J Am Oil Chem Soc (2018) 95: 371–382

DOI 10.1002/aocs.12021

ORIGINAL ARTICLE

Processing Parameters on the Extraction of Olive Pomace Oil

and Its Bioactive Compounds: A Kinetic and Thermodynamic
Study
Sofia Chanioti1 · Constantina Tzia1

Received: 27 July 2017 / Revised: 13 November 2017 / Accepted: 13 November 2017

© 2018 AOCS

Abstract The effect of temperature (40–60
C), solid/liq- Nomenclature

uid ratio (1/4–1/12 g mL−1), and agitation speed Symbols
(AS) (100–800 rpm) on the extraction yield of olive pom- A surface area for mass transfer pro-
ace oil and on the recovery of its unsaponifiable matter cess (m2)
(USM) during extraction were studied. Two kinetic models calci calculated values of the oil yield or unsa-
were tested to correlate the experimental data; the first pro- ponifiable matter (USM) by the afore-
posed by So and Macdonald and the second by Sulaiman mentioned process simulation
et al. The two models adequately describe the extraction Ce concentration of the oil or USM in the
process of both oil and USM. Higher extraction tempera- solution at equilibrium (g m−3)
tures, solid to liquid ratios, and AS led to increased oil Ct concentration of the oil or USM in the
yield and favored USM in the extracted oil, and also solution at time t (g m−3)
increased the calculated mass transfer coefficients of the dWt/dt rate of mass transfer of oil or USM
extraction. Changes in enthalpy and entropy were found to (g min−1)
be positive while change in free energy was negative, indi- expi experimental values of the oil yield or
cating that the process was endothermic, irreversible, and USM directly measured at certain pro-
spontaneous. Under equilibrium conditions, the oil yield cessing times
was increased by a factor of approximately 1.096 and k mass transfer coefficient (m min−1)
1.054 for the model of So and Macdonald and Sulaiman kw mass transfer coefficient for the washing
et al., respectively, for every 10
C rise in temperature. mechanism (min−1)
kd mass transfer coefficients for the diffu-
Keywords Olive pomace  Unsaponifiable matter  sion mechanism (min−1)
Solid–liquid extraction  Kinetics  Thermodynamic kα volumetric mass transfer coefficient (min−1)
parameters K distribution coefficient
R gas constant (8.314 × 10−3 kJ mol−1 K−1)
J Am Oil Chem Soc (2018) 95: 371–382. T absolute temperature (K)
t time (min)
V volume of solution (m3)
We mass of olive pomace oil or USM at
equilibrium (g)
Wt mass of the olive pomace oil or USM at
* Constantina Tzia any time (g)
tzia@chemeng.ntua.gr Ye yield of oil or USM at the equilibrium
1
Laboratory of Food Chemistry and Technology, School of
condition (%)
Chemical Engineering, National Technical University of Athens,
9 Iroon Polytechniou St, 15780 Zografou, Greece

J Am Oil Chem Soc (2018) 95: 371–382

372
Yew hypothetical yield of oil or USM at equi-
librium due to washing mechanism (%)
Yed hypothetical yield of oil or USM at equi-
librium due to diffusion mechanism (%)
Ye0 olive pomace oil yield at T = 0
C (%)
Yt yield of oil or USM at any time (%)
Ye solid amount of unextracted oil remained in
the solid residue at T (K)
Ye miscella equilibrium oil yield at temperature
T (K)
ΔH enthalpy change (kJ mol−1)
ΔS entropy change (J mol−1 K−1)
ΔG Gibbs free energy change (kJ mol−1)
Greek symbols
γ temperature coefficient
Sub- and superscripts
d diffusion mechanism
e equilibrium
t time
w washing mechanism
Introduction
Over the last few decades, the production process of olive
oil has rapidly undergone changes including olive pomace
extraction. In the past, mechanical pressing had been com-
monly used in olive oil production, though it was replaced
by the continuous centrifugation process, performed
through a three-phase and later a two-phase system
(Rodríguez-Gutiérrez, Lama-Muñoz, Ruiz-Méndez, Rubio-
Senent, & Fernández-Bolaños, 2012). Oil production, inde-
pendently of the applied process, generates a semidry solid
residue called “olive cake” or “olive pomace residue”
(Amarni & Kadi, 2010; Caputo, Scacchia, & Pelagagge,
2003). Olive pomace can reach up to 30% of olive mill
manufacturing process (Chanioti, Siamandoura, & Tzia,
2016). This residue consists of pulp fragments (21–33%,
w/w), pit (42–54%, w/w), olive fruit skin (10–11%, w/w),
and variable moisture content depending on the extraction
system (25–30%, 45%, and 70%, w/w, dry basis for mechan-
ical pressing, three-phase and two-phase centrifugal sys-
tems, respectively) (Sanchez Moral & Ruiz Mendez, 2006;
Uribe et al., 2012). Its oil content may exceed 8–12%, w/w;
thus oil can be recovered and used for consumption after
refining. Olive pomace residue can also be valorized
through utilization of its valuable bioactive substances.
Olive oil production represents an important economic and
social industrial activity for Greece, as the annual olive oil
output comes to 300,000 tones (International Olive Oil
J Am Oil Chem Soc
Council, 2012); thus, olive pomace extraction is of outmost
significance.
Compared to other vegetable oils, olive oil has a signifi-
cant nutritional value due to the abundance of the monoun-
saturated fatty acid, oleic acid, ranging from 56 to 84% of
the total contained fatty acids. In addition, the individual
compounds of olive oil’s unsaponifiable fraction contribute
to its stability and provide a particular flavor character
(Murkovic, Lechner, Pietzka, Bratacos, & Katzogiannos,
2004). Olive pomace oil displays many similarities to olive
oil; both oils are derived from olives; the olive oil by
mechanical process (pressing or centrifugation, without sol-
vent usage) while the olive pomace oil by solvent extrac-
tion. Although these oils may not significantly differ from
their fatty acid profile, olive pomace oil has higher unsapo-
nifiable matter (USM) content than olive oil. Therefore, the
sustainable recovery of the USM is considered important
for industrial applications (Moghaddam et al., 2012). Now-
adays, high interest has been shown in the study of minor
compounds which generally constitute the USM,
i.e., sterols, fatty alcohols, tocopherols, triterpene alcohols,
and squalene. These compounds bear important bioactive,
nutritional, and characteristic compositional properties.
Additionally, they are recommended for their functional
properties, i.e., anti-inflammatory, antibacterial, antifungal,
antiulcerative, and antitumoral activities (Czaplicki, Ogro-
dowska, Derewiaka, Tanska, & Zadernowski, 2011;
Temime et al., 2008).
Solvent extraction is the most widely applied technique
for extracting oil from oilseed. Hexane is often used for
vegetable oil extraction by solvent extraction industries,
mainly due to its efficient dissolving ability and ease of
recovery and reuse. The scope of the kinetic modeling is to
determine the parameters that are affected by the process
variables, such as temperature, solid/liquid ratio, agitation
speed (AS), and particle size of solid, in order to estimate
mathematically the total extraction evolution and to evalu-
ate the cost for its viability and applicability on an indus-
trial scale. Numerous theories have been proposed to
explain the mechanism of oil recovery by solvent from
ground and flaked oilseeds or oilseed cake residues
(Amarante, Oliveira, Schwantes, & Morón-Villarreyes,
2014; Amarni & Kadi, 2010; Baümler, Crapiste, & Carelli,
2010; Dagostin, Carpiné, & Corazza, 2015; Fernandez,
Perez, Crapiste, & Nolasco, 2012; Kostic et al., 2014;
Meziane & Kadi, 2008; So & Macdonald, 1986; Sulaiman,
Aziz, & Aroua, 2013; Toda, Sawada, & Rodrigues, 2016).
According to these theories, the performance of an extrac-
tion process is governed by both mass transfer and thermo-
dynamic equilibrium phenomena (Baümler et al., 2010;
Chanioti, Liadakis, & Tzia, 2014; Fernandez et al., 2012).
Temperature is primarily an important factor that should be
taken into account during oil extraction process. Higher
J Am Oil Chem Soc (2018) 95: 371–382
J Am Oil Chem Soc
temperature promotes elevated extraction yields. At high
temperatures, the solvent efficiency increases because of a
decrease in viscosity and surface tension, enhancing solubi-
lization, and improving matrix wetting and penetration.
There are three main steps that occur during the solvent
extraction process: (1) penetration or diffusion of the sol-
vent into the pores of the solid matrix, (2) dissolution of the
solvent into the solute and transport of the latter to the sur-
face of the solid matrix, and (3) migration of the extracted
solute from the external surface of the solid material into
the bulk solution (Aguilera, 2003).
Until now, most studies have focused on oil extraction
kinetics without considering the extraction kinetics of minor
components, such as of USM. Several works studying the
extraction of the minor undesirable compounds from various
feedstocks have been published, such as tocopherols, phos-
pholipids, and waxes extraction from sunflower collets
(Baümler et al., 2010) and canola seeds (Fernandez et al.,
2012); free fatty acids from soybean collets (Toda et al.,
2016); and gossypol from cottonseed (Saxena, Sharma, &
Sambi, 2011). However, no emphasis has been put on the
kinetics of olive pomace oil extraction and no studies on
kinetics of its minor useful component extraction can be
found in the literature. Thus, the knowledge of the extraction
rate of the USM under determined conditions of tempera-
ture, solid/liquid ratio, and AS can allow the production of
olive pomace oils enriched in bioactive compounds.
The aim of this work was to determine the kinetics and
thermodynamic parameters of the olive pomace oil extrac-
tion and of USM from olive pomace using hexane as sol-
vent at three different temperatures, solid/liquid ratio, and
AS levels. Mathematical models suggested by So and Mac-
donald (1986) and Sulaiman et al. (2013) were used to
describe the experimental data.
Materials and Methods
Raw Materials
Olive pomace was obtained as a by-product of mechanical
extraction of olives by a local olive oil mill equipped with
a continuous three-phase centrifugation system. The raw
olive pomace was subjected to proper treatment in order to
avoid oil deterioration and to facilitate the extraction pro-
cess. Thus, the olive pomace was air dried by an airstream
oven (35
C for 24 hours) to remove the majority of mois-
ture and was ground by a cutting mill (Pulverisette
15, FRITSCH, Idar-Oberstein, Germany). The processed
olive pomace was also subjected to granulometric analysis
of the solid particles using a set of standard sieves. The
ground olive pomace was analyzed in terms of moisture
and lipids (AOCS, 1998). All experimental determinations
J Am Oil Chem Soc (2018) 95: 371–382
373
were obtained in triplicate. Hexane used as solvent was
reagent grade (Merck, Darmstadt, Germany).
Extraction of Olive Pomace Oil Experiments
The ground olive pomace (20 g) and a volume of n-hexane
(solid/liquid ratio of 1:4, 1:8, or 1:12 g mL−1) were added
to an Erlenmeyer flask (250 mL) fitted to a reflux column.
The flask was placed in a thermostatically controlled bath
at temperature of 40, 50, or 60
C and for specific time
span (0–60 min). In order to agitate the mixture, a magnetic
stirrer was used at the specified AS of 100, 400, or
800 rpm. At the end of each experiment, the exhausted
solid was separated by filtration through Whatman
No. 42 filter paper and the miscella was collected. The
recovered miscella was vacuum distilled at 50
C by means
of a rotary evaporator (BUCHI 461; Buchi Laboratotiums
Tchnik AG, Flawil, Switzerland) and hexane traces were
removed by a nitrogen stream. The amount of extracted oil
was weighed (precision: 10−1 mg). Results obtained were
expressed as described hereinafter:
oil collected ðgÞ
Y ð% Þ = × 100% ð1Þ
mass of olive pomace ðgÞ
The unsaponifiable fraction of the oil was determined
using diethylether according to AOCS Official Method Ca
6b-53 and expressed in oil weight percent (AOCS, 1998).
Kinetic Models
The two major mathematical models, the first suggested by
So and Macdonald (1986) and the second proposed by
Sulaiman et al. (2013), were comparatively used to describe
the experimental data on the kinetics of extraction of the
olive pomace oil and USM. The parameters of both models
were determined by using the nonlinear regression proce-
dure in Sigma Plot (Version 10 SYSTAT; Point Richmond,
CA, USA).
Model of So and Macdonald (1986)
The model proposed by So and Macdonald (So & Macdon-
ald, 1986) comprises a modification of the model suggested
by Patricelli, Assogna, Casalaina, Emmi, and Sodini (1979)
and takes into account two extraction mechanisms, that is
the washing of the oil on the surface of the solid at the
beginning of the oil extraction process and the extraction of
the oil that remains in the cells by diffusion process.
In this way, the oil yield at any time (t) can be described
by the following equation:



Yt = Yew 1 −e − kw t + Yed 1 −e − kd t ð2Þ
374 J Am Oil Chem Soc
h i
where Yt is the oil yield at any time; Yew and Yed are the YC = YCS 1 −e − ð kL αÞt ð8Þ
hypothetical oil yields at equilibrium due to washing and
diffusion mechanisms, respectively; kw and kd are the mass where Ye is the yield of oil or USM at the equilibrium
transfer coefficients for the different extraction mecha- conditions.
nisms (min−1).
The total yield of oil or USM at equilibrium will be Assessment of the Model’s Applicability
Ye = Yew + Yed ð3Þ
The model’s applicability was assessed through the calcula-
where Ye is the yield of oil or USM at the equilibrium con- tion of the average relative deviation (ARD) by using the
ditions and is experimentally obtained. following equation:
n  
100 X 
 expi −calci 
Model of Sulaiman et al. (2013) ARD =  ð9Þ
n i=1 expi 
As extraction process is controlled by diffusion, Sulaiman
where expi represents the experimental values of the oil
et al. (2013) suggested the use of a diffusive model solving
yield or USM directly measured at certain processing
Fick’s law to explain the mass transfer of oil from the solid
times for the batch extraction and calci represents
to the solvent. However, mass flow by diffusion requires
the calculated values by the aforementioned process
knowledge of the concentration gradient inside the parti-
simulation.
cles, which is difficult to determine. At the solid/liquid
interface, mass flow by diffusion is equal to mass flow by
Thermodynamic Parameters
convection. This assumption is in accordance with other
findings (Liauw et al., 2008; Santos, Martins, Caneschi,
The thermodynamic parameters, enthalpy and entropy
Aguilar, & Reis Coimbra, 2015).
change, for the olive pomace extraction were determined
Considering that the mass transfer of oil from the solid
from the van’t Hoff equation:
to the solvent is the main mechanism controlling the extrac-
tion rate and that no reaction between the oil and solvent ΔH ΔS
ln K = − + ð10Þ
takes place, mass transfer rate can be rewritten as follows: RT R
where K is the distribution coefficient, ΔH is the enthalpy
dWt
= kAðCe −Ct Þ ð4Þ change (kJ mol−1), and ΔS is the entropy change
dt
(J mol−1 K−1).
where dWt/dt is the rate of mass transfer of oil (g min−1); The Gibbs free energy change, ΔG (kJ mol−1), for the
k is the mass transfer coefficient (m min−1); A is the surface extraction process is estimated as follows:
area for mass transfer process (m2); Ct and Ce are the con- ΔG = ΔH − TΔS ð11Þ
centrations of the oil in the solution at time t and at equilib-
rium (g m−3), respectively. The distribution coefficient (K) is calculated as follows:
As the extraction was conducted in a batch process and YCS YCS
the volume was constant during the process, Eq. 4 can be K= = ð12Þ
YU Y0 −YCS
written as:
where Ye solid is the amount of unextracted oil remained
dWt A in the solid residue at T (K) and Ye miscella is the equilib-
= k ðWe −Wt Þ ð5Þ
dt V rium oil yield at temperature T (K). The value of Ye solid
dWt was estimated by the deduction of the average total oil
= k α ðWe −Wt Þ ð6Þ content of the olive pomace (8.52%) and the value of
dt
Ye miscella.
where kα is the volumetric mass transfer coeffi-
cient (min−1).
Upon integration, assuming no transport of oil occurs at
time zero, the following equation is obtained: Results and Discussion
h i
Wt = We 1− e − ðk αÞt ð7Þ The olive pomace used in extraction experiments had initial
moisture content of 45.0  0.11% (w/w, dry basis) and of
As yield per mass of solid YC is proportional to WC, the 4.5  0.08% (w/w, dry basis) after drying. After grinding,
following equation can be derived: the olive pomace had mean particle diameter of

J Am Oil Chem Soc (2018) 95: 371–382

J Am Oil Chem Soc 375

(a) 8 (b) 5

4
6

Oil Yield (%)

3

USM %
4

40oC
2 40oC
1 50oC
50oC
60oC
60oC
0 0
0 20 40 60 0 20 40 60
Time (min) Time (min)

Fig. 1 Extraction of olive pomace oil (a) and its USM (b) at different temperatures. Conditions: solid/liquid ratio of 1:4 g mL−1; stirring velocity
of 800 rpm. Points represent average values of experiments, bars stand for SD, and lines correspond to fitting curves obtained from the model of
Sulaiman et al. (dotted line) and the model of So and Macdonald (continuous line)

0.79  0.09 mm, oil content of 8.52  0.08% (w/w, dry
basis), and USM of 4.68  0.05 (w/w, dry basis).
Experimental data of the oil yields obtained from the
olive pomace using hexane as solvent at different tempera-
tures, solid/liquid ratios, and AS are presented in Figs 1a,
2a and 3a, respectively. It is clear from the data shown that
the beginning of the extraction process is dominated by a
washing mechanism. In this stage, hexane solubilizes rap-
idly the olive pomace oil which is available on the surface
of the solid particle and thus the oil yield increases
promptly with time. For example, in the first 10 min of
extraction, a yield of up to 6% (at 60
C in Fig. 1a) is
obtained, a value that corresponds to 73% of final oil yield.
Thereafter, the extraction rate significantly decreases, as the
diffusion becomes the predominant process. This kinetic
behavior has also been verified in studies for the oil extrac-
tion from olive cake (Amarni & Kadi, 2010; Meziane &
Kadi, 2008), sunflower (Baümler et al., 2010; Santos et al.,
2015), canola (Fernandez et al., 2012; Sulaiman et al.,
2013), neem (Patricelli et al., 1979), Jatropha (Liauw et al.,
2008), coconut (So & Macdonald, 1986), castor cake
(Amarante et al., 2014), soybean collets (Dagostin et al.,
2015; Toda et al., 2016), and also for polyphenols extrac-
tion from grape seeds (Guerrero, Torres, & Nuñez, 2008;
Tao, Zhang, & Sun, 2014) and berries (Cacace &
Mazza, 2003).
Effect of Extraction Temperature
The effect of temperature on the extraction process was stud-
ied from 40 to 60
C and the results are shown in Fig. 1a. As
expected, the kinetic data obtained show that the amount of
extracted oil increases with temperature. At each temperature
examined, the yield of oil extracted increases rapidly in the
beginning stage of the process that is governed by washing;
however, the rate slows down in the later stage. The final oil
yield changes from 5.88 to 6.56% by increasing the extrac-
tion temperature from 40 to 60
C. The increase in tempera-
ture causes the solubility of the olive pomace oil in hexane
to increase, besides decreasing the viscosity of both oil and

(a) 8 (b) 5

4
6
Oil Yield %

3
USM %

2 1:4 g/mL
1 1:4 g/mL
1:8 g/mL
1:8 g/mL
1:12 g/mL
1:12 g/mL

0 0
0 20 40 60 0 20 40 60
Time (min) Time (min)

Fig. 2 Extraction of olive pomace oil (a) and its USM (b) at different solid/liquid ratios. Conditions: temperature at 50
C; stirring velocity of
800 rpm. Points represent average values of experiments, bars stand for SD, and lines correspond to fitting curves obtained from the model of
Sulaiman et al. (dotted line) and the model of So and Macdonald (continuous line)

J Am Oil Chem Soc (2018) 95: 371–382

376
(a)
8
6
Oil Yield %
4
2 100 rpm
400 rpm
800 rpm
0 0
0 20 40 60
Time (min)
Fig. 3 Extraction of olive pomace oil (a) and its USM (b) at different AS. Conditions: solid/liquid ratio of 1:4 g mL−1; temperature at 50
C.
Points represent average values of experiments, bars stand for SD, and lines correspond to fitting curves obtained from the model of Sulaiman
et al. (dotted line) and the model of So and Macdonald (continuous line)
hexane, favoring the mass transfer rate (Amarante et al.,
2014; Sulaiman et al., 2013; Toda et al., 2016).
Although there is great interest, both from researchers and
industrial technologists, in oil recovering from oilseed by sol-
vent extraction, until now few researchers have investigated
the unsaponifiable components’ recovery. Olive pomace is
rich in such minor compounds with recognized bioactivity
and thus their recovery may be an alternative utilization path.
The kinetics of extraction of USM can be observed in
Fig. 1b. Similarly to what occurred for olive pomace oil
extraction (Fig. 1a), again a first fast extraction stage (washing
step) and a subsequent slower stage (diffusion step) were
observed reaching equilibrium at 20 min. In Fig. 1b, it can be
noted that increasing the temperature also promotes the extrac-
tion of USM. These results are in good agreement with previ-
ously published works on the extraction of minor compounds,
such as free fatty acids in soybean oil (Toda et al., 2016), and
tocopherols and phospholipids in sunflower oil (Baümler
et al., 2010). The final USM changes from 3.05 to 4.47% by
increasing the extraction temperature from 40 to 60
C.
Kinetic Models
The experimental data present in Fig. 1a were used to esti-
mate the parameters of the mathematical models proposed by
So and Macdonald (1986) and Sulaiman et al. (2013). The
above models showed very good fit to the experimental data,
with determination coefficient values varying between 0.993
and 0.997 for the Sulaiman et al. model and between 0.998
and 0.999 for the So and Macdonald model. The latter model
showed lower average relative error values, ranging from
0.66 to 1.42%, while the values for the Sulaiman et al. model
varied between 1.73 and 3.13% (Table 1a, b). Regarding the
USM (Fig. 1b), the So and Macdonald model showed very
good fit to the experimental data, with high values of the
coefficient of determination (0.998 ≤ R2 ≤ 0.999) and low
J Am Oil Chem Soc
(b) 5
4
USM %
2
100 rpm
1 400 rpm
800 rpm
0 20 40 60
Time (min)
values of relative deviations (1.98 ≤ ARD ≤ 3.05) for the
kinetics of USM. However, the Sulaiman et al. model
showed lower values of the coefficient of determination
(0.975 ≤ R2 ≤ 0.994) and higher values of relative deviations
(3.75 ≤ ARD ≤ 5.73) (Table 1a, b).
Table 1a also presents the mass transfer coefficients and
yields at the equilibrium conditions calculated for the extrac-
tion kinetics of olive pomace oil and its USM at different
temperatures, using the So and Macdonald model. Concern-
ing the kinetic parameters of oil extraction (Table 1a), the
predominance of the washing process was proved since the
washing coefficients are, on average, almost 13 times higher
than the corresponding diffusion coefficients. It can also be
seen that higher coefficients could be noted at higher tem-
peratures (50 and 60
C). As reported by Toda et al. (2016)
in experiments of soybean oil extraction using ethanol as
solvent, the higher the extraction temperature the higher the
yields of the extracted soybean oil at equilibrium. Meziane
and Kadi (2008) referred to similar results in a kinetic study
of olive cake extraction using ethanol concluding that
increasing the temperature from 20 to 50
C resulted in an
increased oil yield. As far as the kinetic data in Table 1a are
concerned, USM extraction evolved similarly to that previ-
ously presented for the oil kinetic extraction; higher values
of mass transfer coefficients were observed again in the pre-
dominant washing step of the extraction process of these
minor compounds, calculated on average about eight times
higher than the ones of diffusion process.
Table 1b presents also the mass transfer coefficients and
equilibrium yields performed by the Sulaiman et al. model
for the extraction kinetics of olive pomace oil and its USM,
respectively. According to the kinetic data of the table, the
values of parameters Ye and kα increased with increasing
temperature in the experiments on the kinetics of oil extrac-
tion and on the kinetics of USM. These observations are in
good agreement with the studies previously published by
Sulaiman et al. (2013) and Liauw et al. (2008).
J Am Oil Chem Soc (2018) 95: 371–382
J Am Oil Chem Soc 377

Table 1 Effect of temperature (T) on the parameters of kinetic model of So and Macdonald (1986) (a) and of Sulaiman et al. (2013) (b) for olive
pomace oil and its USM extraction

(a) Model of So and Macdonald (1986)

Substance Process parameter, T ( C) Mass transfer coefficients Yields at equilibriuma R2c ARDd
(min−1)a
kw kd Yew Yed Ye

Olive pomace oil 40 1.24  0.09 0.11  0.06 4.92  0.02 0.49  0.08 5.41  0.10 0.998 1.42
50 2.05  0.07 0.12  0.02 5.49  0.04 0.52  0.03 6.01  0.07 0.999 0.66
60 2.27  0.08 0.21  0.06 5.71  0.05 0.79  0.07 6.50  0.12 0.999 0.67
USM 40 0.78  0.09 0.10  0.01 1.02  0.07 1.97  0.05 2.99  0.12 0.999 1.98
50 1.09  0.02 0.12  0.03 1.80  0.02 1.79  0.03 3.59  0.05 0.998 2.88
60 2.02  0.06 0.24  0.07 1.12  0.07 3.28  0.02 4.40  0.09 0.998 3.05
(b) Model of Sulaiman et al. (2013)
Substance

Process parameter, T ( C) kαb (min−1) Yeb (%) R2c ARDd

Olive pomace oil 40 0.97  0.06 5.59  0.07 0.993 3.04

50 1.83  0.11 5.93  0.04 0.997 1.73
60 1.86  0.03 6.21  0.07 0.993 3.13
USM 40 0.27  0.03 2.84  0.11 0.975 5.73
50 0.34  0.03 3.40  0.08 0.989 4.46
60 0.34  0.02 4.33  0.07 0.994 3.75
a
Estimated values  SD obtained from model-fitting curve of Eq. 2 (Fig. 1).
b
Estimated values  SD obtained from model-fitting curve of Eq. 8 (Fig. 1).
c
Coefficient of determination.
d
ARD calculated according to Eq. 9.

Effect of Solid/Liquid Ratio
The effect of solid/liquid ratio on the extraction process was
studied from 1:4 to 1:12 g mL−1 and the results are shown
in Fig. 2a. Similarly, the fastest transfer of soluble compo-
nents to the solvent at the beginning of the process, fol-
lowed by a transfer rate decrease until it became constant,
corresponding to the maximum extraction yield. The
amount of extracted oil increases with the solid/liquid ratio.
This effect was expected as the concentration gradient that
is the driving force in extraction processes is supposed to be
higher when decreasing the solid/liquid ratio, leading to
higher diffusion and yields (Meziane & Kadi, 2008; Şahin &
Şamli, 2013). The final oil yield changes from 6.03 to
7.12% by decreasing the solid/liquid ratio from 1:4 to
1:12 g mL−1. The kinetics of extraction of USM in respect
to solid/liquid ratios can be observed in Fig. 2b. The final
USM changes from 3.58 to 4.23% by decreasing the solid/
liquid ratio from 1:4 to 1:12 g mL−1. The washing step
through the oil and USM extraction occurs, respectively, in
the first 10 and 20 min of contact between the olive pomace
and the hexane; in particular, the oil yield extraction reached
values from 69 to 82% of the total yield, while the USM
varied from 72 to 85% of the total USM yield. Toda
et al. (2016) reported that in the beginning of the extraction
process (first 10 min) at 60
C using ethanol, the oil yield
represented the 85% of the total yield.
Kinetic Models
According to the data in Table 2a, the mass transfer coeffi-
cients and yields at the equilibrium conditions were calcu-
lated for the extraction kinetics of olive pomace oil and its
USM at different solid/liquid ratios, using the So and Mac-
donald model. The model showed very good fit to the experi-
mental data for the oil extraction (Table 2a), with all the
determination coefficient values to 0.999 and very low
values of relative deviations (0.40 ≤ ARD ≤ 1.12); similarly,
the determination coefficient values for the USM extraction
(Table 2a) varied from 0.996 to 0.998 and almost low values
of relative deviations (2.77 ≤ ARD ≤ 3.13). The kinetic
parameters of oil extraction (Table 2a) verified again the
prevalence of the washing process in relation to the diffusion
process, since the washing coefficients are, on average, about
14 times higher than the diffusion coefficients. Regarding the
USM kinetic data (Table 2a), similarly, the values of mass
transfer coefficients in the washing step were found almost
eight times higher than the ones of diffusion process.
Moreover, as expected the mass transfer coefficients and
extraction yields increased with rising temperature.

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378 J Am Oil Chem Soc

Table 2 Effect of solid/liquid ratio (S/L) on the parameters of kinetic model of So and Macdonald (1986) (a) and of Sulaiman et al. (2013)
(b) for olive pomace oil and its USM extraction

(a) Model of So and Macdonald (1986)

Substance Process parameter, Mass transfer coefficients Yields at equilibriuma R2c ARDd
S/L (g mL−1) (min−1)a
kw kd Yew Yed Ye

Olive pomace oil 1/4 2.22  0.05 0.12  0.08 5.45  0.04 0.46  0.03 5.91  0.07 0.999 0.68
1/8 2.26  0.07 0.20  0.04 5.65  0.04 1.21  0.02 6.86  0.06 0.999 1.12
1/12 2.27  0.07 0.21  0.05 5.60  0.08 1.51  0.01 7.11  0.09 0.999 0.40
USM 1/4 0.76  0.12 0.13  0.04 1.82  0.05 1.71  0.03 3.53  0.08 0.996 2.97
1/8 1.13  0.09 0.13  0.02 1.44  0.07 2.56  0.05 4.00  0.12 0.998 2.77
1/12 1.50  0.06 0.15  0.03 1.48  0.08 2.71  0.08 4.19  0.16 0.996 3.13
(b) Model of Sulaiman et al. (2013)
Substance Process parameter, S/L (g mL−1) kαb (min−1) Yeb (%) R2c ARDd

Olive pomace oil 1/4 1.36  0.08 5.81  0.07 0.997 1.81
1/8 1.68  0.09 6.45  0.10 0.985 4.60
1/12 1.81  0.02 6.89  0.09 0.991 4.40
USM 1/4 0.29  0.04 3.38  0.09 0.991 4.49
1/8 0.31  0.01 3.87  0.11 0.987 5.51
1/12 0.32  0.03 4.03  0.12 0.980 5.63
a
Estimated values  SD obtained from model-fitting curve of Eq. 2 (Fig. 2).
b
Estimated values  SD obtained from model-fitting curve of Eq. 8 (Fig. 2).
c
Coefficient of determination.
d
ARD calculated according to Eq. 9.

Table 2b shows the mass transfer coefficients and equi-
librium yields proposed by the Sulaiman et al. model for
the extraction kinetics of olive pomace oil and its USM,
respectively. This model showed good fit to the experimen-
tal data for the oil extraction (Table 2b), with the determi-
nation coefficient values varying from 0.985 to 0.997 and
low values of relative deviations (1.81 ≤ ARD ≤ 4.60).
Regarding the kinetics of USM extraction (Table 2b), the
values of determination coefficient varied from 0.980 to
0.991 and even higher values of relative deviations than the
ones of the So and Macdonald model (Table 2a)
(4.49 ≤ ARD ≤ 5.63). It can also be observed in Table 2b
that the values of parameters Ye and kα increased with
decreasing solid/liquid ratio in both oil and USM extrac-
tion. The results are in agreement with other researchers
who reported similar effect of solid/liquid ratio on the
extraction yield of oil from pomegranate or of antioxidants
from pomegranate marc (Goula, 2013; Qu, Pan, &
Ma, 2010).
Effect of Agitation Speed (AS)
The effect of AS on the extraction process was studied
from 100 to 800 rpm, the solid/liquid ratio of 1:4, the
temperature of 50
C, and the results for the kinetics of
olive pomace oil and USM extraction are shown in Fig. 3a,
b, respectively. High-speed agitation can cause turbulence
resulting in a high solute mass transfer rate, and therefore
increasing the amount of extracted oil and USM. The
increasing AS increases the diffusion of the solutes to the
bulk of the solution and tends to reduce the boundary layer
resistance. The increase of AS also prevents sedimentation-
thus providing a homogenous solution. On the contrary, at
low speed of 100 rpm, a large portion of seed settled to the
bottom of the flask resulting in low equilibrium yields
(Diphare & Muzenda, 2014; Zhou et al., 2015). As a result,
the final oil yield changes from 5.60 to 6.02% while the
final USM from 2.92 to 3.58% by increasing the solid/liq-
uid ratio from 100 to 800 rpm. The washing step through
the oil yield and USM extraction occurs, respectively, in
the first 5 and 20 min of contact between the olive pomace
and the hexane. During this stage, the oil yield extraction
reached values from 65 to 69% of the total yield, while the
USM yield varied from 60 to 72% of the total USM yield.
Zhou et al. (2015) reported that by increasing the AS from
300 to 1400 rpm, the equilibrium yield and diffusion coef-
ficients of extraction of chrysin from Oroxylum indicum
seeds were also increased.

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J Am Oil Chem Soc 379

Kinetic Models
According to the kinetic data present in Table 3a, the mass
transfer coefficients and yields at the equilibrium conditions
were calculated for the extraction kinetics of olive pomace
oil and USM at different AS, using the So and Macdonald
model. This model showed very good fit to the experimental
data for the oil extraction (Table 3a), with the determination
coefficient values varying from 0.996 to 0.999 and low
values of relative deviations (0.66 ≤ ARD ≤ 1.72); simi-
larly, in the USM extraction (Table 3a), the determination
coefficient values varied from 0.996 to 0.998 and almost
low values of relative deviations (2.21 ≤ ARD ≤ 2.91). The
kinetic parameters of oil extraction (Table 3a) proved again
the predominance of the washing stage in relation to the dif-
fusion stage, since the washing coefficients are, on average,
about eight times higher than the diffusion coefficients.
Regarding the USM kinetic data (Table 3a), similarly, the
values of mass transfer coefficients in the washing step were
found to be almost nine times higher than the ones of diffu-
sion process. Moreover, the oil yield obtained with an AS of
800 rpm was slightly increased compared with the one of
400 rpm (Fig. 3a). This indicates that such a change in AS
affects the diffusion coefficients but not the amount of oil
eventually extracted by the washing and diffusion stages.
This observation has also been verified in the oil extraction
from canola (rapeseed) by So and Macdonald (1986).
Table 3b shows the mass transfer coefficients and equi-
librium yields proposed by the Sulaiman et al. model for
the extraction kinetics of olive pomace oil and its USM,
respectively. This model showed good fit to the experimen-
tal data for the oil extraction (Table 3b), with the determi-
nation coefficient values varying from 0.997 to 0.998 and
relatively low values of relative deviations (1.66 ≤
ARD ≤ 2.16). However, in the USM extraction (Table 3b),
the values of determination coefficient varied from 0.981 to
0.985 and even higher values of ARD than the ones of So
and Macdonald model (Table 3a) (4.12 ≤ ARD ≤ 5.53). It
can also be observed in Table 3b that the values of parame-
ters Ye and kα increased with increasing AS in the oil and
USM extraction. The results are in agreement with the report
of Diphare and Muzenda (2014), who reported that the oil
extraction yield from waste lubricating grease increased from
49 to 75% with an increase in AS from 200 to 1200 rpm.
Thermodynamic Parameters
Based on the data of the olive pomace oil yield at equilib-
rium, the thermodynamic parameters (the enthalpy change,
the entropy change, and the Gibbs free energy) of the oil

Table 3 Effect of AS on the parameters of kinetic model of So and Macdonald (1986) (a) and of Sulaiman et al. (2013) (b) for olive pomace oil
and its USM extraction

(a) Model of So and Macdonald (1986)

Substance Process parameter, Mass transfer coefficients Yields at equilibriuma R2c ARDd
AS (rpm) (min−1)a
kw kd Yew Yed Ye

Olive pomace 100 1.05  0.10 0.13  0.09 5.42  0.02 0.24  0.03 5.66  0.05 0.996 1.72
oil 400 1.10  0.06 0.20  0.09 4.75  0.09 1.05  0.08 5.80  0.17 0.998 1.28
800 2.26  0.07 0.21  0.09 5.48  0.04 0.48  0.03 5.96  0.07 0.999 0.66
USM 100 1.25  0.08 0.15  0.02 0.78  0.05 2.08  0.06 2.86  0.11 0.998 2.21
400 1.55  0.05 0.16  0.03 0.81  0.08 2.32  0.07 3.13  0.15 0.996 2.79
800 1.78  0.09 0.18  0.05 1.81  0.04 1.74  0.02 3.55  0.06 0.997 2.91
(b) Model of Sulaiman et al. (2013)
Substance Process parameter, AS (rpm) kαb (min−1) Yeb (%) R2c ARDd

Olive pomace oil 100 0.98  0.05 5.62  0.05 0.996 2.16
400 1.06  0.04 5.79  0.04 0.998 1.66
800 1.83  0.11 5.83  0.04 0.997 1.73
USM 100 0.30  0.02 2.80  0.06 0.982 5.53
400 0.32  0.02 3.12  0.06 0.985 4.12
800 0.34  0.03 3.40  0.08 0.981 4.46
a
Estimated values  SD obtained from model-fitting curve of Eq. 2 (Fig. 3).
b
Estimated values  SD obtained from model-fitting curve of Eq. 8 (Fig. 3).
c
Coefficient of determination.
d
ARD calculated according to Eq. 9.

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380 J Am Oil Chem Soc

Table 4 Thermodynamic parameters for olive pomace oil extraction

Model T (
C) Ye miscella (%) Ye solid (%) Ka ΔHb (kJ mol−1) ΔSb (J mol−1 K−1) ΔGc (kJ mol−1)

So and Macdonald (1986) 40 5.41 3.11 1.74 26.65 89.77 −1.44

50 6.01 2.51 2.39 −2.34
60 6.50 2.02 3.22 −3.24
Sulaiman et al. (2013) 40 5.59 2.93 1.91 14.87 52.88 −1.69
50 5.93 2.59 2.29 −2.21
60 6.21 2.31 2.69 −2.74
a
Estimated values obtained from Eq. 12.
b
Estimated values obtained from Eq. 10 (Fig. 4).
c
Estimated values obtained from Eq. 11.

extraction process were estimated. Table 4 presents the
equilibrium oil yield (Ye miscella), the equilibrium unex-
tracted (residue in the solid particle) oil (YU), the thermody-
namic constant (K) calculated using Eq. 12, and the main
thermodynamic parameters of the olive pomace oil extrac-
tion at different extraction temperatures.
Fig. 4 shows the linear dependence of ln K on 1/T from
the data obtained by the two models (R2 = 0.999 for the So
and Macdonald model and 0.996 for the Sulaiman
et al. model). The values of enthalpy (ΔH) and entropy
(ΔS) obtained from the slope and the intercept of the plot,
respectively, were found be ΔH = 26.65 and 14.87 kJ
mol−1, by So and Macdonald and Sulaiman et al. models,
respectively, and ΔS = 89.77 and 52.88 J mol−1 K−1, by
So and Macdonald and Sulaiman et al. models, respec-
tively. Positive enthalpy indicates that the system should
absorb an amount of energy to enable the olive pomace oil
extraction process, and therefore the extraction process is
endothermic. The oil molecules’ extraction leads to an
increase of system’s entropy while a positive value
1.4
indicates the irreversible character of the process. The same
results have been reported by other researches regarding
extraction of olive cake, soybeans, cottonseeds, Jatropha
curcas, coconut waste, hempseeds, and castor cake
(Amarante et al., 2014; Amin, Hawash, Diwani, & Rafei,
2010; Kostic et al., 2014; Meziane & Kadi, 2008; Rodri-
gues, Aracava, & Abreu, 2010; Saxena et al., 2011; Sulai-
man et al., 2013).
The free energy values were negative and ranged abso-
lutely between 1.44 and 3.24 kJ mol−1. Negative free
energy change means that the olive pomace oil extraction
was feasible and spontaneous. The degree of spontaneity of
the process increases with an increase of the temperature of
the extraction and indicates that the olive pomace oil
extraction was favored at higher temperatures. The results
are in agreement with reported ΔG in other works
(Amarante et al., 2014; Amin et al., 2010; Meziane & Kadi,
2008; Rodrigues et al., 2010).
Temperature Extraction Coefficient

So and Macdonald model The temperature extraction coefficient (γ) indicates the
Sulaiman et al. model
1.2
increase of the extraction of oil from olive pomace for
every 10
C increase in extraction temperature and is
defined as
1.0
Ye = Ye0 γ T=10 ð13Þ
ln K

0.8 where γ is the temperature coefficient, Ye and Ye0 are the

olive pomace oil yields at temperatures T (
C) and 0
C,
0.6 respectively. Fig. 5 presents the dependence of ln Ye on T/
10 (
C). The value of temperature extraction coefficient (γ)
obtained from the slope of the linearized transformation of
0.4
0.00295 0.00300 0.00305 0.00310 0.00315 0.00320 0.00325 Eq. 13 (R2 = 0.995 and R2 = 0.993, by So and Macdonald
1/T (1/K) and Sulaiman et al. model, respectively) was 1.096  0.03
and 1.054  0.01 for So and Macdonald and Sulaiman
et al. model, respectively. It means that the olive pomace
Fig. 4 Dependence of ln K (equilibrium constant) on 1/T (tempera-
ture [K]). Conditions: solid/liquid ratio of 1:4 g mL−1; stirring speed oil yield increased by a factor of about 1.096 or 1.054 for
of 800 rpm (Eq. 10) every 10
C rise in temperature. The value of γ is in

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J Am Oil Chem Soc
1.90
So and Macdonald model
Sulaiman et al. model
1.85
1.80
ln Ye
1.75
1.70
1.65
3.5 4.0 4.5 5.0 5.5
T/10 (oC)
Fig. 5 Dependence of ln Ye on T/10 (Eq. 13)
agreement with the literature for the oil extraction from
hempseed, olive cake, and rubber and melon seeds
(1.01–1.14) (Kostic et al., 2014; Meziane & Kadi, 2008).
Conclusions
In this work, the kinetics of oil extraction from olive pom-
ace and its USM were accomplished at different tempera-
tures (40, 50, and 60
C), solid/liquid ratios (1/4, 1/8, and
1/12 g mL−1), and AS (100, 400, and 800 rpm). It was
proved that the beginning of the extraction process was
dominated by a washing mechanism, where most of the oil
and USM present on the surface of the solid particles were
rapidly extracted, while afterwards the extraction rate
diminished and the process became controlled by the diffu-
sion of the solutes contained inside the particles in the sol-
vent until it reaches the equilibrium conditions. Higher
values of temperature, solid/liquid ratios, and AS favored
the oil and USM extraction yields and consequently the
mass transfer coefficients at various levels. Two mathemati-
cal models were used and showed good performance in
describing the experimental data, resulting in ARD of
1.85% in So and Macdonald’s model and of 3.77% in the
model proposed by Sulaiman et al. Enthalpy and entropy
were positive and free energy was negative, indicating that
the process is endothermic, irreversible, and spontaneous.
Under equilibrium conditions, the yield of oil increased by
a factor of approximately 1.096 and 1.054 for the So and
Macdonald and Sulaiman et al. models, respectively, for
every 10
C rise in temperature. The results of this study
can provide useful information for designing, optimizing,
and scaling up the recovery of USM of olive pomace from
the oil industry.
J Am Oil Chem Soc (2018) 95: 371–382
381
Conflict of interest The authors declare that they have no conflicts
of interest.
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