 375 500 625 750
Temperature/°C
Fig. 1 Example of DTG curve deconvolution
Evaluation of different aging procedures on biodiesel thermal degradation process

Infrared (FTIR)
The spectrum data for all samples were recorded in trans-
mittance mode, using the Nicolet spectrometer, model
Magna IR-760 (ThermoNicolet Analytical Instruments,
Madison, WI), equipped with DTGS (deuterated tri-glycine
sulfate) as detector and potassium bromide (KBr) as beam
splitter. The samples for FTIR analysis were applied as a
film on pressed by KBr cells. The analyses were performed
using 4000–500 cm-1 range, by accumulating 16 scans
with 4 cm-1 resolution.
Results and discussion
The results obtained by thermogravimetric analysis (TG/
DTG) are presented in Figs. 2–5, and the FTIR spectrums in
Figs. 6–8. Figure 2a shows TG/DTG curve of fresh biodiesel
(BS100). From Fig. 2a, it can be seen that fresh BS100 shows
a single significant step of mass loss, in N2 and air atmo-
spheres, with a very pronounced DTG peak, which can be
attributed mainly to the volatilization of biodiesel. During
the analysis in air, afterward, a second small mass loss step
occurs, characterized in the DTG curve by a much lower
mass loss rate, due to the thermal decomposition of higher
molecular products formed in the previous step by the oxi-
dation promoted by the air. The total temperature ranges of
mass losses are 100–274 C in nitrogen, and 101–500 C in
air, considering respective TG curves.
As shown in Fig. 2b–d, the TG/DTG curves for the aged
samples in nitrogen and air show two or more mass loss
steps, and some of them are not completely separated. The
first probably corresponds to the volatilization of the
residual biodiesel original components loss, and the
other(s) can be attributed to the loss of higher molecular
weight components formed during aging, and/or during the
runs in air. The overlayed TG/DTG curves indicate that in
air, all aged samples show a higher content of heavy oxi-
dation products than in N2 case, because in air, they rep-
resent the sum of those produced during aging and those
produced during analysis. The degradation during storage,
characterized by a higher mass loss after the first mass loss
step, is more severe at higher storage temperatures, as
shown in Fig. 3.
Figure 4 presents the TG/DTG curves of biodiesel fresh
and aged samples at 43 and 150 C in nitrogen. The aging
temperature of biodiesel is a determining factor for the
degradation degree of the original biodiesel components.
As is shown in this figure, aging at 43 C for 90 days and at
150 C for 2 days promotes practically equivalent
degradation.
In Fig. 5 is shown, for biodiesel fresh and all aged
samples, the quantification of the heavy fraction (temper-
ature decomposition higher than 300 C) formed during
aging and during analysis in air and in nitrogen. It can be
noted that for all the evaluated samples, there was a greater
formation of heavy fractions in the analyses performed in
air, when compared with the respective runs carried out in
nitrogen. As the biodiesel was being oxidized, products
were formed which products decompose in different ways
and at higher temperatures, indicating that heavier products
than BS100 were produced. For samples aged for 90 days

Fig. 2 TG/DTG curves for 110 12

40
fresh and aged biodiesel 100 85
(b)

Deriv.mass/% min–1
35 60 10
(a)
Deriv.mass/% min–1

samples at 43, 110 and 150 C 35

50 30 10 8
25
0
Mass/%
Mass/%

6
20
15 4
10 Aged 43 °C- N2
Non aged- N2 Aged 43 °C- air 2
Non aged- air 5
0 0
25 125 225 325 425 525 625 725 25 125 225 325 425 525 625 725
Temperature/°C Temperature/°C

12 115 12
115
Deriv.mass/% min–1
Deriv.mass/% min–1

65 (c) 10 65 (d) 10

15 8 15 8
Mass/%

Mass/%

6 6

4 Aged 150 °C- N2 4

Aged 110 °C- N2
Aged 150 °C- air
Aged 110 °C- air
2 2

0 0
25 125 225 325 425 525 625 725 25 125 225 325 425 525 625 725
Temperature/°C Temperature/°C

123
 R. S. Leonardo et al.

260 25.5 100

240 90
20.5
220 80

% Transmittance
200 15.5

Deriv.mass/% min–1
70
180 10.5
60
160
Mass/%

5.5 50
140
120 0.5 40
100 –4.5 30 Non aged
80 20 Aged 43 °C
Aged 43 °C –9.5 Aged 110 °C
60 10
40 Aged 110 °C –14.5 Aged 150 °C
Non aged 0
20 –19.5 4000 3500 3000 2500 2000 1500 1000 500

0 200 400 600 800 Wavenumber/cm–1

Temperature/°C
Fig. 6 Overlapping of IR spectrum of original and aged biodiesel
Fig. 3 TG/DTG curves of BS100 samples: fresh and aged at 43 and
110 C for 90 days, in N2 place, it can be observed the appearance of the band related
to the stretching frequency of a free O–H bond, near
300
25 3500 cm-1, which intensity is higher when the sample is
270
20 submitted to more severe aging conditions. This indicates

Deriv.mass/% min–1
240
210
15 that the BS100 decomposition can form compounds such as
10 acids, alcohols and aldehydes, an evidence of biodiesel
Mass/%

180
150 5 degradation process.
120 0 The presence of other carbonyl-containing products in
90
Aged 43 °C (90days)
–5 their structure other than the esters constituting the bio-
60 Aged 150 °C (2 days) –10 diesel can be confirmed by analyzing the C=O stretch band.
Non aged
30
–15 The carbonyl stretching band (C=O) presents in the non-
0 200 400 600 800 aged BS100 spectrum and becomes wider in the aged
Temperature/°C samples as shown in Fig. 7. The C=O stretching band
overlapping obtained from the all samples infrared spec-
Fig. 4 TG/DTG curves of BS100 samples: fresh and aged at 43 and
150 C, in N2 trum confirms the presence of other carbonyl-containing
products in their structure, which were formed during the
100 oxidation process. Several studies confirm that the changes
that occur in the region of 3025 cm-1 at 2900 cm-1, and
80
between 1640 and 1850 cm-1 results from elevated
Mass loss/%

60

40

20

0
non aged 43°C 90 days 110°C 90 days 150°C 2 days
Heavy fraction (air) 6,8 36,5 71,3 44,4

Heavy fraction (N2) 3,9 31,2 69,4 42,1

Fig. 5 Quantification of the oxidized biodiesel heavy fractions in air

and nitrogen

under different temperature conditions, it was observed that

the mass of heavy fractions formed at 110 C is twice Non aged
higher than that formed at 43 C. This evidences that the Aged 43 °C
Aged 110 °C
higher is the temperature for a same storage time, the Aged 150 °C
higher is the formation of sediments in the fuel.
Figure 6 shows the overlapping of infrared spectrum of
1885 1740 1595
the fresh biodiesel and aging biodiesel samples. It can be
observed changes in the intensities of the bands in all Wavenumber/cm–1
spectrum regions when aged biodiesel is compared with Fig. 7 Carbonyl stretching band (C=O) for BS100 before and after
fresh BS100. As the biodiesel oxidation process takes aging

123
Evaluation of different aging procedures on biodiesel thermal degradation process

temperatures that accelerate the oxidation process [50, 51].
These changes in the carbonyl band confirm that the above-
mentioned products and of ketones present in biodiesel,
after the aging process [52].
After the aging process, it can be observed changes in
the IV spectrum that occur in the region between
3025 cm-1 at 2850 cm-1. The C–H stretching band at
3009 cm-1, associated with double-bond groups, tends to
disappear in the aged samples, as shown in Fig. 8. The
intensity of the = CH band (3009 cm-1) is related to the
alkyl radical double bonds present in the biodiesel
chemical structure. The biodiesel used in this work was
produced from soybean oil, which has a high content of
polyunsaturated fatty acids (linoleic and linolenic acids) in
its composition. As the sample oxidation proceeds, the IR
absorption bands at 3009 cm-1 tends to disappear and it is
observed the overlapping of the C–H absorption bands at
3150–2800 cm-1 [53]. These facts may be associated with
the formation of gums and sediments resulting from the
oxidation process. This is confirmed by the displacement,
to lower transmittance levels, of the IR spectrum bands, in
the 500–1500 cm-1 region, as shown in Fig. 6.

Fig. 8 IR spectrum of original 100

100
and differently aged BS 100 (a) (b)
biodiesel: CHn stretching bands.
a non-aged biodiesel, b aged at
43 C, c aged at 110 C, d aged 80
at 150 C 80
% Transmittance

% Transmittance
60 60

40 40
3009 cm–1

20 20

0 0
3150 3000 2850 2700 3150 3000 2850 2700
Wavenumber/cm–1 Wavenumber/cm–1

100 100
(c) (d)

80 80
% Transmittance

% Transmittance

60
60

40
40

20
20

0
3150 3000 2850 2700 3150 3000 2850 2700
Wavenumber/cm–1 Wavenumber/cm–1

123

Conclusions
• IR spectra suggest that during the degradation process,
biodiesel is decomposed into aldehydes, acids, ketones
and alcohols, and into heavy fractions, gums and sed-
iments. The resulting IR spectra are complex, which
makes it difficult to quantify the heavier fractions.
• However, the heavy fraction products formed during
biodiesel aging, consisting of gums and sediments, can
be quantified using TG/DTG thermogravimetry.
• This quantification must be obtained from respective
TG/DTG curve data in inert atmosphere, because air
promotes additional oxidation products during analysis.
• The aging temperature of biodiesel is a determining
factor for the degradation rate of the original compo-
nents. Thus, the higher is the temperature for a same
biodiesel storage time, the higher is the mass formed of
oxidation products.
• The previous conclusion also indicates that at higher
temperatures and lower storage times, a similar sedi-
ment mass can be formed, but not necessarily with a
same composition, as was noticed in the present work.
Acknowledgements To the Laboratory of Biodiesel Stability Eval-
uation of the Chemistry School and the Laboratory of instrumentation
and Research—Inorganic Chemistry Department of the Chemistry
Institute, both at Federal University of Rio de Janeiro, Brazil, where,
respectively, TG/DTG experiments and FTIR spectrums were per-
formed by the authors and also to the Brazilian National Council of
Research (CNPq).
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