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Chemical Engineering Science, Vol. 53, No. 21, pp.

3711—3718, 1998
( 1998 Elsevier Science Ltd. All rights reserved
Printed in Great Britain
PII: S0009–2509(98)00150–X 0009—2509/98/$—See front matter

Almond oil extraction by supercritical CO2 :


experiments and modelling
C. Marrone,* M. Poletto,* E. Reverchon*- and A. Stassi‡
* Dipartimento di Ingegneria Chimica e Alimentare, Universita% di Salerno, Via Ponte Don
Melillo, I-84084 Fisciano (SA), Italy;

Dipartimento di Scienze e Tecnologie Alimentari e Microbiologiche, Universita% di Milano,
Via Celoria 2, I-20133 Milano, Italy

(Received 5 January 1998; in revised form 5 May 1998; accepted 18 May 1998)

Abstract—Oil from crushed almond seeds was extracted with supercritical CO at 350 bar and
2
40°C. Almond particles of three different mean sizes were tested. Extraction of the smaller
particles was performed at two different solvent flow rates. Oil yields were obtained with
asymptotic values at large extraction times that were close to the values obtained by Soxhlet
extraction. An extraction model based on the physical evidence of broken and intact oil cells
has been developed. It accounts for a former equilibrium regime and a latter finite mass transfer
regime. All model parameters except the internal mass transfer coefficient and the oil concentra-
tion at solvent saturation have been determined with independent experiments. The model
solution was calculated with a finite difference numerical technique. A good agreement was
obtained between model curves and the experimental data for an internal mass transfer
coefficient of 7.5]10~9m/s. Solute concentration profiles within the extractor were evaluated
with our model. ( 1998 Elsevier Science Ltd. All rights reserved.

Keywords: Supercritical extraction; almond oil; modelling.

INTRODUCTION ration. Bulley et al. (1984), Lee et al. (1986) and Fattori
Supercritical fluid extraction (SFE) of seed oil has et al. (1988) assumed that mass transfer resistance was
been studied by several authors from the processing only in the solvent phase. King and Catchpole (1993)
point of view and a wide range of seed species has used a shrinking core model to describe a variable
been explored: wheat germ (Taniguki et al., 1985), oats external resistance where the solute balance on the
(Fors and Ericksson, 1990), corn germ (Christianson solid phase determines the thickness of the mass
et al., 1984), cottonseed (Stahl et al., 1980; List et al., transfer layer in the external part of the particles.
1984; Snyder et al., 1994), soybean (Stahl et al., 1980; Sovová (1994), Sovová et al. (1994a,b) and Goto et al.
Friedrich and List, 1982; Eggers et al., 1985; Eisen- (1993) considered the solid phase as divided between
bach, 1988; Snyder et al., 1994), evening primrose broken and intact cells. Two separate mass balances
(Favati et al., 1991), jojoba (Stahl et al., 1984), rice were written and different mass transfer resistances in
bran (Ramsay et al., 1991), rapeseed (Eggers et al., the solvent phase for the broken cells and in the solid
1985), peanut (Snyder et al., 1994) and grape seed phase for the intact ones were considered. This model
(Molero Gomez et al., 1994). was based on sound physical hypotheses and repre-
Despite the large number of species processed, only sented the first attempt to introduce a description of
some models of the SFE of seeds have been published. the structure of the vegetable matter by a mathemat-
They all agree with the fact that at least the first part ical model. However, it required several parameters
of the SFE process is governed by the solubility equi- related to physical properties of the seed which were
librium between the oil and the fluid phase. The equi- difficult to be measured or calculated and, therefore,
librium relationship has been generally supposed to were adjusted by the authors to fit the experimental
be linear since more precise information is not avail- results.
able in such complex systems. Many authors simplified the system of partial dif-
From the mathematical point of view, all models ferential equation coming from mass balances in or-
proposed are based on differential mass balance integ- der to obtain an analytical solution. However, Poletto
and Reverchon (1996) proved that this procedure can
significantly modify the model results. The only ex-
-
Corresponding author. Tel.: #[39]089964116; fax: ception are represented by Bulley et al. (1984) and
#[39]089964057; e-mail: reverch@dica.unisa.it. Perrut et al. (1997) that obtained a numerical solution
3711
3712 C. Marrone et al.
of their model using the method of characteristics. section of the plant. In this latter section a rotameter
Therefore, further research activity is required to and a dry test meter were, respectively, used to
develop models that can adequately describe and, measure the instantaneous flow rate and the quantity
possibly, simulate the supercritical extraction of of CO delivered. All lines were electrically heated and
2
vegetable oils. insulated to keep the fluid temperature constant along
The aim of this study was to perform the supercriti- the different sections. Pressures were measured by
cal fluid extraction of almond oil at different mean manometers and temperatures by thermocouples.
particle sizes and solvent flow rates. Then, the model of The extraction bed was made of crushed fresh
broken and intact cells, firstly proposed by Sovová almond seeds. Different degrees of crushing were used
(1994), was applied giving a particular emphasis on the to change the average particle size. Particle size distri-
specification of macroscopic and microscopic charac- butions were measured with a Malvern laser analyser
teristics of almond particles, to obtain a closer repres- for the two finer powders. Sieving was used for the
entation of the vegetable matter and a significant re- coarser sample. The solvent used was CO at 99.95%
2
duction of the adjustable parameters within the model. purity. The extraction pressure and temperature were
350 bar and 40°C in all tests performed. Different
solvent flow rates were also used. A summary of the
EXPERIMENTAL SET UP tested experimental conditions is given in Table 1.
A scheme of the extraction unit used in this work is
given in Fig. 1. The extractor had an internal volume MATHEMATICAL MODELLING
0.2 dm3 (length ¸"160 mm internal diameter
ID"40 mm). A fine aluminum net and a shallow bed General hypotheses
of rashig rings were placed at the extractor bottom as Some hypotheses were made to model the extrac-
a solvent distributor. Carbon dioxide, withdrawn tion system. Most of them are related to the solute
from the cylinder, was pressurized and driven by and the solvent involved in the extraction and are
a diaphragm compressor (Nova Swiss). The pressure common to most of SFE models.
in the extractor was regulated by a Tescom valve
placed between the compressor and the extractor. The (a) Several components are generally involved in
solvent was brought to the extraction temperature by the extraction of a seed oil. However, we sup-
using a heating coil immersed in a thermostated posed that their behavior with respect to the
liquid. Thermostated liquid jackets were also used to mass transfer phenomena is similar and can be
control the extractor and the separators temperatures. described by a single pseudo-component which
A micrometering valve between the extractor and the will be called the ‘solute’.
separator regulated the solvent flow rate. The separ- (b) The commonly accepted continuous description
ator had an internal volume of 0.15 dm3 and was of the extraction bed has been assumed with the
provided with a tangential inlet to enhance the liquid implicit hypothesis that the relevant concentra-
droplet separation. The pressure inside the separator tion gradients in the fluid phase develop at
is controlled by a back pressure regulating valve larger scales than the particle size. The solute
placed between the separator and the atmospheric concentration in the fluid phase depends only

Fig. 1. Experimental apparatus. AS, rotameters; B, CO cylinder; CdF, flow rate counter; DC, diaphragm
2
compressor; E, extractor; H1, solvent heater still; M1, M2 and M3, pressure indicators; P, pressure
dampener; RD, rupture disk; S1, separator; T1, pressure regulator; T2, back pressure regulator; Tc1 and
Tc2, thermocouples; VM, micrometering valve.
Almond oil extraction by supercritical CO 3713
2
Table 1. Experimental conditions

Test condition A B C D

Particle mean Sauter diameter (mm) 0.30 0.70 0.30 1.9


Solvent flow rate (kg h~1) 0.72 1.43 1.43 1.43
Bed mass (kg) 0.160 0.072 0.084 0.072
Bed height (mm) 160 115 115 115
Symbol h v j m

Fig. 2. Scanning electron microscope image of the surface of an almond particle extracted with supercritical
CO . Broken vegetable structures (cells) that contained the free oil phase are clearly evident. Inside the cells
2
it is possible to see the presence of non-extractable starch grains. The mean cell diameter can be estimated
around 20 km.

on time, t, and on the axial coordinate, z. Its that we call cells and contained the almond oil which
value, C, is given in terms of solid mass per unit is freely available for extraction. These cells should
of solvent mass. not be confused with the biological cells, which are
(c) The solvent flow rate, with interstitial velocity u, much smaller and, in fact, are the basis of the veg-
is uniformly distributed in every section of the etable tissue forming the walls of the cavities that, in
extractor. The pressure drop can be neglected as the whole seed, contain oil and starch. Both the oil
well as temperature gradients within the col- and the starch constitute a nutrient reservoir for the
umn. The axial dispersion is negligible. germinating plant. The starch is not extractable and,
(d) The volume fraction of the fluid, e, is not affec- in fact, in Fig. 2 it is possible to see its agglomerates
ted by the reduction of the solid mass during the still present after the extraction. The mean size of
extraction; in other words, the solids do not a cell, d , was measured from Fig. 2 and is approxim-
c
change their volume during the extraction pro- ately equal to 20 km. The biological cells on the cavity
cess. walls can be observed in higher enlargement photos.
In the inner portion of the particles, the remaining
Further hypotheses regard the natural matrix. Such part of the oil is contained inside the closed cells.
kind of hypotheses are not easily exchangeable among Given the different oil condition on the particle sur-
different kinds of matrix and have to be particularized face and inside, it is likely that the mass transfer
to the specific microscopic structure. Figure 2 shows resistance to extract the oil available at the surface is
the surface of an extracted almond particle as it ap- considerably lower than that to extract the remaining
pears by scanning electron microscopy. It shows that part of it. This feature is summarized in the following
the surface is formed by a structure of broken cavities and schematically shown in Fig. 3.
3714 C. Marrone et al.
by the structure of the insoluble solids which is not
affected by the extraction. This can be verified by
Fig. 2, which shows that in the extracted particles the
structure of the insoluble solids is intact, and by the
experimental evidence that the extracted particles are
lighter but not apparently smaller than the untreated
ones. Furthermore, the small value of / (order of
f
magnitude of d /d ) makes negligible the effective e in-
c p
crease due to the reduction of the volume occupied by
the free oil phase during the extraction. Taking into
account that the inclusion of such e and / changes in
a mathematical model would make its resolution con-
Fig. 3. Scheme of the partition of the bed volume in the siderably harder we avoided it, according to hypothe-
different phases used in the model and the corresponding sis (d).
contributions to the solute balance during the extraction.
Mass balance equations
According to the above hypotheses the mass bal-
ance on the solute in the extractor is
(e) The solute in the solid is present in two separate
phases. LC LC
eo #eo u
(f ) One phase includes the oil contained inside the f Lt f Lz
particles (the ‘tied oil’ phase). Besides this oil, it
includes also the non-soluble solids contained LP Lt
#(1!e)/ o #(1!e)/ q "0 (2)
in the seeds and it fills a fraction / of the overall t s Lt f o Lt
t
volume occupied by the seed particles. This
where o is the fluid density, which is supposed to be
value, according to the above hypothesis (d), f
not affected by the presence of the solute, o is the bulk
does not change with time during the extraction s
density of the non-soluble solid that is the mass of
process and, therefore, / is considered to be
t non-soluble solids in the seeds per unit of particle
constant (see further discussion on this point
volume. This is somewhat an unusual definition but,
below). The average tied oil concentration, in
as it will be shown in the following, the corresponding
terms of mass of oil per mass unit of non-soluble
o value can be easily evaluated from experimental
solid, is called P. s
data.
(g) The other phase is made of the oil freely avail-
The mass balance on the phase of the tied oil alone
able on the almond particle surface. The oil
is
concentration here is always the same and, ac-
cording to our hypotheses, it is equal to the LP Ja
pure almond oil density q . "! t (3)
o Lt (1!e)/
(h) The initial fraction of the seed volume filled by t
the free oil is / "1!/ . The volume of each where a is the specific surface of the seed particles and
f t
particle occupied by the free oil is approxim- J is the mass transfer rate between the tied oil phase
t
ately equal to the particle surface multiplied by and the fluid phase. The mass balance on the free oil
the cell radius. Using a spherical geometry and phase alone is
averaging over all the particle sizes, it is:
Lt Ja
q "! f (4)
nd2(d /2) d o Lt (1!e)/
/ " p c "3 c (1) f
f nd3/6 d
p p where J is the mass transfer rate between the free oil
f
where d is the Sauter mean particle diameter phase and the fluid phase per surface unit. In both eqs
p
and d is the cell diameter. (3) and (4) the mass transfer area was put equal to a.
c
(i) The fraction of the seed occupied by the free oil This is not strictly true because fluxes J and J might
f t
during the extraction is t/ where, of course, affect different area partitions of the particle surface.
f
we always have t)1. Our model however is unable to make a distinction
between the effect of a mass transfer area change and
During the extraction both the free oil and the tied oil that of a mass flux J change. For this reason, the mass
move from the seed particles to the solvent. This oil transfer area was conventionally put to a.
flux might reduce the volume occupied by the seed The system of equations (2)—(4) has a unique solu-
particles and probably change the / and / values. In tion when the initial conditions (i.c.) on C, P and
f t t and the boundary condition (b.c.) on C are given:
particular, during the extraction, the volume occupied
by the free oil phase in the untreated particles is filled i.c. CD "C ; PD "P ; tD "t (5)
by the solvent. Nevertheless, we think that the ex- t/0 0 t/0 0 t/0 0
ternal volume of the particle is essentially determined b.c. CD "0. (6)
z/0
Almond oil extraction by supercritical CO 3715
2
Moreover, we supposed that the loading time of the
solvent into the extractor was long enough to enable
the fluid to reach the equilibrium concentration be-
fore the extraction started. Therefore, we have
q "KtC (7)
o 0
where Kt is the equilibrium constant between the
solvent and the free oil phase. This means that before
the extraction starts a part of the solute present in the
seed saturates the fluid. In the absence of specific
experimental findings, we also suppose that there is no
solute flux between the two solid phases before the
extraction starts or, in other words, that the presence
of the solvent does not change the oil equilibrium
between the two solute phases in the solid. This condi-
tion, together with eq. (7), implies that the tied oil
phase and the solvent are at equilibrium at the extrac-
Fig. 4. Extraction yield as a function of time. Symbols are
tion start:
experimental data; continuous lines are model results. Refer
P "K C (8)
0 p 0 to Table 1 for symbol legend.
where K is the equilibrium constant between these
p
two phases. A consequence of this hypothesis is that
the free oil alone participates to the initial saturation
of the solvent. In turn this implies that the free oil
phase is large enough for it to outlast the oil transfer
to the solvent. This condition is necessary for eq. (7) to
apply. Therefore, the volume fraction t of the free oil
0
at the extraction start is different from unity that,
according to our definition, is the value of t in the
untreated seed. The free oil mass balance relates
C and t to the loading of the untreated solid:
0 0
q (1!e)/ "q (1!e)/ t #C o e. (9)
o f o f 0 0 f
Both eqs (7) and (8) are valid under the hypothesis
of a linear equilibrium relationships between the sol-
vent and any of the oil phases. This provides a simpli-
fied view of the system. However, we do not have
more accurate information regarding its thermodyn-
amic behavior to confidently assume more complex
equilibrium models. The main scope here is to cor- Fig. 5. Extraction yield as a function of the dimensionless
rectly express the oil mass balance at the extraction mass of solvent used, m /m . Symbols are experimental data;
s 0
start and during its course. The value of K and continuous lines are model results. Refer to Table 1 for
p symbol legend.
Kt will be calculated in the section ‘Model evaluation
and discussion’ below.
extraction. For extraction yields larger than 10%, the
EXPERIMENTAL RESULTS extraction curves show a considerable spreading sug-
Results of the extraction tests are reported in Fig. 4 gesting the onset of a mass transfer resistance. Indeed,
where the yield, ½, i.e. the quantity of oil extracted in Fig. 4, an increase of particle size increases the
divided by the weight of the initial charge, is given as extraction time as it is expected from a corresponding
a function of the extraction time, t. The same results decrease of the mass transfer rate. For very large
are shown in Fig. 5 where the yield is given as a func- extraction times, we can identify an asymptotic value
tion of the specific mass of solvent used, i.e. the ratio of the yield of about 50% by weight. This value is in
between the mass of CO used and the mass of seeds good agreement with the oil content measured with
2
charged in the extractor. From the comparison be- a Soxhlet extraction with hexane, which gave about
tween the experimental data in Figs 4 and 5 it is 54% of weight fraction of oil and was assumed to be
possible to observe that, during the first part of the the maximum possible yield, ½ .
=
extraction process, the mass of oil extracted is inde-
pendent of both the particle size and the solvent flow
rate. These considerations strongly suggest that the MODEL EVALUATION AND DISCUSSION
thermodynamic equilibrium of the oil between the The initial part of the extraction curves with
solid and the fluid phases applies to this part of the their linear shape strongly suggests that equilibrium
3716 C. Marrone et al.
conditions are attained in the fluid coming out of the the mass transfer between the phases, because part of
extractor. Therefore, the initial oil concentration in it might be hindered by contacts with neighboring
the fluid C can be evaluated from the experimental particles. For this reason, in experimental conditions
0
plot of the oil yield as a function of the mass of solvent B, C and D, the specific particle surface was deter-
flowed, m : mined as if the particles were freely moving:
s

N
m m m m
C " e" e 0"½ s (10) 6(1!e)
0 m m m m a" . (13)
s 0 s 0 d
p
where m is the mass of the extracted oil and m the
e 0 For experimental condition A, a was evaluated with
initial mass of seed. The last term of eq. (10) is the
the hypothesis of a linear variation with bed voidage
slope of the linear section of the yield curve.
starting from the loosely packed configuration:
Our model also requires the values of the bulk
density of the non-soluble solids o and the initial 6(1!e ) e
s a" o . (14)
values P and t . The value of o can be obtained d e
0 0 s p o
from the particle effective density o with a mass
e In particular, e "0.47 was used which is the voidage
balance on the non-soluble solids: o
of the bed C, and was made of particles of the same
o / "o (1!½ ). (11)
s t e = size as those used in experimental condition A, but
Using the value of C obtained from eq. (10), eq. (9) was not compressed.
0
can be used to evaluate t . A mass balance on the free A definite transition between the initial equilibrium
0 regime and the final mass transfer regime can also be
oil allows to evaluate P :
0 observed from experimental results as a sharp vari-
q / #P o / "o ½ . (12)
o f 0 s t e = ation of the slope of the experimental extraction
The equilibrium constants K and K can be cal- curve. It has already been observed in the SFE of
p t flower concretes that this phenomenon is due to the
culated according to eqs (7) and (8).
The set of parameters obtained for the extraction exit of a solute concentration shock from the extractor
experiments is reported in Table 2. The strong de- outlet (Reverchon and Poletto, 1996). In that case, the
pendence of / on the particle diameter is due to eq. concentration shock wave inside the extractor was
f modelled applying a solute mass balance. In this work
(1) used to evaluate it. The consequence is that
/ ("1!/ ) also depends on the particle diameter as mass transfer rates J and J of oil from the two solid
t f
t f
well as the values of o calculated according to phases were modelled with constant mass transfer
s coefficients, k and k , respectively:
eq. (11). A justification for this dependency is to be t f
found in the increasingly larger weight on o of the
s J "k (P!K C)
t t p
(15)
mass of the external insoluble surface of the particle and
for the smaller particles. Changing the particle dia-
J "k (q !K C). (16)
meter, the relative mass of the tied oil with respect to f f o t
the insoluble solids also changes. Therefore, the oil In eq. (15), for the tied phase, the driving force is
mass balance on the particles, eq. (12), produces differ- expressed with the use of the average oil concentra-
ent values of P . tion, P, to account for the reduction of the mass
0
From Table 2 it appears that the bed voidage for transfer rate at longer extraction times. The initial
the test conditions A is much lower than in the other equilibrium regime was simulated by applying very
cases. This is due to a different loading procedure of large values to the mass transfer rates k . The correct-
f
the extractor that, in this case, determined a higher ness of this procedure was verified by changing these
compression of the powders with respect to the nat- values and observing that this was not significant to
urally loose configuration in experimental conditions the model results regarding the extraction kinetic. The
B, C and D. For such compressed conditions, it is set of differential equations (2)—(6) was solved using a
likely that not all the particle surface is available for finite difference method. An implicit Crank—Nicholson

Table 2. Parameter evaluation

Test condition A B C D

e 0.25 0.47 0.47 0.47


a (m~1) 5590 4506 10516 1660
/ 0.07 0.08 0.2 0.03
f
o (kg m~3) 536 540 620 510
s
C 0.011 0.011 0.011 0.011
0
t 0.94 0.87 0.94 0.65
0
P 1.04 1.02 0.81 1.11
0
K 94.7 93.5 73.1 101.7
p
K (kg m~3) 81.8 81.8 81.8 81.8
t
Almond oil extraction by supercritical CO 3717
2
numerical cell was adopted. The proved numerical side and a finite mass transfer region near the inlet.
stability of this cell made the implemented algorithm The sharp concentration change between these two
fairly robust. For some experimental conditions these regions that propagates towards the outlet is evident
model results were compared with those obtained by from the figure. This transition should be a shock
applying the method of characteristics coupled with represented by a vertical line. The slight inclination in
the simulation of the propagation of a concentration the figure is due to the finite number of points of the
shock as it was developed by Reverchon and Poletto grid used for the finite difference analysis.
(1986). No significant differences were detected. More complex extraction models have also been
Since all the values of the other parameters were tested: (1) a simplified shrinking core model with con-
evaluated directly from experimental measurements, stant driving force (P !K C ) and (2) a non-linear
0 p 0
the model developed has only one adjustable para- equilibrium curve with a constant mass transfer rate.
meter: the mass transfer coefficient for the tied oil k . In the former case, model results poorly fitted the
t
Furthermore, since the prevailing resistance for the experimental data. In the latter case the improvement
extraction of the oil from the inner cell of the particle did not justify the use of a more complex relationship
depends on the internal mass transfer, k should be for thermodynamic equilibrium with the introduction
t
independent of the solvent flow rate. Therefore, we of a second adjustable parameter.
looked for a k value that, independently of the par-
t
ticle diameter, provided the best fit between the model CONCLUSIONS
curves and the experimental data. The best value
In the first part of the extraction experiments the
obtained is k "7.5]10~9 m s~1. Model curves ob-
t solvent exits the extractor saturated with the almond
tained using this value of k are shown by continuous
t oil. This period is longer for smaller particles. This
lines in Figs 4 and 5. The general agreement between
extraction feature can be explained by considering
model and experimental data appears fairly good for
two different phases in which the oil can be found
all the conditions tested. In spite of some simplifying
within the seeds: (1) a freely available oil phase con-
hypotheses adopted, the model is able to evaluate
tained within broken cavities (cells) on the surface of
satisfactorily the transition from equilibrium to mass
the crushed particles; and (2) a tied oil phase, either
transfer regime and to carefully follow data points
contained within closed cells inside the particles or
during the mass transfer regime. An important source
somewhat tied to their internal structure.
of error that might justify the difference between
An extraction model considering these two different
model curves and experimental data is the uniform
phases was proved to describe fairly well the whole
diameter hypothesis. Indeed, particle size distribution
extraction process. It is significant that only the mass
might provide larger extraction yields in the first part
transfer coefficient, among the many parameters in-
of extraction as indicated by experimental results.
volved, was considered adjustable but was set at the
An example of the concentration profiles in the
same value for all the conditions tested. Indeed, apart
fluid phase predicted by the model is proposed in
from the solvent saturation that was evaluated from
Fig. 6 in the case of extraction test B. In this figure,
the initial part of the extraction experiments in Fig. 4,
values of C are given as a function of the axial coordi-
all the other model parameters were evaluated with
nate along the bed axis and are parametric in the
independent experiments. In particular, scanning elec-
extraction time. Curves at lower extraction times (25
tron microscopy was used to evaluate the volume of
and 50 min) show the equilibrium region on the outlet
the free oil phase. This reduction of the arbitrary
parameters involved in the model makes the valida-
tion of the model itself more significant. Reduction of
arbitrary parameters is important, particularly, if
modeling is aimed at determining the most relevant
physical phenomenon in a complex process, like the
extraction of natural matrices with supercritical fluids.
The concentration profiles within the extractor cal-
culated with our model confirm the existence of
a marked concentration shock wave during the first
extraction stages.

NOTATION
a specific surface of the solid, m~1
C solute concentration in the solvent in terms
of mass of solute per unit mass of solvent,
dimensionless
C solute concentration in the solvent at the
0
Fig. 6. Concentration profiles in the gaseous phase accord- extraction start, dimensionless
ing to model evaluation relative to experimental condition B. d cell diameter, m
c
Curves are given at different extraction times. d particle diameter, m
p
3718 C. Marrone et al.
J volumetric mass transfer flux from the free Fors, S. M. and Ericksson, C. E. (1990) Characteriza-
f
oil phase to the solvent, kg m~2 s~1 tion of oils extracted from Oats by supercritical
J volumetric mass transfer flux from the tied carbon dioxide. ¸ebensmittel ¼iss. º. ¹echnol. 23,
t 390—395.
oil phase to the solvent, kg m~2 s~1
k mass transfer coefficient from the free oil Friedrich, J. P. and List, G. R. (1982) Characterization
f of soybean oil extracted by supercritical CO and
phase to the solvent, m s~1 2
hexane. J. Agric. Food Chem. 30, 192—193.
k mass transfer coefficient from the tied oil
t Goto, M., Sato, M. and Hirose, T. (1993) Extraction of
phase to the solvent, m s~1 peppermint oil by supercritical carbon dioxide. J.
K oil equilibrium constant between the tied oil Chem. Engng Japan 26, 401—407.
p
phase and the solvent, dimensionless Lee, A. K. K., Bulley, N. R., Fattori, M. and Meisen,
Kt oil equilibrium constant between the free oil A. (1986) Modelling of supercritical carbon dioxide
phase and the solvent, kg m~3 extraction of canola oilseed in fixed beds. JAOCS
m mass of the seed charge, kg 63, 921—925.
0 List, G. R., Friedrich, J. P. and Pominski, J. (1984)
m mass of the extracted oil, kg
e Characterization and processing of cottonseed oil
m mass of the flowed solvent, kg
s obtained by extraction with supercritical carbon
P solute concentration in the solid in terms of
dioxide. JAOCS 61, 1847—1849.
mass of solute per unit mass of non-soluble King, M. B. and Catchpole, J. R. (1993) Physico-
solid, dimensionless chemical data required for the design of near criti-
P solute concentration in the solid at the ex- cal fluid extraction process. In Extraction of Natu-
0
traction start, dimensionless ral Products ºsing Near-Critical Solvents, eds M. B.
q almond oil density, kg m~3 King and T. R. Bott, pp. 184—228. Chapman
o
t extraction time, s & Hall, New York.
u interstitial velocity of the solvent, m s~1 Molero Gomez, A., Huber, W., Pereyra Lopez, C. and
½ extraction yield, dimensionless Martinez de la Ossa, E. (1994) Extraction of grape
½ maximum extraction yield, dimensionless seed oil with liquid and supercritical carbon diox-
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