Ultrasonics - Sonochemistry 58 (2019) 104693

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Ultrasonics - Sonochemistry
journal homepage: www.elsevier.com/locate/ultson

Effect of ultrasonic vacuum pretreatment on mass transfer kinetics during T

osmotic dehydration of black jamun fruit
Maanas Sharma, Kshirod K. Dash
⁎

Department of Food Engineering and Technology, Tezpur University, Tezpur, Assam 784028, India

ARTICLE INFO ABSTRACT

Keywords: The study investigates the effects of novel combination of ultrasound and vacuum pre-treatment on osmotic
Ultrasonic vacuum dehydration of black jamun fruit. The osmotic dehydration was conducted under three different conditions
Pre-treatment namely atmospheric osmotic dehydration (AOD), vacuum pre-treated osmotic dehydration (VOD), ultrasonic
Osmotic dehydration vacuum pre-treated osmotic dehydration (USVOD). The changes in water and solute content during osmotic
Water loss
dehydration were fitted to Peleg model to predict the equilibrium moisture and solute content values. The
Solid gain
Mass transfer kinetics
adequacy of Weibull distribution model for predicting the moisture and solute contents during osmotic dehy-
Effective diffusivity dration at different temperatures were assessed. The effective diffusivity of samples in AOD, VOD and USVOD
were estimated by application of Fick’s second law. The high regression coefficient (R2 > 0.9) and low χ2 value
represented the suitability of Peleg model for predicting equilibrium moisture and solute content and Weibull
model for predicting both moisture and solute fraction in jamum fruit during AOD, VOD and USVOD processes.
Both vacuum and ultrasound vacuum pretreatment enhanced the moisture loss and solute uptake during osmotic
dehydration. The results showed the osmotic drying rate was significantly influenced by different pre-treatment
techniques and both vacuum and ultrasonic vacuum pretreatment process enhanced moisture loss and solute
uptake during osmotic dehydration. The effective moisture and solute diffusivity were highest in ultrasonic
vacuum pretreated samples and the values at 30–50 °C temperature were ranged from 8.53 × 10−10 to
9.27 × 10−10 m2/s and 3.81 × 10−10 to 4.39 × 10−10 m2/s respectively. The results were interrelated to
changes in tissue structure caused by application of vacuum and ultrasonic vacuum pretreatment.

1. Introduction
Jamun (Syzygium cumini) is an underutilized fruit that belongs to the
Myrtaceae family. Jamun is a seasonal fruit that is most likely available
in the month of May to July with a shelf life of 2–3 days at room
temperature [1]. The fruit is pulpy, oval in shape and dark purple color
with high-therapeutic worth used for the treatment of several diseases
such as an astringent, antiscorbutic, diuretic, antidiabetic, and in
chronic diarrhea and enlargement of the spleen [2]. The fresh fruit
mainly consumed in raw form and also used to prepare jams, juices,
vinegar, wine and squash [3–5].
Dehydration is the common preservation technique to reduce post-
harvest loss and dehydration process extends the shelf life and avail-
ability of the product in all seasons [6]. Osmotic dehydration is a
process in which the food is immersed in a hypertonic solution of high
osmotic pressure for the partial removal of water resulting in inter-
mediate moisture content product [7]. The complex cellular structure of
food (i.e., fruit, vegetable, fish, etc.) acts as a semi-permeable
membrane and two major countercurrent flows take place simulta-
neously [8]. The diffusion of moisture takes place as the primary flow
took out by the counter-diffusion of solutes from the osmotic solution
into the food as the secondary flow [9,10]. The rate of diffusion of
water and osmotic solutes during the osmotic dehydration depends on
several parameters such as the raw material (shape, size, porosity,
maturity level), the composition and concentration of the osmotic
medium, the temperature, the immersion time, the ratio of sample to
solution and degree of agitation [11]. The osmotic dehydration process
is used an supplementary processing step before thermal dehydration as
an energy efficient and cost reducing process [12]. This process pro-
vides close to fresh food to satisfy the consumer's demands of minimally
processed food that is essential to maintain its nutritional character-
istics [10,13]. The osmotic agent used in osmotic dehydration can be a
sugar, salt, starch or even a combination of various osmotic agents [14].
Empirical models like Peleg model can be used to predict the behavior
of water loss and solid gain at the equilibrium [15]. Peleg model was
used to describe the mass transfer (moisture loss and solid gain) during

⁎
Corresponding author.
E-mail address: kshirod@tezu.ernet.in (K.K. Dash).

https://doi.org/10.1016/j.ultsonch.2019.104693
Received 16 April 2019; Received in revised form 5 July 2019; Accepted 14 July 2019
Available online 15 July 2019
1350-4177/ © 2019 Elsevier B.V. All rights reserved.
M. Sharma and K.K. Dash
Fig. 1. Ultrasonic vacuum osmotic dehydration of black jamun fruit.
osmotic dehydration of sardine sheets [16], pulsed vacuum osmotic
dehydration of mango slices [17] and ultrasound pretreated osmotic
dehydration of kiwifruit [18]. Weibull model representing exponential
shape have been used to predict osmotic dehydration rates of foods
after specific time interval of the dehydration process.
There are several methods used to enhance the mass transfer in the
osmotic process like agitation or rotation, pulsed-vacuum [19], high
pressure [20], ohmic heating [21], pulse electric field [22], cen-
trifugation and ultrasound [23] to reduce processing time. Pretreatment
techniques like vacuum or ultrasound essential to accelerate the drying
process that improves quality and safety. This pre-treatment techniques
were used to upsurge the mass transfer rate between the sample and its
enclosing causing acceleration in the drying process [24,25].
Ultrasound is a novel technology in which sound waves at frequency
16 kHz to 100 MHz produce alternative compression and expansions
and produce acoustical cavitation rupturing the cell of fruit or vegetable
[26-28]. The process parameters influencing the osmotic dehydration
rate and structure of the end product were ultrasound frequency, pro-
cessing time and ultrasound power [29,30]. Ultrasonic assisted osmotic
dehydration was enhanced the mass transfer in different fruits and
vegetable like broccoli [31], cranberries [26] kiwi fruit [18], and
pineapple [32]. Application of vacuum in osmotic dehydration pro-
motes the dehydration rate by augmenting penetration of osmotic
medium into the pores of the fruit and vegetable tissues. Vacuum os-
motic dehydration was enhanced the dehydration process in various
fruits and vegetables such as melon [33], granny smith apple [34] and
guava [35].
In this study, a novel design was presented to enhance the osmotic
2
Ultrasonics - Sonochemistry 58 (2019) 104693
dehydration by combining ultrasound and vacuum processes. The ob-
jectives of the study were (i) to evaluate the effect of vacuum and ul-
trasound-assisted vacuum on osmotic dehydration of jamun fruit in
sucrose solution (ii) to study the applicability of Peleg model and
Weibull frequency distribution model in predicting moisture content
and solute content during osmotic dehydration of jamun fruit (iii) to
determine the moisture and solute diffusivity by applying the Fick’s
second law.
2. Materials and methods
2.1. Materials and preparation of the osmotic solution
Black jamun (Syzygium cumini) were purchased from local market
nearby Tezpur University, Assam, India. They were sorted depending
on their maturity, shape, size, and color. The initial moisture of the fruit
was estimated by gravimetric method [36] and the average initial
moisture content was found to be 88.19 ± 1.26% (wet basis as mass of
water per total mass of sample). Food grade sucrose was used as an
osmotic agent. The osmotic solution was prepared by dissolving sucrose
in distilled water by means of a magnetic stirrer (model no. 4050,
Tarson, India). The concentration of osmotic solution was 60oB in
binary solution. The soluble solid content of the osmotic solution was
determined by refractometer.
2.2. Osmotic dehydration experiment
The osmotic dehydration experiment was carried out under three
M. Sharma and K.K. Dash Ultrasonics - Sonochemistry 58 (2019) 104693

different conditions i.e. atmospheric pressure osmotic dehydration wf sof wissi

Solid Gain (%) = SGt = × 100
(AOD), vacuum pretreated osmotic dehydration (VOD) and ultrasonic wi (2)
vacuum pretreated osmotic dehydration (USVOD). A sample to solution
mass ratio of 1:10 was used in all experiments in order to avoid sig- wi wf
Weight reduction (%) = WRt = WLt SGt = × 100
nificant changes on osmotic solution concentration during the experi- wi (3)
mental process. The osmotic dehydration was carried out at five dif-
where wi and wf are the initial and final weight (g) of the sample; si and
ferent temperature such as 30, 35, 40, 45 and 50 °C for 300 min. The
sf are the initial (t = 0) and final (t = t) moisture content (g moisture/g
temperature ranges was chosen between 30 and 50 °C because at lower
dry matter) of sample; ssi (ssi = (1 si) ) and sof (sof = (1 sf ) ) is the
temperature below 30 °C the process is very slow and takes very longer
initial and final soluble solid content (g solid/g) respectively.
duration and higher temperatures above 50 °C may lead to enzymatic
browning and flavour deterioration [37].
2.5. Mass transfer models
The atmospheric osmotic dehydration process was carried out in a
shaking incubator (Sartorius Stedim Biotech Certomat IS, Goettingen,
2.5.1. Peleg model
Germany) at constant agitation of 60 rpm to ensure a uniform tem-
Peleg model is a two parameter model which describes the kinetics
perature throughout the experiment. At every 30 min the dehydrated
of moisture sorption that approaches equilibrium asymptotically. The
samples of each group were drained in slow tap water, wiped with
version of this model implemented for the water loss and solid gain is
blotting paper to remove excess solution from the outer surface of the
presented in Eqs. (4) and (5) respectively.
fruit, and then weighed gently. Vacuum pre-treatment was performed
at different temperatures at 30, 35, 40, 45 and 50 °C in a vacuum drying WL =
t
chamber at pressure 100 mbar (750 mmHg) for a period of 20 min. k1w + k2w × t (4)
Subsequently, the atmospheric pressure was re-established and the os-
t
motic dehydration was conducted at atmospheric condition until the SG =
k1s + ks2 × t (5)
end of the process. All experiments were performed in triplicate and the
obtained data were expressed as the mean ± standard deviation. where k1w and are the parameter for water loss,
k2w are the k1s andks2
parameter for solid gain. The reciprocal value of k1 is the initial rate of
water loss or solute gain. The parameter k2 is known as Peleg capacity
2.3. Design for ultrasonic vacuum pre-treatment of black jamun
constants. The Peleg capacity constants were dependent to equilibrium
moisture constant and equilibrium solid gain, it means lower the k2
The ultrasonic vacuum equipment was composed of an ultrasound
value higher will be the equilibrium moisture content and mass transfer
water bath (30 kHz, amplitude: 100%, 100 W power, Bandelin Sonorex,
rate [39].The reciprocal value of k2 allows determining the equilibrium
Germany) equipped with a capped 250 ml Buchner flask (Fig. 1).
moisture and solute content.
Buchner flask was connected to a vacuum pump by flexible hose to
regulate the vacuum level inside the chamber. The bath temperature
2.5.2. Weibull’s distribution model
was maintained at 30, 35, 40, 45 and 50 °C within a maximum error
The Weibull distribution representing the probability distribution
of ± 1 °C. The ultrasonic vacuum pretreatment was carried out by im-
functions was widely used in reliability and life data analysis due to its
mersing the fruit in distilled water and the ratio of jamun fruit to water
versatility. The Weibull distribution can be used for predicting the
was set to 1:4 (w/w). Distilled water was used as the liquid medium in
moisture and solid contents of jamun fruit during AOD, VOD and
the ultrasonic vacuum treatment to avoid interference between osmotic
USVOD processes. The fractional amount of moisture loss and solid gain
solution and fruit during the pretreatment process. During experiments,
during osmotic dehydration can be expressed in Eqs. (6) and (7)
a pressure of 100 mbar (750 mm Hg vacuum) was maintained. The
[40,41].
buchner flask under vacuum was subjected to ultrasonic waves for a
period of 20 min. Studies on ultrasound assisted osmotic dehydration WL t w
showed the changes caused by ultrasonic waves on the effective water 1 = MR = exp
WL w (6)
diffusivity became slight after 20 min and below10 min the effect of
ultrasound was insignificant [38]. After the ultrasonic vacuum pre-
SG t s
treatment process, the osmotic dehydration of samples was conducted 1 = SR = exp
SG (7)
at a temperature range of 30–50 °C at the atmospheric condition. s

During this process, fruits were removed from the osmotic solution at
every 30 min interval and weighed to estimate the water loss during the
process. The total solids were determined gravimetrically by drying the
samples to constant weight at 70 °C in a vacuum oven to evaluate the
solid gain. Each experiment was carried out in triplicate and the data
were presented as the average of three data sets.
where MR and SR are the dimensionless moisture and solute ratio, w is
scale parameter, w is shape parameter and t is sampling time (s). w , s ,
w , s are the parameters of the Weibull model associated with the
process rate.
2.6. Diffusivity

2.4. Estimation of water loss & solid gain Mass transfer kinetics during osmotic dehydration was based upon
various solutions to Fick’s law of diffusion. The Fick’s unsteady state
The performance parameters of osmotic dehydration i.e. water loss diffusion model presented in Eq. (8) was implemented to describe the
(WL), and solid gain (SG), and weight reduction (WR) at specific time osmotic dehydration of jamun fruit considering it as a sphere of radius
intervals were calculated using Eqs. (1), (2) and (3) respectively. Water r.
loss was defined as the grams of net water loss at time t from the fresh
C C2
sample based on an initial dried weight (g) and solid gain was defined =
(8)
t r2
as the grams of net increase of the osmosed sample at time t based on an
initial dried weight (g). The solution of Fick’s second law for diffusion for a spherical pro-
duct was done based on the following assumptions.
wi si wf s f
Water loss (%) = WLt = × 100
wi (1) i. Moisture transfer is predominantly one-dimensional;

3
M. Sharma and K.K. Dash Ultrasonics - Sonochemistry 58 (2019) 104693

1
N 2
1
RSME = (Ei Oi )2
N i=1 (13)

where N is the total number of data values used to fit the equation, Oi
and Ei are the experimental and predicted model values respectively. Ei
is the average of all experimental data.

3. Results and discussion

3.1. Effect of temperature and time on water loss and solid gain under
atmospheric pressure

In osmotic dehydration process, the moisture was transferred from

fruit to the solution and the solute was transferred from the osmotic
solution to the fruit in a counter-current manner under different con-
ditions (AOD, VOD, and USVOD). During the osmotic dehydration of
Fig. 2. Changes in water loss and solid gain during osmotic dehydration of
jamun fruit, the moisture content and solute content at different in-
black jamun fruit in a sucrose solution at 50 °C.
terval of immersion times were experimentally obtained over a tem-
perature range of 30–50 °C. The obtained moisture content data were
ii. The initial moisture content is distributed uniformly in the product; used to evaluate moisture ratio and the solute ratio (Eqs. (6) and (7)).
iii. Shrinkage is negligible The variations of moisture loss and solute gain with immersion time at
iv. The diffusion coefficient, considered as constant and homogeneous dehydration temperature of 50 °C under AOD, VOD and USVOD was
during drying. presented in Fig. 2. The moisture ratio and solute ratio were initially
steeper at the time of 0–150 min due to rapid moisture loss and solute
The solution of Eq. (8) for spherical geometry presented in Eqs. (9) gain in the beginning, which became shallow after a period of 150 min.
and (10) was used to analyze unsteady-state moisture and solute dif- The moisture loss and solute gain were faster in the beginning due to
fusivity in symmetric porous material like jamun fruit. the large osmotic driving force between the dilute sap of the fresh fruit
and the surrounding hypertonic osmotic solution.
6 t
n2 The osmotic dehydration temperature was found to have a sig-
MR = exp 2D
2 ew 2
n=1
r (9) nificant effect (p < 0.05) on water loss and solid gain. The results
showed that the amount of water reduction and solute uptake was more
6 2D t intense at a higher temperature. Hence, the drying time was sig-
SR = 2
exp n2 es 2
n =1
r (10) nificantly decreased by increasing the dehydration temperature. After
300 min of osmotic dehydration at 30 °C, the water loss and solid gain
where Dew and Des are the effective diffusivities of water and solute
was around 0.352 g/g and 0.046 g/g of initial mass respectively
respectively.
whereas at 50 °C, water loss and the solid gain values were 0.401 g/g
and 0.068 g/g of initial mass respectively. The water loss and solid gain
2.7. Scanning electron microscopy (SEM) in watermelon were found to be 0.30 to 0.60 g/g and 0.1 to 0.2 g/g of
initial mass at 40 °C in 50 °Brix sucrose solution [45]. Similarly in
The microscopic structure of the osmotic dehydrated jamun fruit apricot also the water loss and solid in the range of 0.10–0.40 g/g and
were scanned using JEOL scanning electron microscope (JSM 6390 LV, 0.02–0.11 g/g of fresh fruit at 25–45 °C in 40–70% sucrose solution
Japan, PN junction type, and semi-conducting detector) at an accel- [46].
erating voltage of 20 kV at 500X magnification. It was observed from
1 mm thickened thin slice of the osmotic dried jamun samples that was 3.2. Effect of vacuum pre-treatment on water loss and solid gain
fixed on the SEM stub followed by a thin layer of platinum coating.
The osmotic dehydration followed by vacuum as a pre-treatment
2.8. Statistical analysis process under 100 mbar (750 mmHg vacuum) pressure in the vacuum
drier at 30–50 °C enhanced the moisture loss and solute gain of jamun
The statistical analysis of experimental data were conducted using fruit. Compared with atmosphere pressure condition, the vacuum
SPSS statistical software (SPSS Inc., Chicago, IL. U.S.A.) applying the treatment caused higher water loss and solute gain. The vacuum pre-
analysis of variance to estimate statistically significant differences for a treatment removed the gas in the inter-cellular spaces of fruit tissue and
confidence level of 95% (p < 0.05). The coefficient of determination when it was reinstated in an atmospheric condition, the sucrose solu-
(R2), chi-square (χ2), and root mean square error (RMSE) were well tion entered into the pores of the food matrix. This increases the ex-
chosen as the primary criteria to determine the suitability and goodness posed surface area between fruit and osmotic solution resulting in en-
of fit in the model [19,20,42–44]. The higher R2 values and lower χ2 hanced mass transfer rate.
and RMSE values represented the best fitting of the mathematical The moisture loss and solute gain rate was significantly increased
model to predict the behaviour during osmotic dehydration. The 2 , R2 (p < 0.05) by using vacuum as pre-treatment at different temperatures
and RMSE vales were evaluated by applying Eqs. (11)–(13). (Fig. 3B). After 300 min, osmotic dehydration at 30 °C the water loss
and solid gain values were 0.471 g/g and 0.076 g/g of initial mass
N
2 (Oi Ei ) 2 whereas at 50 °C, water loss and solid gain values were 0.524 g/g and
=
cal
I=1
(Ei ) (11) 0.097 g/g of initial mass respectively. Studied on vacuum treated os-
motically dehydrated mango fruit slices showed the water loss and solid
N
(Oi Ei )2 gain was ranged between 0.23–0.54 g/g and 0.01–0.06 g/g dry weight
R2 = 1 respectively within a temperature range of 20–40 °C in 45–65°Brix su-
i=1 (Oi Ei )2 (12) crose solution at vacuum pressure of 50–200 mbar [17]. The VOD for

4
M. Sharma and K.K. Dash
Fig. 3. A plot of moisture ratio vs time and solid ratio vs time of black jamun
fruit at different temperatures (30, 40 and 50 °C) processed by (A) AOD, (B)
VOD, and (C) USVOD.
cherry tomato at the vacuum pressure of 13 kPa for 15 min resulted in
water loss in the range of 10–50% and solid gain in the range of 8–10%
at 50 °C in 50–70 °Brix sucrose solution [7]. Similarly vacuum im-
pregnation (0.04 MPa, 15 min) resulted in an increase of 20.6% water
loss and 31.3% solid gain in comparison to atmospheric osmotic de-
hydration [47].
5
Ultrasonics - Sonochemistry 58 (2019) 104693
3.3. Effect of ultrasound vacuum pre-treatment on water loss and solid gain
The jamun fruits were subjected to USVOD process and its effect on
water loss and solid gain were studied. The plots of USVOD of jamun
fruit were steeper up to 100 min and became shallow beyond that
(Fig. 3C). The USVOD showed significantly higher (p < 0.05) water
loss and solid gain as compared to AOD and VOD at all temperatures.
The water loss and solid gain were higher due to the enhancement of
mass transfer by application of ultrasound and vacuum that may ease
moisture removal during dehydration. The water loss and solid gain at a
temperature of 30 °C after a period of 300 min was 0.545 g/g dry solids
and 0.093 g/g dry solids respectively. When the dehydration tempera-
ture was increased to 50 °C the water loss and the solute gain was in-
creased to 0.583 g/g dry solids and 0.114 g/g solids respectively. Ul-
trasound treatment in pineapple fruit accelerated the mass transfer by
disruption of the fruit tissue resulting in formation of larger number of
microscopic channels in the fruit [48]. The ultrasound-assisted osmotic
dehydration of carambola slices showed 54.36% average water loss and
7% solid gain at 40–60 °C in 50–70 °Brix sucrose solution within a
period of 180 min [29]. The water loss and solid gain were reported in
ultrasound osmotically dehydrated of carrot were 0.58 g/g and 0.14 g/g
wet basis in 40–60% fructose solution in 2 h at 30 °C [49].
3.4. Peleg model
Experimental data within the dynamic segments of water loss and
solid gain and away from equilibrium conditions were used to evaluate
the adequacy of the Peleg’s equation. Tables 1 and 2 presented Peleg
parameters for water loss and solid gain obtained from the non-linear
regression analysis. The Peleg model was fitted to determine the equi-
librium moisture content (EMC) and solute content (ESC) for the os-
motic dehydration process. Peleg’s model parameter for water loss (k1w
and k2w ) and solid gain (k1sks2 ) were shown in Tables 1 and 2 respectively.
The average R2, χ2 and RMSE values obtained by fitting the mass
transfer parameter for water loss data over processing time for AOD
were 0.975, 3.54 × 10 3 and 0.59 respectively. The corresponding values
of R2, χ2 and RMSE for VOD were 0.980, 1.76 × 10 3 and 0.49 and for
USVOD were 0.977, 1.42 × 10 3 and 0.37 respectively. Similarly, for
solid gain, the average R2, χ2, and RMSE for AOD were 0.960,
1.61 × 10 3 and 0.12, for VOD were 0.981, 1.37 × 10 3 and 0.11 and for
USVOD were 0.989, 1.26 × 10 3 and 0.11 respectively. Therefore, the
high values of R2 and the low values of both chi-square and RMSE
(Tables 1 and 2) suggested the adequacy of Peleg’s equation to de-
scribes mass transfer kinetics terms during osmotic dehydration of
jamun fruit at given solution concentrations and temperatures over
immersion time [16].
The reciprocal of k1 described the initial mass transfer rate, e.g., the
lower the k1, the higher mass transfer rate. At atmospheric osmotic
dehydration the k1w values decreased from 2.33 to 1.68 as the tem-
perature increased by 30–50 °C. For USVOD the k1w values decreased
from 0.99 to 0.80 in the temperature range 30–50 °C, which specifies an
increase in the initial rate of mass transfer for the combined ultrasonic
and vacuum assisted pretreated samples. During osmotic dehydration of
seedless guava the k1 was also decreased (p < 0.05) with increasing
temperature using 30–50% (w/w) sucrose solution at 30–50 °C [50].
The k2w values in the temperature range of 30–50 °C were varied in
the range of 0.020–0.018, 0.017–0.016 and 0.015–0.014 for AOD, VOD,
and USVOD samples respectively. The ks2 values for AOD, VOD, and
USVOD samples were varied in between 0.120–0.092, 0.089 and 0.074,
0.071 and 0.061 respectively within 30 to 50 °C dehydration tempera-
ture. The variations of k2 revealed that temperature and pretreatment
process significantly (p < 0.05) affected the Peleg constant k2 for
water loss and solid gain during osmotic dehydration of jamun fruit.
Considering that 1/k2w and 1/ks2 describes the equilibrium condition it
was observed that using USVOD the EMC and ESC were higher as
compared to VOD and AOD. The EMC for combined ultrasound vacuum
M. Sharma and K.K. Dash Ultrasonics - Sonochemistry 58 (2019) 104693

Table 1
Parameters evaluated of Peleg model for Water loss.
Treatment Temperature (°C) k1w k2w χ2 (×10−3) Adj. R2 RMSE

Atmospheric 30 2.337 ± 0.098 0.0203 ± 0.00054 4.018 0.969 0.6339

35 2.000 ± 0.076 0.0197 ± 0.00043 3.612 0.975 0.6011
40 1.899 ± 0.070 0.0195 ± 0.00039 3.498 0.976 0.5915
45 1.800 ± 0.064 0.0194 ± 0.00037 3.347 0.978 0.5786
50 1.681 ± 0.057 0.0188 ± 0.00033 3.240 0.980 0.5693

Vacuum 30 0.990 ± 0.024 0.0176 ± 0.00015 1.933 0.990 0.4397

35 0.926 ± 0.021 0.0172 ± 0.00014 1.836 0.991 0.4285
40 0.867 ± 0.019 0.0168 ± 0.00012 1.746 0.992 0.4179
45 0.814 ± 0.017 0.0164 ± 0.00011 1.662 0.993 0.4077
50 0.789 ± 0.016 0.0162 ± 0.00011 1.622 0.933 0.4028

Ultrasonic-vacuum 30 0.721 ± 0.014 0.0156 ± 0.000097 1.510 0.994 0.3887

35 0.700 ± 0.013 0.0155 ± 0.000091 1476. 0.994 0.3842
40 0.672 ± 0.012 0.0153 ± 0.000081 1.420 0.968 0.3769
45 0.650 ± 0.011 0.0151 ± 0.000083 1.380 0.958 0.3716
50 0.614 ± 0.010 0.0148 ± 0.000076 1.315 0.971 0.3627

pretreated samples were varied between 0.641 and 0.676 g/g fresh
fruit, whereas for the vacuum pretreated sample the EMC was varied
between 0.568 and 0.617 g/g of fresh fruit. Similarly, the ESC values
were 0.083–0.108 g/g for AOD, 0.112–0.135 g/g for VOD and
0.141–0.164 g/g for USVOD respectively. The equilibrium of jenipapo
at 30 °C in 30–70°Brix sucrose solution was reached after 12 – 32 h
where the EMC and ESC concentration were ranged between 36 and
66 g/100 g and 31–49 g/100 g in atmospheric condition [51]. The EMC
and ESC values of coconut slices were found to be 0.58 kg/kg and
0.09 kg/kg respectively in 12.5% sucrose solution with ultrasound
treatment [27]. Peleg’s model was also found to adequately describe
both the water loss and solid gain kinetics of the osmotic dehydration of
strawberry samples under pulsed vacuum and ultrasound treatment
[52].
3.5. Water loss and the solid gain ratio
The ratio of water loss and solid gain (WL/SG) was used to de-
termine the process efficiency of the osmotic dehydration process. High
water loss and solid gain ratios give rise to intensive water removal
from the fruit samples with minimal solid gain [53]. The WL/SG ratio
was gradually decreased during the osmotic dehydration of black
jamun fruit, after the initial rise within the first 30 min of the process.
The values were ranged from 5.996–12.780 for atmospheric,
5.681–10.878 for vacuum and 4.910–8.945for ultrasound vacuum
treatment (registered at 50 °C, 60°B solution, after 300 min). The
highest WL/SG ratio value of 12.78 was achieved at 30 °C at 300 min in
60 °B solution.
3.6. Weibull model
Weibull model is an empirical model based on the exponential be-
havior that is implemented to express the osmotic dehydration rates of
foods [19,54]. The Weibull model depends on equilibrium moisture
content and solid gain (WL∞ and SG∞) values to determine moisture
ratio and solid ratio. The Weibull model parameters w and s were
scale parameters for water loss and solute gain which were associated
with the rate of process. w and s were shape parameters for water loss
and solid gain and were associated with the mass transfer rate at the
beginning of the process [15]. The Weibull model (Eqs. (6) and (7)) was
fitted to the data obtained by different in osmotic dehydration treat-
ments and the estimated parameters are listed in Tables 3 and 4.
3.6.1. Weibull model parameters for water loss
The results showed that αw and βw were affected both by pre-
treatment method and temperature of osmotic dehydration process
(Table 3). The Weibull model exhibited a strong fit to predict the
moisture ratio as indicated by the higher R2 (0.962–0.995) with low-
ered χ2 (3.04 × 10 4 5.21 × 10 4) and RMSE (0.017–0.023) values. At
atmospheric condition, αw values were ranged from 199.948 to
159.631 (min) and the βw values, 0.726 to 0.691, respectively. Both the
scale parameter and shape parameter for water loss were decreased
significantly (p < 0.05) with increasing osmotic dehydration process
temperature. In the vacuum pretreated samples at 100 mbar, αw values

Table 2
Parameters evaluated of Peleg model for Solid gain.
Treatment Temperature (°C) k1s ks2 χ2 (×10−3) Adj. R2 RMSE

Atmospheric 30 36.551 ± 2.551 0.120 ± 0.0119 0.17 0.990 0.1325

35 30.563 ± 1.883 0.114 ± 0.0090 0.16 0.927 0.131
40 23.307 ± 1.177 0.102 ± 0.0057 0.16 0.951 0.1272
45 19.439 ± 0.872 0.097 ± 0.0043 0.15 0.962 0.1243
50 15.917 ± 0.632 0.092 ± 0.0032 0.14 0.970 0.1208

Vacuum 30 14.467 ± 0.542 0.089 ± 0.0028 0.14 0.974 0.1194

35 12.307 ± 0.410 0.082 ± 0.0021 0.138 0.979 0.1178
40 11.154 ± 0.349 0.079 ± 0.0018 0.135 0.982 0.1165
45 11.043 ± 0.340 0.077 ± 0.0018 0.136 0.985 0.1168
50 9.756 ± 0.279 0.074 ± 0.0015 0.132 0.984 0.115

Ultrasonic-vacuum 30 8.879 ± 0.238 0.071 ± 0.0012 0.130 0.987 0.1141

35 8.273 ± 0.213 0.069 ± 0.0011 0.128 0.988 0.1141
40 7.769 ± 0.193 0.067 ± 0.0010 0.126 0.989 0.1125
45 7.198 ± 0.170 0.065 ± 0.0009 0.124 0.990 0.117
50 6.462 ± 0.142 0.061 ± 0.0007 0.123 0.991 0.111

6
M. Sharma and K.K. Dash Ultrasonics - Sonochemistry 58 (2019) 104693

Table 3
Estimated parameters for the Weibull model of Water loss.
Treatment Temperature (°C) αw (min) βw χ2 (×10−4) Adj. R2 RMSE

Atmospheric 30 199.948 ± 2.378 0.726 ± 0.0396 5.21 0.980 0.0231

35 178.396 ± 1.470 0.708 ± 0.0372 5.07 0.981 0.0225
40 172.434 ± 1.236 0.703 ± 0.0359 4.99 0.971 0.0223
45 165.063 ± 1.192 0.696 ± 0.0359 4.95 0.985 0.0222
50 159.631 ± 2.762 0.691 ± 0.0350 4.80 0.962 0.0219

Vacuum 30 102.527 ± 1.026 0.628 ± 0.0298 4.02 0.994 0.0200

35 98.354 ± 1.272 0.622 ± 0.0351 3.88 0.983 0.0196
40 94.476 ± 1.187 0.616 ± 0.0787 3.74 0.980 0.0193
45 90.671 ± 1.088 0.611 ± 0.0283 3.60 0.984 0.0189
50 89.059 ± 0.148 0.608 ± 0.0276 3.54 0.988 0.0188

Ultrasonic-vacuum 30 84.131 ± 0.924 0.601 ± 0.0164 3.36 0.995 0.0183

35 82.667 ± 0.893 0.598 ± 0.0211 3.30 0.992 0.0181
40 80.232 ± 0.838 0.595 ± 0.0266 3.22 0.993 0.0179
45 78.370 ± 0.784 0.592 ± 0.0128 3.14 0.985 0.0177
50 75.608 ± 0.458 0.587 ± 0.0259 3.04 0.996 0.0174

were decreased from 102.527 to 89.059 and βw values were decreased
from 0.628 to 0.608. Furthermore, under ultrasonic vacuum pre-treat-
ment, αw values were decreased from 84.131 to 75.608 and the βw
values from 0.601 to 0.587. The scale parameter in the Weibull time
reliability relationship scales the value of process time ‘t’ i.e. it stretches
or contracts the failure distribution along the time axis.
Hence the value and unit of scale parameter are determined by the
unit of time‘t’. At any specific temperature level, the αw in ultrasound
vacuum treatment is lower than vacuum treatment and atmospheric
condition, which indicated the higher water loss rate in USVOD process
than VOD and AOD process. The shape parameter (βw) is also known as
the Weibull slope or the threshold parameter. The shape parameter was
related to the velocity of the mass transfer at the beginning of the os-
motic dehydration process. Among the three different processes i.e.
USVOD, VOD and AOD the βw value were lowest in USVOD samples.
Hence, the initial rate of water loss in USVOD was faster than VOD and
AOD process. A similar trend was reported of Fuji apple where αw va-
lues were lower (0.46) in ultrasound treated at 50/60 Hz and 185 W as
compared to pulse vacuum (0.56) at 13 MPa and agitation (0.57) at
55 rpm [19]. αw of corn cereal and peanut butter cereal were decreased
as increased in temperature of 5–55 °C from 97.6 to 8.4 and 1268.8 to
104.7 [55].
3.6.2. Weibull model parameters for solute gain
The values of scale (αs) and shape (βs) parameters of the Weibull
model for the fractional amount of solute content at different tem-
perature for pretreated and untreated samples are shown in Table 4. For
solid ratio, the R2, χ2 and RMSE values were ranged between
0.942–0.996, 2.11 × 10 4 3.75 × 10 4 , and 0.0145–0.0193 respec-
tively indicating higher predictive capability of Weibull model for
prediction of solute ratio during osmotic dehydration process. In AOD
process the αs values were ranged from 284.386 to 452.068 (min) and
βs values were ranged from 0.771 to 0.844 within temperature of 30 to
50 °C. Under vacuum treatment, the αs and βs values were ranged from
224.739 to 268.819 (min) and 0 0.733 to 0.761 whereas in USVOD
process the values of αs and βs were varied from 185.617 to 215.460
and 0.704 to 0.726 respectively.
At any particular temperature level, the values of shape factor βs in
atmospheric condition were found to be higher than that of the sample
pretreated with vacuum and ultrasound vacuum condition. The lowest
value of the shape factor ‘βs’ with ultrasound vacuum pre-treatment
revealed that solute uptake in this process was faster than VOD and
AOD process. Hence USVOD process is also more favorable to solute
uptake. The values of βs for fractional amount solute content sig-
nificantly decreased (p < 0.05) with increasing temperature from 30
to 50 °C. Lower shape parameter at the high temperature indicated a
faster solid gain in high temperature processed samples. The scale
parameter αs for solute gain was also found to be decreased (p < 0.05)
with increasing temperature. The value scale parameters of the solid
gain (αs) were higher than those of water loss (αw) at all temperature
levels indicate that the solid gain rate was slower than that of water loss
due to the semipermeable characteristics of the cell walls. Similar
findings were reported in the study of influence of ultrasound and pulse
vacuum on osmotic dehydration kinetics of apples (Fuji) [56].
For variable temperature condition, it was observed that both the
scale parameters (αw, αs) and shape parameters (βw, βs) is a function of

Table 4
Estimated parameters of the Weibull model for solid gain.
Treatment Temperature (°C) αs (min) βs χ2 (×10−4) Adj. R2 RMSE

Atmospheric 30 452.068 ± 3.433 0.844 ± 0.0514 3.75 0.981 0.0193

35 408.373 ± 4.385 0.828 ± 0.0466 3.52 0.942 0.0187
40 360.004 ± 2.432 0.807 ± 0.0396 3.06 0.985 0.0174
45 323.181 ± 1.252 0.789 ± 0.0366 2.92 0.986 0.0171
50 284.386 ± 2.568 0.771 ± 0.03325 2.83 0.967 0.0168

Vacuum 30 268.819 ± 3.613 0.761 ± 0.0315 2.76 0.982 0.0166

35 252.057 ± 2.511 0.751 ± 0.0298 2.55 0.994 0.0159
40 239.394 ± 1.871 0.743 ± 0.0287 2.48 0.988 0.0157
45 241.102 ± 0.889 0.744 ± 0.0282 2.43 0.992 0.0156
50 224.739 ± 1.184 0.733 ± 0.0274 2.37 0.989 0.0154

Ultrasonic-vacuum 30 215.460 ± 2.178 0.726 ± 0.0268 2.30 0.989 0.0151

35 207.392 ± 1.481 0.721 ± 0.0259 2.26 0.992 0.0150
40 200.165 ± 1.245 0.715 ± 0.0254 2.24 0.991 0.0149
45 192.940 ± 1.013 0.710 ± 0.02487 2.19 0.986 0.0148
50 185.617 ± 1.748 0.704 ± 0.02411 2.11 0.996 0.0145

7
M. Sharma and K.K. Dash Ultrasonics - Sonochemistry 58 (2019) 104693

Table 5 that helps in swelling and plasticizing the cell membrane. The solution
Weibull model parameters as a function of osmotic dehydration temperature. diffused inside food structure resulted increased in osmotic pressure
Weibull parameters OD process a b χ2 Adj. R2 that caused higher driving force speeding up the transfer of water vapor
from inside to surface resulting in high diffusivity and consequently the
αw AOD 849.582 −0.4308 0.15 0.936 increase in the rate of mass transfer [27]. The moisture diffusivity of
VOD 271.505 −0.2862 0.22 0.992
pineapple at atmospheric pressure was ranging from 1.9 × 10−10 m2/s
UVOD 170.074 −0.2048 0.18 0.957
βw AOD 0.990 −0.0927 0.01 0.937
to 7.3 × 10−10 m2/s in 40 percent sucrose solution in temperature
VOD 0.783 −0.0650 0.03 0.995 range of 40 and 70 °C [32]. The effective moisture and solute
UVOD 0.699 −0.0442 0.13 0.954 diffusivities of green bean during osmotic dehydration in salt
αs AOD 9175.494 −0.8808 039 0.985 solution in temperature 30–50 °C was also varied between
VOD 788.906 −0.3186 0.03 0.910
1.78 × 10−10–2.71 × 10−10 m2/s and 1.12 × 10−10–1.67 × 10−10
UVOD 574.564 −0.2872 0.16 0.991
βs AOD 1.561 −0.1796 0.01 0.984 respectively [57].
VOD 0.952 −0.0664 0.29 0.908 The effective moisture diffusivity and solute diffusivity for VOD
UVOD 0.891 −0.0598 0.11 0.986 process was in the range of 7.30 × 10−10–8.16 × 10−10 m2/s and
3.04 × 10−10–3.66 × 10−10 m2/s respectively. The Dew and Des in the
temperature range of 30–50 °C were increased by 1.62–1.78 and
holding temperature. An analysis was done to specify the above para- 1.28–1.92 times in jamun after applying vacuum pretreatment. The
meters for this model as functions of temperature. Several equations vacuum pretreatment remove the inside gas from the intercellular space
were tested by non-linear regression and the following model (Eq. (14)) of fruit and provide the entrance to sucrose solution through hydro-
was obtained as the best-fitted models to represent scale parameters dynamic transportation that helped in moisture loss and the solute
(αw, αs) and shape parameters (βw, βs) under different treated and uptake in the jamun fruit. It improves the rate of diffusion of water from
untreated condition at different levels of temperature. the fruit to the surrounding osmotic solution and diffusion of the su-
Wp = aT b (14) crose from the solution to the fruit [7]. The major mass transfer rates of
water and solutes by VOD of jamun fruit was caused by pressure
where Wp represent the Weibull model parameters i.e. w , s, w , and s gradients in fruit sample [35]. The effective moisture diffusivity for
for water loss and solid gain respectively. The values of coefficients ‘a’ pulse vacuum (130 mbar, 15 min) treated figs dried in convective oven
and ‘b’ were obtained from model fitting of Weibull parameters with at 55–75 °C was varied between 3.57 × 10−10–10.25 × 10−10 m2/s
respect to temperature in the range of 30 to 50 °C and the obtained [58]. The effective diffusivity of melon fruit under vacuum (100 mbar,
vales were shown in Table 5. The higher coefficient of determination 15 min) for both water and solids ranged from
(R2 > 0.908) and lower chi square (χ2 < 0.29) indicated a good fit of 1.261 × 10−9–1.601 × 10−9 m2/s in sucrose solution of various con-
Weibull model parameters at different temperatures for all the process centrations [33].
conditions (Table 5). The effective moisture diffusivity and solute diffusivity for USVOD
were around 8.53 × 10−10–9.27 × 10−10 m2/s and 3.81–4.39 × 10−10
3.7. Moisture and solute diffusivity during osmotic dehydration m2/s. Jamun treated with USVOD using sucrose solution in temperature
range of 30–50 °C increased the moisture diffusivity by 1.84–2.09 times
The calculated De values for different pre-treatments of osmotic where as solute diffusivity was enhanced by 1.54–2.41 times than the
dehydration in sucrose solution over the temperature range of 30–50 °C samples dehydrated under atmospheric condition. Application of ul-
is shown in Table 6. The transport of moisture and solute during os- trasound caused distortion of cell resulting in intra-particle and extra-
motic dehydration mainly occurs by diffusion through porous tissue particle moisture transfer resistances. The ultrasound waves occurred
structure. During AOD process the effective moisture diffusivity (Dew) compression and expansion to the fruit microscopic channels that
was varied between 4.09 × 10−10 to 5.03 × 10−10 m2/s and solute promote the entrance of mass transfer through inside capillaries from
diffusivity (Des) was varied between 1.58 × 10−10 to 5.03 × 10−10 m2/ fruit tissue and enhance the rate of diffusion [59]. The ultrasound leads
s. It was observed that both Dew and Des were increased with increase in to deformation of cells in the fruit structure that augments water loss
temperature from 30 to 50 °C. Higher temperature enhances the os- and solute diffusion [48]. The effective moisture diffusivity for ultra-
motic pressure difference and hence capillary flow through pores. This sound pretreated pineapples (at different pretreatment time and dif-
can due to an increase in membrane permeability at higher temperature ferent concentration of osmotic solution) dried by forced circulating air

Table 6
Moisture diffusivity, solid diffusivity, and drying efficiency during osmotic dehydration of Black jamun.
Treatment Temperature (°C) Dew Value (×10−10 m2/ Reduced χ2 Adj. R2 Des Value (×10−10 m2/ Reduced χ2 Adj. R2 (Dew/Des)
s) (×10−4) s) (×10−3)

Atmospheric (untreated) 30 4.09 0.381 0.929 1.58 0.053 0.806 2.585

35 4.55 0.379 0.933 1.83 0.049 0.839 2.488
40 4.69 0.379 0.9338 2.16 0.044 0.872 2.171
45 4.88 0.382 0.934 2.47 0.040 0.893 1.9789
50 5.03 0.383 0.935 2.86 0.037 0.911 1.760

Vacuum 30 7.30 0.461 0.930 3.04 0.036 0.917 2.400

35 7.54 0.471 0.929 3.25 0.034 0.924 2.317
40 7.79 0.481 0.9290 3.43 0.034 0.928 2.268
45 8.04 0.489 0.928 3.41 0.034 0.927 2.361
50 8.16 0.495 0.927 3.66 0.033 0.932 2.230

Ultrasonic-vacuum 30 8.53 0.508 0.926 3.81 0.033 0.934 2.238

35 8.65 0.512 0.926 3.96 0.0328 0.936 2.186
40 8.85 0.519 0.925 4.09 0.032 0.937 2.163
45 9.02 0.523 0.925 4.24 0.0327 0.938 2.129
50 9.27 0.533 0.923 4.39 0.0327 0.940 2.111

8
M. Sharma and K.K. Dash
Fig. 4. SEM micrographs of osmotic dried jamun fruit at 50 °C (A) AOD; (B)
VOD; (C) USVOD.
drying at 60 °C was ranged from 7.4 × 10−9 to 13.8 × 10−9 m2/s [60].
Studies on effect of ultrasound assisted osmotic dehydration pretreat-
ment on the convective drying of strawberry showed the effective dif-
fusivities of ultrasound assisted osmotic dehydration – air dried samples
were higher than fresh-air dried samples and effective diffusivity in-
creased with increase in temperature [61]. The higher effective diffu-
sivity at higher temperature was due to triggering effect of temperature
on water and solute molecules to speed up the mass transfer process
from core to the surface of the matrix.
9
Ultrasonics - Sonochemistry 58 (2019) 104693
3.8. The microstructure of osmotically dehydrated jamun fruit
The effect of different pre-treatments in osmotic dehydration and
conditions on the structure of osmotically dehydrated jamun fruit was
observed under SEM (Fig. 4). The SEM images (500× magnification) in
the section of osmotically dehydrated jamun fruit showed distinct dif-
ferences in the microstructure of jamun fruit subjected to different pre-
treatment methods (Fig. 4 (A), (B) and (C)). AOD fruit cell tissue shown
the orderly arranged, well-structured oval pores (Fig. 4A). That oval
shaped pored contained a high degree of cell partitions and intercellular
voids. VOD treated fruit presented a significant change in the structure
at the cellular level where the air was expelled from raw jamun fruit
tissue (Fig. 4B). The intercellular air expulsion affected the pressure
that caused the tissue breakdown inside the pores. Therefore, the os-
motic solution passes from the inside capillaries and filled the inter-
cellular voids of jamun fruit tissue. Mainly in VOD fruit, the higher
amount of water loss and solid uptake to the fruit tissue had taken
through the empty spaces due to hydrodynamic transportation.
Therefore, the interfacial area lowered the stability in the cell mem-
brane and resulted in a decrease in hydrostatic pressure [19]. This re-
sult showed the mass transfer rate enhancement during the vacuum pre-
treatment of osmotic dehydration of jamun fruit. USVOD treated jamun
fruit showed the cellular distortion, tissue breakdown and produced
irregular intercellular spaces. Ultrasound treatment generated acoustic
waves that create the cavitation voids near the fruit surface, the cavi-
tation void showed compression, and expansion phases and then it
collapsed. This process releases out the gases from the intercellular
spaces that might responsible for spongy effect and change the fruit
tissue [18]. The spongy effect enhances the number of microscopic
channels or pores in the fruit surface. SEM images of USVOD processed
jamun fruit further confirmed the channeling effect caused by ultra-
sonic and vacuum combined treatment (Fig. 4C).
4. Conclusion
The research work showed the novel design to enhance the mass
transfer rate and shorten the duration by providing vacuum and ul-
trasonic vacuum treatment to jamun fruit prior to osmotic dehydration
process. Compared with the AOD and VOD, USVOD samples had a
higher value of water loss and solid gain. USVOD was found to improve
the mass transfer in sugar immersion process of jamun fruit. USVOD
caused the removal of a significant amount of water within a short time
period. The higher R2 and lowered χ2 value represented the accept-
ability of Peleg model for equilibrium moisture content and Weibull
model for predicting both moisture and solute fraction during aOD,
VOD and USVOD process. In the microstructure of osmotic dried jamun
fruit, the large oval pores structure were observed in AOD samples as
compare to VOD (small and irregular intercellular spaces) and USVOD
(shrunk cellular structure) samples. Hence, it was finally concluded
simultaneous application of ultrasound and vacuum treatment prior to
osmotic dehydration can enhance the mass transfer rate by lowering the
drying duration and producing good quality products. It could be sug-
gested that this process can also commercially suitable for development
of shelf stable intermediate moisture product infused with osmotic so-
lute and this ultrasonic vacuum osmotic dehydration method could
produce a substantial impact to the food processing industry. Osmotic
dehydrated jamun can be utilised in dairy industry as an ingredient to
develop the fruit enriched custard, yoghurt and ice cream and as bakery
ingredient in developing muffins, fruit pastry and fruitcake.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://
doi.org/10.1016/j.ultsonch.2019.104693.
M. Sharma and K.K. Dash
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