Journal of Food Engineering 46 (2000) 83±89

www.elsevier.com/locate/jfoodeng

E€ect of a novel physical pretreatment process on the drying kinetics

of seedless grapes
Marisa Di Matteo *, Luciano Cinquanta 1, Gianni Galiero, Silvestro Crescitelli 2
Chemical and Food Engineering Department, Salerno University, Via Ponte Don Melillo, 84064 Fisciano, Italy
Received 26 March 1999; accepted 3 April 2000

Abstract
In this paper an alternative physical method for enhancing the drying rate of seedless grapes is proposed. It consists of the
super®cial abrasion of the grape peel using an inert abrasive material. The e€ectiveness of this novel process was compared to that of
the traditional ethyl oleate dipping process by analysing not only their respective drying times, but also the peel surfaces by scanning
electron microscopy. Moreover, the drying kinetics of the above two treatments was reconstructed by using a mathematical model in
which the grape pretreatment used was assumed to a€ect the water di€usivity in the grape peel, but not in the grape pulp. Even
though the abrasion method was found to be as e€ective as the traditional method and gave rise to a darker ®nal product, which is
less attractive to consumers, it would allow grape pretreatment thus avoiding the use of chemical additives, and permit safer raisins
to be produced. Ó 2000 Elsevier Science Ltd. All rights reserved.

Keywords: Grape drying; Abrasion; Dipping; Modelling; Browning

1. Introduction of a preliminary abrasion of the grape peel so as to ac-

Grape drying to produce raisins is a very slow process
(King, 1977; Peri & Riva, 1984; Rizvi, 1986; T ut
unc
u&
Labuza, 1996; Labuza & Hyman, 1998), due to the pe-
culiar structure of grape peel, that is covered by a waxy
layer (Chambers & Possingham, 1963; Aguilera, Op-
permann & Sanchez, 1987; Mahmuto glu, Emõr & Saygi,
1996). Its removal has been so far carried out by using
several chemical pretreatments (Pointing & Mc Bean,
1970; Bolin, Petrucci & Fuller, 1975; Bolin & Sta€ord,
1980; Riva & Peri, 1986; Saravacos & Marousis, 1988).
For example, when grapes are dipped into an alkaline
solution containing, for instance, ethyl oleate, this
component penetrates into the waxy layer and causes
the formation of many small pores. As a consequence,
the drying time of pretreated grapes is up to four times
shorter than the drying time of untreated grapes.
In view of the increasing interest in minimally pro-
cessed food products, the main aim of this work was to
develop an alternative physical pretreatment consisting
*
Corresponding author.
1 s, so as to reduce the average moisture of grapes to
Present address: DI.S.T.A.A.M., Molise University, Via F. De
Sanctis, 86100 Campobasso, Italy.
2
Present address: Chemical Engineering Department, Federico II
University, P.le V. Tecchio, 80125 Napoli, Italy.
0260-8774/00/$ - see front matter Ó 2000 Elsevier Science Ltd. All rights reserved.
PII: S 0 2 6 0 - 8 7 7 4 ( 0 0 ) 0 0 0 7 1 - 6
celerate grape drying to almost the same of that of the
traditional ethyl oleate dipping process. At this point in
time, the feasibility of this process on an industrial scale
was not considered. The aim was to study the e€ec-
tiveness of the process under laboratory conditions.
2. Materials and methods
Seedless white grapes (var. Nevado), harvested from
Trinitapoli in the Puglia region (Italy) and stored at 5°C
for two days before testing, to simulate long distance
transport conditions usually adopted, were used
throughout all experiments. Table 1 shows the main
chemical and physical parameters of about 100 fresh
grape berries.
The abrasion of the grape peel was carried out in a
shaker the walls of which were covered by coating with
abrasive sheets (USM ± Canada, grit range 60±80) as
reported before (Di Matteo, Donsõ, Ferrari, Cinquanta
& La Notte, 1997). Drying experiments were carried out
in a convection oven at 50°C, with an air speed of 0.5 m/
about 20% w/w. Before drying, samples of about 50
grape berries were submitted to one of the following
pretreatments (TR):
84 M. Di Matteo et al. / Journal of Food Engineering 46 (2000) 83±89

Notation r distance from the grape center (m)

B parameter de®ned by Eq. (5) R1 pulp radius (m)
c1 water concentration in the grape pulp (moles/m3 ) R2 overall grape berry radius (m)
c2 water concentration in the grape peel (moles/m3 ) t time (h)
c3 water vapour concentration in air (moles/m3 )
k mass transfer coecient, de®ned by Eq. (8) Greek symbols
Di water di€usivity in the grape pulp …i ˆ 1† and peel …i ˆ 2† bn nth root of Eq. (13)
(m2 /h) d peel thickness …d ˆ R2 ÿ R1 † (m)
h convective mass transfer coecient (m/h) Subscripts
H grape humidity, (%) dry matter 0 refers to time t ˆ 0
K1 equilibrium constant, de®ned by the ratio between the 1 refers to grape pulp
equilibrium concentrations of water in the grape pulp and in 2 refers to grape peel
the grape peel 3 refers to air surrounding the grape berry
K2 equilibrium constant, de®ned by the ratio between the eq refers to equilibrium conditions …t ! ‡1†
equilibrium concentrations of water in the grape pulp and in 1 refers to air bulk
the grape peel
K3 equilibrium constant, de®ned by the ratio between the Superscripts
equilibrium concentrations of water in the grape pulp and TR refers to treated grape berries: abraded (Abr) or dipped
vapour in air (EtOl)
L parameter de®ned by Eq. (12) UT refers to untreated grape berries
N total test number WP refers to grape berries with no peel

Table 1 ments, UK) to evaluate the e€ectiveness of the physical

Main chemical composition and dimensions of 100 fresh grape berries
of var. Nevado
Moisture (% w/w) 84:0  1:6
Acidity (% w/w) 0:2  0:01
Reducing sugar (% w/w) 14:1  0:4
Average radius of grape 1:1  0:1…10ÿ2 †
berries (m)
Average peel thicknessa (m) 15  0:2…10ÿ6 †
a
Measured with scanning electron microscope.
1. immersion in an aqueous solution at 2% (v/v) ethyl
oleate and 2.5% (v/v) K2 CO3 at 40°C for 3 min
(EtOl);
2. abrasion in the shaker for 10 min (Abr);
while untreated samples (UT) were used as reference.
Moisture and reducing sugars content of fresh sam-
ples, as well their acidity expressed as equivalent tartaric
acid (by titration with NaOH solution), were measured
according to AOAC (1989). All measurements were
performed in triplicate.
During and after drying, the colour of the berries was
determined three times on 20 di€erent samples by means
of a colorimeter (chroma-meter type CR-200b, Minolta,
Japan) using the Hunter colorimetric system (L, light-
ness; a , redness; b , yellowness, as de®ned by Hunter,
1979) and by measuring the absorbance (OD) at 425 nm
(Peri & Riva, 1984) with a spectrophotometer (Varian
DMS 100S).
Before drying, the peel of untreated and pretreated
samples was removed, washed with ethanol and dehy-
drated by means of aqueous solutions at 40±100% (w/w)
acetone. Then, after immersion in liquid nitrogen and
vacuum plating, the peel was examined using a scanning
electron microscope (Stereoscan 90, Cambridge Instru-
and chemical methods at removing the waxy layer from
the grape surface.
During the drying process, at each time t, in addition
to the water content, the axes of the grapes (considered
as ellipsoids) were measured; from these values it was
possible to compute the equivalent radius, Ri , as the
radius of the sphere having the same volume of the el-
lipsoid. To take into account the volume reduction of
the grape berries that takes place during the dehydration
process, a staircase function was considered for the
equivalent radius Ri in the mathematical model de-
scribed in the following paragraphs; the value of each
step of the function was computed as the mean between
the initial and the ®nal equivalent radius of each mea-
suring interval.
3. Results and discussion
At the end of the drying process the original structure
of the berries was maintained independently of the
pretreatment used. The abrasion was quite uniform over
the entire surface of the grapes and did not involve any
loss of juice since not one crack was observed both after
the physical pretreatment and after drying. Moreover,
after abrasion the grapes were rougher and had a slight
tissue softening. The drying curves of pretreated and
control grape berries are shown in Fig. 1. Not only was
the drying time needed to reduce the average moisture of
the grape berries from 84% to 20% w/w at 50°C in the
order of 35 h, but also the pattern of the drying curves
was quite similar for both the chemically and physically
treated samples. This drying time was about one third of
the time required to dry the untreated grape berries.
 M. Di Matteo et al. / Journal of Food Engineering 46 (2000) 83±89 85

Fig. 1. Experimental values of humidity (% dry matter) vs drying times

for grape berries the peel of which was untreated (UT) or pre-treated
by dipping into ethyl oleate (EtOl) or by abrasion (Abr).

The e€ect of these methods on the waxy layer re-

moval from the grape peel was analysed by scanning
electron microscopy, as shown in Fig. 2.
In the untreated berries, Fig. 2(a) clearly shows the
waxy network. Fig. 2(b) refers to the peel of a sample
dipped in the ethyl oleate solution. As a result of waxy
solubilization by ethyl oleate, a number of micropores
in the waxy layer was formed, but this was accompa-
nied by a non-uniform redistribution of the waxy
component on the berry surface. Finally, in the peel of
the abraded sample, the waxy layer was almost com-
pletely removed in a quite uniform way (Fig. 2(c)).
The total sugar content, measured on a dry basis, did
not vary after drying and berries showed no sticky
surface.
The quality of grape berries and raisins was assessed
by measuring their colour in terms of the Hunter scale
variables (Table 2). In particular, lightness L and the
yellow chroma component (b ) were in¯uenced by the
pre-treatment used. As a result of drying, the variable L
tended to decrease slightly in all samples, its values being
always greater in pretreated samples than in the un- Fig. 2. Scanning electron micrograph of the peel of a grape berry
treated ones; while the variable b increased in all pre- untreated (a), or pre-treated by dipping in ethyl oleate (b), or by
treated grape berries, being greater for the chemically abrasion (c).
treated samples. After drying the OD values at 425 nm
were lower in chemically treated samples than in phys-
ically and untreated ones.
Generally, the colour of the abraded grape berries and non-enzymatic browning reactions (the former be-
was darker than that of the chemically treated samples, ing due to the polyphenoloxidase mainly located in the
which showed a lighter colour more appreciated peel, Aguilera et al., 1987), the overall e€ect of the grape
by consumers (Grncarevic & Hawker, 1971). Since peel abrasion appeared to be that of enhancing the de-
browning in white grape berries occurs by enzymatic gree of enzymatic browning.
86 M. Di Matteo et al. / Journal of Food Engineering 46 (2000) 83±89

Table 2
Colour parameters of grape berries as fresh product or dried after 48 h when using no pretreatment (UT), ethyl oleate dipping (EtOl) or abrasion
(Abr)

Grape berries Samples pretreatment L a b OD at 425 nm

Fresh UT 42:3  7:2 )3.3 ‹ 0.4 5.6 ‹ 0.7 0:163  0:02

Dried UT 37:1  6:5 )3.1 ‹ 0.3 5.4 ‹ 0.6 0:528  0:04
Dried EtOl 41:8  6:8 2.5 ‹ 0.2 13.8 ‹ 0.9 0:331  0:02
Dried Abr 38:2  5:2 2.7 ‹ 0.2 9.3 ‹ 0.7 0:493  0:03

4. Mathematical model of grape dehydration

In the dehydration process of grape berries by means

of warm air, simultaneous heat and water (liquid and
vapour) transport in the pulp, in the peel (if present) and
in the gaseous ®lm surrounding the grapes, take place.
Since the duration of the thermal transient was generally
found to be far less than the duration of the dehydration
process, mass transport may be regarded as taking place
under isothermal conditions. In other words, the whole
drying process is controlled by mass transport only
(Bird, Stewart & Lightfoot, 1960; Peri & Riva, 1984).
Under the assumptions that pulp and peel (if present)
are uniform and isotropic, and the grape berries are
spherical, the mathematical model of grape dehydration
can be reduced to that of mass di€usion from a spherical
body (Bird et al., 1960; Luikov, 1968; Crank, 1975;
Carslaw & Jaeger, 1980).
Fig. 3 shows the schematic water concentration pro-
®les in the grape pulp and peel, as well as in the gaseous
®lm surrounding each grape berry.
The mathematical model that describes the di€usion
of water through whole grape berries must account for
its di€usion both in the pulp and in the peel. Both the
processes, are described by the model: Fig. 3. Schematic diagram of water (or steam) concentration pro®les in
 2  the grape pulp and peel, and in the gaseous ®lm surrounding each
oci o ci 2 oci grape berry.
ˆ Di ‡ ; …1†
ot or2 r or
where the index i ˆ 1 refers to the pulp [i.e., for
be a linear one, characterised by the equilibrium con-
r 2 …0; R1 †] and i ˆ 2 to the peel [i.e., for r 2 …R1 ; R2 †],
stant K1 . Similarly, water concentration within the grape
D1 is the water di€usivity in the grape pulp, which is
peel can be obtained by solving Eq. (1) for i ˆ 2 with the
much higher than that in the grape peel …D2 †.
following initial and boundary conditions:
Water concentration within grape pulp can be esti-
mated by solving di€erential equation (1) for i ˆ 1 with c10
c2 …r; 0† ˆ ; r 2 ‰R1 ; R2 Š; t ˆ 0;
the following initial and boundary conditions: K1
 
oc2 c2 …R2 ; t†
c1 …r; 0† ˆ c10 ; r 2 ‰0; R1 Š; t ˆ 0; ÿ D2 ˆh ÿ c31 ; r ˆ R2 ; t > 0 if h 6ˆ 1;
or K2
oc1
ˆ 0; r ˆ 0; t > 0; c2 …R2 ; t† ˆ K2 c31 ; r ˆ R2 ; t > 0 if h ! 1;
or …2†
oc1 oc2 …3†
D1 ˆ D2 ; r ˆ R1 ; t > 0;
or or
where the equilibrium±distribution curve relating water
c1 ˆ K1 c2 ; r ˆ R1 ; t > 0;
concentrations at peel/outer environment interface was
where the equilibrium±distribution curve relating water assumed to be a linear one, characterised by the
concentrations in the pulp/peel interface was assumed to equilibrium constant K2 . Water di€usion in the gaseous
 M. Di Matteo et al. / Journal of Food Engineering 46 (2000) 83±89 87

®lm around the grape berry was described by means of steam in the gaseous ®lm surrounding the grape berry.
the convective mass transfer coecient h (Bird et al., The di€usion of water in the pulp is described by dif-
1960). ferential equation (1) with i ˆ 1 together with the fol-
Owing to the thinness of grape (Table 1), it is possible lowing initial and boundary conditions:
to neglect water accumulation in the peel, thus consid-
ering a steady-state distribution of c2 …r; t† in the peel for c1 …r; 0† ˆ c10 ; r 2 ‰0; R1 Š; t ˆ 0;
any time. In this case, the second boundary condi- oc1
ˆ 0; r ˆ 0; t > 0;
tion for the di€usion in the pulp (if h 6ˆ 1) (Eq. (2)) or
becomes: oc1
  D1 ˆ h‰c3 …R1 ; t† ÿ c31 Š; r ˆ R1 ; t > 0 if h 6ˆ 1;
oc1 c1 …R1 ; t† or
ÿD1 jrˆR1 ˆ B ÿ c2eq ; …4† c1 …R1 ; t† ˆ c1eq ; r ˆ R1 ; t > 0 if h ! 1:
or K1
…14†
with
 
D2 D2 =d Under the assumptions that in each instant there is a
Bˆ 1ÿ ; …5† thermodynamic equilibrium at the interface gas/grape
d h=K2 ‡ D2 =d
pulp and that this equilibrium is expressed as a linear
c2eq ˆ K2 c31 : …6† law, it follows that
For h ! 1, Eq. (4) reduces to c1 …R1 ; t†
c3 …R1 ; t† ˆ if h 6ˆ 1; …15†
oc1 K3
ÿD1 j ˆ k…c1 …R1 ; t† ÿ c1eq † …7†
or rˆR1 or
with
c1eq ˆ K3 c31 if h ! 1: …16†
D2
kˆ …8†
dK1 Again, since the gaseous velocity was quite high, it is
and possible to neglect the resistance to the mass transport
out of the grape (i.e. h ! 1). In these circumstances, an
c1eq ˆ K1 K2 c31 : …9† analytic solution (in series) (Carslaw & Jaeger, 1980) can
In the experiments described here, the gaseous ve- be used to estimate water di€usion in a spherical peeled
locity was quite high, thus allowing the resistance to the grape berry (Carslaw & Jaeger, 1980):
mass transport out of the grape to be neglected (i.e.
X  
h ! 1). Under this hypothesis, an analytical solution c1 ÿ c1eq 1 sin …npr
R1
† n2 p2 D1 t
(in series) exists (Luikov, 1968; Crank, 1975): ˆ 2…ÿ1†n‡1 R1 exp ÿ :
c10 ÿ c1eq nˆ1
npr R21
c1 ÿ c1eq 2LR2 X
1
exp …ÿD1 b2n t=R22 † …17†
ˆ
c0 ÿ c1eq r nˆ1 b2n ‡ L…L ÿ 1†
sin …bn r=R2 † By integrating Eq. (17) over the whole volume of any
 : …10† grape berry devoid of its peel, it was possible to derive
sin …bn †
the following time distribution for its humidity:
By integrating Eq. (10) over the whole volume of any
grape berry, it was possible to derive the following time  
H ÿ Heq 6X1
1 n2 p2 D1 t
distribution for its humidity: ˆ 2 exp ÿ : …18†
H0 ÿ Heq p nˆ1 n2 R21
H ÿ Heq X1
exp …ÿD1 b2n t=R22 †
ˆ 6L2 2 2
; …11† By considering just the ®rst term of the above series,
H0 ÿ Heq nˆ1 bn …bn ‡ L…L ÿ 1††
it is possible to describe the logarithmic reduction of the
with ®rst term of Eq. (18) as a linear function of time, as
R2 k previously proposed by Peri and Riva (1984):
Lˆ ; …12†      2 
D1 H ÿ Heq 6 p D1
ln ˆ ln ÿ t: …19†
when bn is the nth root of the following trascendental H0 ÿ Heq p 2 R21
equation:
It has to be pointed out that even if this equation has
bn cot…bn † ‡ L ÿ 1 ˆ 0: …13†
often been used in the literature to estimate the pa-
When any grape berry is peeled, its dehydration rameter D1 , it should be used only for large values of
process can be mathematically described by accounting t; …t ! 1†: in fact for t ˆ 0 it does not forecast
only for the di€usion of water in the grape pulp and H ! H0 .
88 M. Di Matteo et al. / Journal of Food Engineering 46 (2000) 83±89
5. Parameter estimation
The values of unknown parameters of the models
described here were estimated by ®tting the experimental
drying data collected when using peeled, untreated and
chemically and physically treated grape berries. As can
be seen from Fig. 1, humidity±time data for abraded and
dipped berries practically coincided.
The unknown parameters to be estimated are the
following: D1 and c1eq , for all three kinds of grape berries
used, and k for the untreated or treated ones.
A ®rst assessment of such parameters was performed
as follows:
(1) The equilibrium values of the moisture content
…H1eq † for all grape berries used was estimated by aver-
aging the experimental humidity determined at the end
of each drying process on the assumption that such
mean values coincided with the equilibrium ones. From
WP UT TR
these values …Heq ; Heq ; Heq †c1eq for grapes without
peel …c1eq † for untreated grapes …cUT
WP
1eq † and for treated
grapes …cTR1eq † can be easily estimated by considering a
suitable spherical volume.
(2) The di€usivity of water in the grape pulp …D1 † can
WP
be easily estimated via Eq. (19) using the above Heq end
value and the experimental H±t data pertaining to
peeled grape berries. Such a parameter was also used to
describe water di€usivity in the grape pulp of all the
samples tested, these being always composed of grape
berries of the same variety, that were almost simulta-
neously harvested in the same region.
(3) The starting value of the mass transfer coecient
k, which accounts for water di€usivity in the untreated
or treated grape peel …D2 † and equilibrium constant at
the pulp/peel interface …K1 †, was obtained by plotting
the corresponding experimental humidity ratio
…H ÿ Heq †=…H0 ÿ Heq † vs time, by estimating numerically
its slope for t ˆ 0 and by equating such a slope to the
derivative of the above humidity ratio with respect to
time as calculated from Eq. (11) and computed by ac-
counting for the ®rst term of the series only and for
t ˆ 0:
! !
UT
d H ÿ Heq b21 1 average water di€usivity in the whole grape berry, that is
ˆ 6L2 ÿ D1 :
dt H0 ÿ Heq
UT R22 b21 …b21 ‡ L…L ÿ 1††
…20†
Since the parameter k is used to de®ne L and thus im-
plicitly b1 , its estimate has to be obtained by means of
successive iterations.
The optimal estimates of all the unknown parameters
…D1 ; k UT ; K TR ; cWP UT TR
1eq ; c1eq ; c1eq † were derived by mini-
mising the following performance index:
X
N
ÿ
2
Uˆ HiS ÿ HiT …21†
iˆ1
which represents the sum of the squared di€erences
among the experimental humidity HiS data referred to
peeled, untreated and treated grape berries and those
calculated via their corresponding HiT models. More
speci®cally, for the grapes without peel HiT was com-
puted from Eq. (19), thus obtaining HiT ˆ H …D1 ; cWP 1eq †;
for the untreated berries HiT was estimated via Eq. (11)
obtaining HiT ˆ H …D1 ; k UT ; cUT
1eq †; and ®nally for chemi-
cally or physically treated grape berries HiT was com-
puted from Eq. (11) obtaining HiT ˆ H …D1 ; k TR ; cTR 1eq †.
Moreover, any water content was forecasted by con-
sidering the ®rst n terms of any series only, n being
suciently high to assure a relative error between the
generic n and …n ‡ 1† terms summation of less than 1%.
In all the forecasts computed a value of n ˆ 2±3 was
sucient.
The minimisation exercise was carried out by using a
non-linear estimation method based on a mixed (direct/
gradient) algorithm (Buzzi Ferraris, 1972) thus leading
to the optimal values of the above unknown parame-
ters. Their covariance matrix was also computed to
determine the con®dence intervals of all the estimates at
a 95% con®dence level (Buzzi Ferraris, 1972; Bard,
1974).
During the minimisation exercise, the progressive
reduction of the dimensions of any grape berries (due
to their loss of water) was taken into account by
considering their equivalent radius, Ri , as described
before.
The continuous and broken lines in Fig. 1 show the
calculated time variation in moisture content for the
grape berries tested and shows quite a good agreement
with the corresponding experimental values. As previ-
ously stated, it was impossible to detect any moisture
content variation between physically and chemically
treated grape berries.
The optimal value of the water di€usion coecient in
the pulp D1 equal to
D1 ˆ 0:4  10ÿ4  0:1  10ÿ4 …m2 =h†;
was found to be larger than the values reported else-
where (e.g. Riva & Peri, 1986), which referred to the
in its pulp and peel. Therefore, the value determined
here represents the true water di€usivity in the grape
pulp only.
As far as the optimal values are concerned, that is
k TR ˆ 2:817  10ÿ4  2  10ÿ5 …m=h†;
k UT ˆ 7:067  10ÿ5  1:13  10ÿ6 …m=h†;
k TR was obviously found to be greater than k UT and
measures the greater capability of the pre-treatments
used to enhance water di€usivity in the grape skin rel-
ative to that in the untreated samples.
 M. Di Matteo et al. / Journal of Food Engineering 46 (2000) 83±89
6. Conclusions
Removal of the waxy layer from the grape peel by
abrasion was found to be as e€ective as the traditional
chemical dipping method, as con®rmed by the mass
transport coecient k TR which was about 4 times greater
than k UT determined for untreated samples. Not only
the drying time but also the pattern of the drying curves
was quite similar for both the chemically and physically
treated samples. Despite the fact that the physical
method gives rise to a more coloured ®nal product than
the chemical one, it makes no use of chemical additives
and therefore allows safer raisins to be produced.
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