Chemical Engineering Research and Design 1 6 5 ( 2 0 2 1 ) 172–179

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Chemical Engineering Research and Design

journal homepage: www.elsevier.com/locate/cherd

Effect of moisture content on the extraction rate of

coffee oil from spent coffee grounds using
Norflurane as solvent

Rosa Colucci Cante a , Isidoro Garella b , Marianna Gallo a , Roberto Nigro a,∗
a Department of Chemical Engineering, Material and Industrial Production, University of Naples Federico II, P.
Tecchio, 80, Naples, Italy
b I. T. P. Innovation and Technology Provider S.r.l. Via Bisignano a Chiaia, 68 80121 Naples, Italy

a r t i c l e i n f o a b s t r a c t

Article history: Recently, vegetable oils have been widely used in several industrial fields as food additives,
Received 30 June 2020 biofuels, cosmetic ingredients, packaging materials, or pharmaceutical compounds. In this
Received in revised form 17 study, we investigated the extraction of lipids from spent coffee grounds using an innova-
September 2020 tive system and the hydrofluorocarbon Norflurane, as solvent. Extraction experiments were
Accepted 3 November 2020 performed on matrices at different levels of moisture under a recirculating solvent flow in
Available online 9 November 2020 the pressure range 5−11 bar.
The results confirmed the effectiveness of the novel extraction process on wet, dried and
Keywords: partially dried matrices, and the oil yields and the extraction times (approximately 92% in 75,
Spent coffee grounds 90 and 285 min respectively) were comparable with those obtained using the more expensive
Extraction rate supercritical CO2 process. A kinetic approach was used to model the extraction rates of wet,
Fatty acid profile dry and partially dried samples. It showed that a partial drying of the SCG promoted the
Hydrofluorocarbon solvent solubilization of oil in Norflurane during the first extraction stage and improved the contact
Moisture content between Norflurane and the oily solute.
The fatty acid profiles of the extracts were determined and the results revealed the pres-
ence of palmitic (C 16:0) and linoleic (C 18:2) acids, as major components, and stearic (C 18:0)
and oleic (C 18:1) acids, as minor components.
© 2020 Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.

1. Introduction of these residues, and the environmental effect of their dis-

According to the International Coffee Organization data, the
global coffee production in 2016, was estimated at 150 624 mil-
lion 6̈0 kg bags,̈ which was 1.9% higher than in 2014. Because
of the ever-increasing demand for coffee on the international
market, researcher have focused on the possibility of re-using
and valorising the large quantities of by-products generated
by the coffee industry for energy production, the isolation of
value-added compounds of interest for the cosmetic, pharma-
ceutical, and food industry, the decrease in the toxicity levels
∗
Corresponding author.
E-mail address: rnigro@unina.it (R. Nigro).
https://doi.org/10.1016/j.cherd.2020.11.002
0263-8762/© 2020 Institution of Chemical Engineers. Published by Elsevier B.V. All rights reserved.
posal (Mussatto et al., 2011a). Spent coffee grounds (SCG) and
coffee silverskin, which are generated during the extraction
processes involved in the production of instant coffee and
bean roasting, respectively, are the main coffee industry by-
products.
Approximately 16% of the coffee oil that can be extracted
from the waste SCG generated during beverage prepara-
tion can be converted into biodiesel via transesterification
(Kondamudi et al., 2008; Blinová et al., 2017), and the
exhausted solid can be used as a raw material for the produc-
tion of ethanol (Sendzikiene et al., 2004; Woldesenbet et al.,
2016), fuel pellets (Kondamudi et al., 2008), as potential source
of sugars (Mussatto et al., 2011b), or as adsorbent material
for the removal of metal ions from aqueous solutions (Fiol
 Chemical Engineering Research and Design 1 6 5 ( 2 0 2 1 ) 172–179 173

et al., 2008). Among the main extraction techniques studied

Table 1 – Spent coffee grounds samples with different
for vegetable matrices, cold pressing provides low extraction levels of residual moisture (Xw, g water / g IMC ×100).
yields and the hydrodistillation process could alter the qual-
Sample S1 S2 S3 S4 S5 S6 S7
ity of the extracts by degrading the thermolabile substances
in the extracts (Illes et al., 2000). Furthermore, traditional Xw (%) 100 86 67 47 22 0 62
extraction systems based on maceration or percolation pro-
cesses using organic solvents, such as n-hexane, methanol,
Table 2 – Process conditions during Norflurane
acetone, chloroform, and dichloromethane, provide very high extraction. Xw , Qsol , and t denote the residual moisture,
yields; however, they present high environmental impact, solvent flow rate, and extraction time, respectively.
require expensive safety measures owing to the toxicity and Trial/run# Sample Xw [%] Qsol [mL/min] t [h]
flammability of the solvents, and involve high costs for solvent
separation and purification and for the disposal of the solvent T1 /#1 S1 100 100 5.75
T1 /#2 S6 0 100 2
residues and spent solid.
T2 /#1 S1 100 100 0.5
Supercritical fluid extraction (SFE) is one of the most
T2 /#2 S2 86 100 0.5
popular innovative extraction techniques owing to its high T2 /#3 S3 67 100 0.5
extractive yields, low environmental impact, and great process T2 /#4 S4 47 100 0.5
selectivity, ensured by the possibility of adjusting the pressure T2 /#5 S5 22 100 0.5
and temperature and selecting suitable co-solvents. T2 /#6 S6 0 100 0.5
CO2 is the most commonly used solvent for SFE owing to its T3 /#1 S7 62 100 1.75

relatively low critical pressure and temperature, non-toxicity,

non-flammability, availability at high purity, and low costs. De
Melo et al. (2014), subjected an SCG matrix to SFE and reported
a maximum extraction yield of 80% of the total oil content in
120 min, at 300 bar, 50 ◦ C, and a CO2 flow rate of 10 g/min.
SCG extraction technique using supercritical CO2 (sc-CO2 )
was studied by Couto et al. (2009). Using different operating
temperatures and pressure, the authors obtained a maximum
yield of 19.4 g oil /100 g dry SCG at 50 ◦ C and 200 bar, using ethanol
as co-solvent.
The use of hydrofluorocarbon solvents under subcritical
conditions for the extraction of vegetable oils can be a feasi-
ble alternative to the traditional extraction techniques using
organic solvents and sc-CO2 extraction. Among the hydroflu-
orocarbon solvents, Norflurane (1,1,1,2-tetrafluoroethane),
known as R134a, is one of the main candidates for the extrac-
tion of lipophilic compounds (Abbott et al., 2005; Corr, 2005)
owing its low toxicity, safety, and low operating costs; more-
over, Norflurane is easily liquefiable at relatively low pressures
and can be easily separated from extracts owing to its high
volatility (Babu et al., 2014; Lapkin et al., 2006). Norflurane is
a hydrofluorocarbon refrigerant typically used as propellant
for inhalers and extinguishing agent with a global warming
potential of 1300 and no ozone depleting effects (Lapkin et al.,
2006). Furthermore, Norflurane has been certified as G̈enerally
Recognised As Safeb̈y the Food and Drug Administration and
its use as extracting solvent for several valuable compounds,
such as artemisinin from Artemisia annua (Lapkin et al., 2006),
astaxanthin from Euphausia pacifica (Han et al., 2012), turmeric
and palm oil (Babu et al., 2014; Mustapa et al., 2009), and bil-
berry oil from waste seeds (Colucci Cante et al., 2020) has
already been investigated. In this context, the goal of this
study was to analyse the feasibility of the novel extraction
process developed by Garella (2012) for oil recovery from waste
SCG.
The effect of the SCG moisture content on the extrac-
tion yields and rates was investigated to overcome the
need for a drying pre-treatment of the matrix, which was
deemed indispensable for other extraction techniques, includ-
ing SFE. Moreover, the fatty acid profile of the lipid extract
was determined and simplified kinetic modelling of the
extraction process was conducted to investigate the effect
of the moisture content on the mass transfer mecha-
nisms.
2. Material and methods
2.1. Raw materials and sample preparation
SCG, the waste material from brewing traditional espresso
coffee, was supplied by a local coffee shop in Naples and con-
sisted of 100% Arabica cultivar. The initial moisture content
(IMC) of the SCG was determined by drying the sample for 24
h at 105 ◦ C. The drying trials were performed in triplicate and
the mean IMC value was determined to be 60% (g water /g SCG ×
100).
To assess the effect of the moisture content on the extrac-
tion rates, seven samples (S1 -S7 ) with different levels of
residual moisture (Xw , g water /g IMC × 100) were obtained via
drying SCG at 60 ◦ C in a ventilated stove (Table 1).
The total oil content (OC) of the SCG matrices was deter-
mined by subjecting sample S6 to Soxhlet extraction with 100
mL of n-hexane for 5 h. OC was determined to be 16.6% (g oil /g
SCG ) and this value was used as reference for the extraction
tests with Norflurane.
2.2. Laboratory-scale extraction system
Extraction experiments with Norflurane as solvent were per-
formed using a laboratory-scale system via the patented
process (Garella, 2012) described by Colucci Cante et al. (2020).
Briefly, liquid Norflurane was percolated through the SCG
matrix bed that was placed in an extraction chamber at 8−10
bar to enrich its coffee oil content.
Subsequently the mixture was passed through an expan-
sion vessel where Norflurane was gasified at lower pressure
(approximately 4−5 bar) and the oily solute was released at the
bottom. Afterwards, the clean gaseous Norflurane was recom-
pressed and recycled in liquid form to the extraction chamber,
where the extraction phase was repeated.
2.3. Experimental design
The main process conditions for the extraction experiments
with Norflurane system are summarised in Table 2.
Extraction trials T1 /#1 and T1 /#2 were performed using
samples S1 and S6 , respectively. During each extraction run,
the extract was collected every 15 min, and the cumulative oil
yields and extraction rates were also determined. Extractions
174 Chemical Engineering Research and Design 1 6 5 ( 2 0 2 1 ) 172–179
Table 3 – Lipid extracts subjected to gas chromatography
analysis.
Extract Sample Extraction technique
E1 S6 Soxhlet with n-hexane
E2 S6 Norflurane extraction
E3 S1 Norflurane extraction
T2 /#1-T2 /#6 were performed using samples S1 -S6 , respectively,
with different Xw values, to study the effect of Xw on the
amount of oil extracted during the first 30 min of the extraction
process. Moreover, the cumulative extraction during trial T3 /#1
(1.75 h), which was performed using sample S7 was deter-
mined by collecting and analysing the extracted oil every 30
min.
2.4. Analytical methods
The fatty acid profiles of the extracts reported in Table 3
were determined using a 6890 (Agilent Technologies) gas chro-
matography (GC) system with a Supelco Carbowax 10 column
(length of 30 m, internal diameter of 320 ␮m, thickness of 1
␮m) and a flame ionisation detector.
Helium was used as carrier gas at a flow rate of 1.5 mL/min.
The fatty acids were transesterified by dissolving 15 mg of oil
in 1 mL of hexane and 30 ␮L of a 2 N KOH solution in methanol.
After stirring for 5 min at 20 ◦ C, a solution volume of 1 ␮L was
subjected to GC using the split/splitless method (split ratio of
1:20). The column temperature was initially maintained at 100
◦ C for 2 min to detect the low-boiling substances, then was
increased to 250 ◦ C at a rate of 10 ◦ C/min and maintained for
10 min to separate the high-boiling substances. The injector
and detector temperatures were controlled at 230 and 300 ◦ C,
respectively, and the total run time was 30 min. A standard
sample that contained C4 -C24 saturated and unsaturated fatty
acids was used to determine the fatty acid profile.
2.5. Kinetic modelling
The oil extraction rate was represented using a kinetic model
(Andrich et al., 2001; Ozkal et al., 2005; Kusuma and Mahfud,
2018), which described the unsteady mass transfer as follows:
dme /dt = ks A (ms − m∗s ) , (1)
where me [g] is the mass of oil extracted at time t, ms [g] is
the mass of residual oil in the solid at time t, m∗s [g] is the
mass of oil in the solid that is at equilibrium with the mass
of oil in the solvent phase, ks [m−2 s−1 ] is the kinetic mass
transfer constant, and A [m2 ] is the wetted particle surface.
Assuming that ks · A = k and considering that m∗s was negligible
because the reactor was fed continuously with pure solvent,
Eq. (1) could be rewritten as:
dme /dt = kms , (2)
and ms can be expressed as the difference between the mass
of oil initially present in the sample (ms,0 ) and me , using Eq.
(3):
dme /dt = k (ms,0 − me ) , (3)
Using the separation of variables in Eq. (3) and integrating
the equation for the initial conditions of me =0 g at t = 0 s, we
obtained the following equation:
 ms,o

In = kt. (4)
ms,0 − me
Both me and the extraction yield (o ) were expressed as
functions of time (t), as follows:
 
me = ms,0 1 − e−kt , (5)
and
o = (me /ms,0 ) × 100 = (1 − e−k t × 100, (6)
and k was calculated 
from theslope of the straight line
obtained by plotting ln
ms,o
vs t.
ms,0 −me
This approach was used for modelling the extraction rate
in samples S1 , S6 , and S7 , to offer a preliminary interpretation
on the effect of the moisture content on the oil extraction rate.
2.6. Statistical analysis
The extraction experiments and fatty acid analysis were per-
formed in triplicate. Statistical analysis was performed using
the Microsoft Excel 2016® software. The mean values and stan-
dard deviations (n = 3) were calculated for all experimental
data. The statistical significance of the data was evaluated
using the Student’s t-test, and only the results with p <
0.05 were accepted as significant. Linear regressions of the
experimental data were performed to calculate the kinetic
constants, and the corresponding coefficients of determina-
tion (R2 ) were also determined.
3. Results and discussion
3.1. Extraction results
The extraction yields of oil (␩o , g oil /g OC ) and water (␩w , g
water /g IMC ) of samples S1 and S6 (trials T1 /#1 and T1 /#2 respec-
tively) are illustrated in Fig. 1.
The Student’s t-test revealed that the ␩o and ␩w values of
the S1 and S6 samples were significantly different (p < 0.05). For
sample S6 , ␩o was 97.6 ± 0.37% after 2 h (trial T1 /#2). Further-
more, 74.23 ± 0.51% of the total OC of sample S6 was extracted
within 1 h. A similar ␩o value was reported by De Melo et al.
(2014) who used sc-CO2 for 2 h at higher temperature and pres-
sure (50 ◦ C and 300 bar, respectively) and a CO2 flow rate of 10
g/min.
As illustrated in Fig. 1a, the presence of water in the wet
matrix of sample S1 affected the extraction performance and
led to an ␩o of 96.11 ± 0.51% and an ␩w of 48.27 ± 0.20% after
5.75 h (trial T1 /#1).
Muangrat and Pongsirikul (2019) subjected a dried SCG
sample to sc-CO2 extraction for 3 h at 50 ◦ C and 225 bar and
reported a maximum ␩o of 13.65%. The Norflurane extraction
method used in this study achieved the same ␩o , which corre-
sponded to approximately 82% of the total OC, in under than
1.25 and 2.70 h for the S6 and S1 samples, respectively. Further-
more, Georgieva et al. (2018) subjected a dried SCG sample to
sc-CO2 extraction for 1 h at 40 ◦ C and 400 bar and reported a
␩o of 9%.
 Chemical Engineering Research and Design 1 6 5 ( 2 0 2 1 ) 172–179 175

Fig. 1 – (a) Oil and water extraction yields (␩o and ␩w , respectively) and (b) oil and water extraction rates (–dXo /dt and
–dXw /dt, respectively) as functions of the residual oil content (OC) (Xo , g oil /g OC × 100) of samples S1 (Xw = 100%), and S6 (Xw
= 0%) during trials T1 /#1 and T1 /#2. All reported results are the mean values of three measurements, and the significant
differences were determined using the Student’s t-test (p < 0.05).

Similar results were obtained using the Norflurane extrac-

tion method (approximately 54% of total OC) for the S6 and S1
samples in under 45 and 75 min, respectively. Moreover, the
differences in the extraction performances owing to the effect
of the moisture content on the extraction process were con-
firmed by the extraction rates of oil and water (–dXo /dt and
–dXw /dt, respectively) reported in Fig. 1
The oil extraction rate for sample S1 (trial T1 /#1) first
increased and then remained constant for up to 135 min; con-
versely, the oil extraction rate was almost constant for sample
S6 (trial T1 /#2) during the first 45 min of extraction (Fig. 1b).
During the first phase of the extraction process, more oil
was available on the outer surface of the solid particles and the
Fig. 2 – Dependence of the fraction of oil extracted after 30
extraction process was governed by the external mass transfer
min (Yo , g oil /g dry SCG ×100) on the residual moisture
of the oily solute that was solubilised in liquid Norflurane.
content (Xw , g water /g IMC ×100) of samples S1 (Xw = 100%),
Conversely, the second phase of the extraction process was
S2 (Xw = 86%), S3 (Xw = 67%), S4 (Xw = 47%), S5 (Xw = 22%),
controlled by the diffusive transfer of oil or the oil dispersed
and S6 (Xw = 0%) during trials T2 /#1-T2 /#6. All results are
in water, which dissolved in the solvent, moved through the
reported as mean values ± standard deviations (n = 3).
internal pores of the SCG matrix, suffered an internal resis-
tance to mass transfer, and led to the decrease in the oil
extraction rate for both samples.
Moreover, the water extraction rate remained constant The ␩o values of samples S1 and S6 during extraction, were
throughout the extraction process. The changes in the frac- compared with that of sample S7 , which presented an Xw value
tion of oil extracted during the first 30 min of the extraction that was lower than the aforementioned critical value of 67%
process (Yo , g oil /g dry SCG ×100) with Xw (trials T2 /#1-T2 /#6) are (Fig. 3a).
presented in Fig. 2. The dependence of the oil extraction rate on Xo during the
Our results revealed that Yo increased as Xw in the matrix extraction process is depicted in Fig. 3b.
was decreased to approximately 67% and remained practically The Student’s t-test confirmed that the results obtained for
constant for lower Xw values. trials T1 /#1, T1 /#2, and T3 /#1 were significantly different (p <
0.05).
176 Chemical Engineering Research and Design 1 6 5 ( 2 0 2 1 ) 172–179

Fig. 3 – (a) Time evolution of the extraction yields (␩o ) and (b) dependence of the oil extraction rate (−dXo /dt) on the residual
oil content (OC) (Xo , g oil /g OC × 100) of samples S1 (Xw = 100%), S6 (Xw = 0%), and S7 (Xw = 62%) during trials T1 /#1, T1 /#2,
and T3 /#1, respectively. All results are reported as mean values of three measurements and the significant differences were
determined using the Student’s t-test (p < 0.05).

The ␩o values of sample S7 were higher than those of sam-

ples S1 and S6 (Fig. 3a), which confirmed that an initial partial
drying of the SCG could increase the efficiency of the extrac-
tion process. Therefore, the extraction rate of sample S7 was
higher than those of samples S1 and S6 (Fig. 3b), which indi-
cated that the higher oil concentration in the residual water
contained in the porous structure of sample S7 resulted in an
increased amount of lipid fraction extracted simultaneously
with water. Mabona et al. (2018) and Efthymiopoulos et al.
(2019), studied the effect of moisture content on oil extrac-
tion from SCG, using polar and non-polar solvents by Soxhlet
technology. Fig. 4 – Oil mass-to-water mass ratio (OWR, g oil /g water ) as
In particular, Mabona et al. (2018) reported that the high- function of the residual oil content (OC) (Xo , g oil /g OC × 100)
est yields were obtained using ethanol on SCG samples at of samples S1 (Xw = 100%), and S7 (Xw = 62%) during trials
moisture content of 40% (g water /g SCG ×100) while no oil was T1 /#1 and T3 /#1.
extracted at higher water concentrations, as the water sur-
rounding wet SCG could have limited the solvent penetration solubility of the lipid fraction in Norflurane being higher than
into the matrix. that of water (Abbott and Eardley, 1998; Jackson et al., 1995).
The changes in the oil mass-to-water mass ratio (OWR), The extraction yield and rate of sample S7 were higher than
which was defined as the ratio of the masses of oil and water those of sample S6 (Fig. 3), and these results were attributed to
extracted, with Xo during trials T1 /#1 and T3 /#1 are presented the plasticising effect of water on the porous structure of the
in Fig. 4. SCG sample S7 (Matveev et al., 2000).
The OWR values during the extraction of sample S7 (trial Conversely, the drying process in the sample S6 led to the
T3 /#1) were higher than those obtained during the extraction shrinking of the porous structure, which hindered the pene-
of sample S1 (trial T1 /#1). During the simultaneous extraction tration of Norflurane into the structure, and therefore slowed
of oil and water from sample S7 , the solvent was able to extract the extraction of the oily fraction compared to sample S7 .
more oil than it did from sample S1 , owing to the greater avail- Moreover, the plasticising effect of water appeared negligible
ability of oil in the oil/water emulsion in sample S7 and the in the completely wet sample S1 , where the resistance to the
 Chemical Engineering Research and Design 1 6 5 ( 2 0 2 1 ) 172–179 177

owing to the drying treatment might have hindered the oil

Table 4 – Kinetic constants (k1 and k2 ) of extraction trials
T1 /#1, T1 /#2, and T3 /#1. Here SCG denotes spent coffee
grounds.
Trial/run# SCG sample k1 [s−1 ] R2 k2 [s−1 ] R2
T1 /#1 S1 0.012 0.971 0.007 0.954
T1 /#2 S6 0.018 0.978 0.042 0.986
T3 /#1 S7 0.030 0.950 0.040 0.988
external mass transport owing to the high-water content was
dominant.
3.2. Kinetic constants
Two extraction trends can be distinguished in the extraction
curves in Fig. 3, and each trend was associated with a different
mass transfer mechanism. The kinetic constants, k1 and k2 ,
for both extraction phases, were calculated for trials T1 /#1,
T1 /#2, and T3 /#1, and the data reported in Table 4 confirmed
the aforementioned hypothesis on the key role of the moisture
content on the extraction performance.
The kinetic constants for trial T1 /#1 were lower than those
for trials T1 /#2 and T3 /#1.
The presence of water in the SCG samples slowed the
extraction rates during both extraction steps, because water
competed with the free oil for solubilisation in Norflurane
and/or interfered with the diffusion of oil into the porous
structure of the SCG matrix.
The absence of water from sample S6 and removal of a frac-
tion of the water from sample S7 increased the availability of
the oil in the inner layers of the solid particles, as indicated by
the k2 values calculated for trials T1 /#2 and T3 /#1, which were
higher than that calculated for trial T1 /#1. Furthermore, the
highest k1 value was obtained for trial T3 /#1, which indicated
that during the first extraction stage of this trial, in which the
moisture content was only partially reduced and the concen-
tration of the dispersed oil in the residual water was high, the
extraction rate was also the highest of all analysed trials.
Moreover, the solubility of water in Norflurane is limited,
and water tends to form a film on the surface of SCG, which
hinders the diffusion of solutes in Norflurane (Han et al., 2012).
Therefore, the partial drying of the SCG led to the removal
of the free water from the outer surface of the SCG particles
and promoted the solubilisation of oil in Norflurane during the
first extraction stage. Moreover, the swelling of the SCG matrix
owing to the presence of residual water in sample S7 improved
the contact between Norflurane and the oily solute and led to
the extraction rate of sample S7 being higher than that of sam-
ple S6 (trial T1 /#2), where the shrinkage of the matrix structure
transfer during the first stage of the extraction process.
3.3. Fatty acid profiles of SCG samples
Table 5 presents the fatty acids profiles of the SCG samples
extracted with n-hexane (E1 ) and Norflurane (E2 and E3 , sam-
ples S6 and S1 , respectively).
The major (palmitic (C 16:0) and linoleic (C 18:2)) and minor
(stearic (C 18:0) and oleic (C 18:1)) fatty acids in the three
analysed extracts were quite similar and the polyunsaturated-
to-saturated fatty acid ratio was approximately 1.01–1.22.
However, statistical analysis showed that palmitic and
linoleic acid concentrations were significantly different in all
the analysed extracts, E1 , E2 , and E3 . Stearic acid significantly
decreased in the Norflurane extract E2 (from sample S6 ) while
a statistically significant increase of oleic acid concentration
was found in both extracts E2 and E3 when compared with E1 ,
obtained with n-hexane.
Moreover, these fatty acid profiles were comparable with
those of the sc-CO2 extracted samples reported by De Melo
et al. (2014) and Muangrat and Pongsirikul (2019).
4. Conclusions
Extractions of SCG were performed to test the feasibility of
the novel extraction process developed by Garella (2012), who
used Norflurane as solvent.
It was demonstrated that the Norflurane extraction
method could be competitive with other extraction tech-
niques, such as sc-CO2 extraction, owing to the low pressure
and temperature required, non-toxicity and non-flammability
of Norflurane, low environmental impact of the system, and
extraction yields achieved. Moreover, the low solubility of the
lipid fractions in Norflurane was compensated by the contin-
uous regeneration and recirculation of the liquid solvent.
The effect of the moisture content on the oil extraction
yields and rates was evaluated for dried, wet, and partially
dried SCG samples. Although the presence of water in SCG
affected the extraction rates, the results were still comparable
with those obtained using sc-CO2 extraction (Georgieva et al.,
2018; Muangrat and Pongsirikul, 2019).
The time evolution of the oil yield for a partially dried
SCG sample with a residual moisture content of 62% (g water /g
IMC ×100) confirmed that even an initial partial drying of the
SCG could improve the efficiency of the oil extraction process,
allowing to overcome the need for a total drying pre-treatment
of the matrix, which was deemed indispensable for other
extraction techniques, including SFE.

Table 5 – Fatty acids compositions of the extracts obtained via Soxhlet extraction with n-hexane (E1 ) and the Norflurane
extraction of samples S1 and S6 (E3 and E2, respectively).
Composition (%) Extract E1 Extract E2 Extract E3

C 16:0 (Palmitic acid) 36.98 ± 0.13a 34.96 ± 0.09b 32.86 ± 0.15c

C 18:0 (Stearic acid) 7.76 ± 0.01a 6.9 ± 0.09b 7.49 ± 0.12a
C 18:1 (Oleic acid) 8.32 ± 0.09a 8.69 ± 0.12b 8.63 ± 0.09b
C 18:2 (Linoleic acid) 40.11 ± 0.14a 44.78 ± 0.16b 45.35 ± 0.1c
C 18:3 (Linolenic acid) 1.06 ± 0.09a 1.65 ± 0.01b 1.42 ± 0.1b
C 20:0 (Arachidic acid) 2.28 ± 0.11ab 2.04 ± 0.08a 2.46 ± 0.1b
C 22:0 (Behenic acid) 1.81 ± 0.08a 0.96 ± 0.08b 0.49 ± 0.08c
Polyunsaturated/saturated 1.01 ± 0.01a 1.22 ± 0.01b 1.28 ± 0.00c

The values marked with the same lowercase letters in the same row are not significantly different (p > 0.05).
178 Chemical Engineering Research and Design 1 6 5 ( 2 0 2 1 ) 172–179
This result was also confirmed via the kinetic modelling
of the experimental data, which revealed the important role
of the water content of the SCG samples in the oil transfer
mechanisms involved in the extraction process.
The fatty acid profiles of the SCG extracts obtained using n-
hexane and Norflurane (on wet and dried samples) indicated
that palmitic (C 16:0) and linoleic (C 18:2) fatty acids were the
major components of the extracts and the polyunsaturated-
to-saturated fatty acid ratio was approximately 1.01–1.22.
Although the fatty acid values changed little, statistically,
some compounds either increased or decreased with drying
compared to Soxhlet treatment and a future purpose will be
to investigate the related causes.
Contributions
Roberto Nigro and Isidoro Garella designed the research
project;
Rosa Colucci Cante, Marianna Gallo, and Isidoro Garella
performed the experiments and collected and analysed the
data; and Rosa Colucci Cante wrote the paper.
Roberto Nigro holds primary responsibility for the final
content of the manuscript.
All authors have read and approved the final manuscript.
The paper was edited by Elsevier Language Editing Services.
Funding
This research did not receive any specific grant from funding
agencies in the public, commercial, or not-for-profit sectors.
Declaration of interests
The authors declare that they have no known competing
financial interests or personal relationships that could have
appeared to influence the work reported in this paper.
Declaration of Competing Interest
The authors report no declarations of interest.
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