This article was downloaded by: [Queensland University of Technology]

On: 31 October 2014, At: 08:17

Publisher: Taylor & Francis
Informa Ltd Registered in England and Wales Registered Number: 1072954 Registered office: Mortimer House,
37-41 Mortimer Street, London W1T 3JH, UK

Drying Technology: An International Journal

Publication details, including instructions for authors and subscription information:
http://www.tandfonline.com/loi/ldrt20

How to Adapt a Lab-Scale Freeze Dryer for Assessing

Dehydrating Curves at Different Heating Conditions
a a
G. Tribuzi & J. B. Laurindo
a
Department of Chemical and Food Engineering , Federal University of Santa Catarina ,
Florianópolis , Brazil
Published online: 22 May 2014.

To cite this article: G. Tribuzi & J. B. Laurindo (2014) How to Adapt a Lab-Scale Freeze Dryer for Assessing
Dehydrating Curves at Different Heating Conditions, Drying Technology: An International Journal, 32:9, 1119-1124, DOI:
10.1080/07373937.2014.886258

To link to this article: http://dx.doi.org/10.1080/07373937.2014.886258

PLEASE SCROLL DOWN FOR ARTICLE

Taylor & Francis makes every effort to ensure the accuracy of all the information (the “Content”) contained
in the publications on our platform. However, Taylor & Francis, our agents, and our licensors make no
representations or warranties whatsoever as to the accuracy, completeness, or suitability for any purpose of the
Content. Any opinions and views expressed in this publication are the opinions and views of the authors, and
are not the views of or endorsed by Taylor & Francis. The accuracy of the Content should not be relied upon and
should be independently verified with primary sources of information. Taylor and Francis shall not be liable for
any losses, actions, claims, proceedings, demands, costs, expenses, damages, and other liabilities whatsoever
or howsoever caused arising directly or indirectly in connection with, in relation to or arising out of the use of
the Content.

This article may be used for research, teaching, and private study purposes. Any substantial or systematic
reproduction, redistribution, reselling, loan, sub-licensing, systematic supply, or distribution in any
form to anyone is expressly forbidden. Terms & Conditions of access and use can be found at http://
www.tandfonline.com/page/terms-and-conditions
 Drying Technology, 32: 1119–1124, 2014
Copyright # 2014 Taylor & Francis Group, LLC
ISSN: 0737-3937 print=1532-2300 online
DOI: 10.1080/07373937.2014.886258

How to Adapt a Lab-Scale Freeze Dryer for Assessing

Dehydrating Curves at Different Heating Conditions
G. Tribuzi and J. B. Laurindo
Department of Chemical and Food Engineering, Federal University of Santa Catarina,
Florianópolis, Brazil

and biochemical derivative reactions and structural defor-

Downloaded by [Queensland University of Technology] at 08:17 31 October 2014

A laboratory-scale freeze dryer was adapted to allow control of
the heat supply and on-line monitoring of sample weight during dry-
ing under vacuum condition. Several tests were carried out to verify
the reliability of the developed system. The system was also tested
with 10-mm-thick banana slices, obtaining the fruit drying rate, at
different sample holder plate temperatures including 20 and 30 C
as well as an unheated plate. The system presented in this work repre-
sents a low-cost, flexible, and easy-to-assemble piece of equipment
that allows the study and optimization of the freeze drying of foods.
Keywords Banana; Freeze drying; Load cell; On-line weighing;
Rate
INTRODUCTION
Some foods are very sensitive to heat during drying,
which can damage their physicochemical characteristics
and texture. One alternative to classical drying techniques
is the use of a freeze-drying process, in which high retention
of the nutritional and sensorial properties is observed.
Moreover, the frozen water maintains the structural rigidity
during dehydration, avoiding structural collapse and
leading to a highly porous structure.[1,2] The rehydration
process is normally extremely quick, due to the open porous
structure, and the texture of the rehydrated product is very
similar to that of the original product and the original
shape, taste, and aroma are recovered. On the other hand,
the open porous structure makes the dried food fragile to
mechanical stress and oxygen can penetrate easily, causing
oxidation of the lipid compounds.[2] Moreover, the freeze-
drying process presents high energy consumption due to
product freezing and the high vacuum requirements.[3] To
reduce the drying time, heat should be provided to the sam-
ple; however, the amount of heat flux cannot be increased
drastically. Actually, if the temperature is increased above
certain limits, the product will suffer nutrient loss and color
change (nonenzymatic browning) in addition to chemical
Correspondence: J. B. Laurindo, Department of Chemical and
Food Engineering, Federal University of Santa Catarina, EQA=
CTC=UFSC, Florianópolis SC 88040-900, Brazil; E-mail: joao@
enq.ufsc.br
mation of the dried layer.[4] Knowledge of the drying rate
is essential in choosing proper freeze-drying conditions.
There are many studies in the literature on the freeze-drying
kinetics of fruits and vegetables, such as pears[5]; carrot,
capsicum, mushroom[6]; mango[7]; and aloe vera[8]; among
others. However, most of the experimental data obtained
to determine the drying curve during freeze drying were
measured discontinuously, with a limited number of experi-
mental points. An on-line weighing system integrated with
the freeze dryer is really a useful tool for investigating the
drying rate of a material, as reported by Barresi et al.[9]
and Menlik et al.[10] Only a few systems that allow on-line
monitoring of the sample weight during freeze drying have
been discussed in the literature. Rovero et al.[11] developed a
prototype of a capacitive balance able to work under the
extreme physical conditions of the freeze-drying process.
This system is based on a parallel-electrode condenser,
whose capacity in affected by the weight of the samples dur-
ing dehydration. A capacitor acts as the reactive element of
an oscillator circuit and the frequency is measured and con-
verted into a signal. This system presented good reproduci-
bility and uncertainty of the weight measurement of about
0.2 g. On the other hand, the system is particularly sensible
to temperature changes, so the heating system must be iso-
lated from the sample holder plate. Another system that
allows on-line determination of sample weight during freeze
drying was presented by Menlik et al.[10] for determination
of the freeze drying curves of apple. In this system, a load
cell was connected on the bottom of the vacuum chamber
to measure the weight variation during dehydration. An
electrical resistance was used to provide the heat to the
dehydration process. It was installed 4 cm from the sample
holder plate to avoid the contact between the heating sys-
tem and the load cell. In both systems mentioned above
the heat sources are separated from the sample and thus
the heat can be transferred to the samples only by radiation.
In this context, the main objective of this study was to
adapt a laboratory-scale freeze dryer to assess the drying
curves of foods. The device allows fixing different heat
inputs during freeze drying and the related freeze-drying

1119
 1120 TRIBUZI AND LAURINDO
curves. Application of the developed device to the
determination of the freeze-drying curves of banana slices
under different drying conditions is presented.
MATERIALS AND METHODS
Experimental Device
For on-line monitoring of the sample mass during freeze
drying, a commercial laboratory-scale freeze dryer (model
L101, Liotop, São Carlos, Brazil) was modified, with a
weighing system and a heated plate in the vacuum chamber.
A detailed sketch of this device is shown in Fig. 1. The con-
densation system of this freeze dryer maintains the tempera-
ture in the condenser surface at 60  1 C. The vacuum
Downloaded by [Queensland University of Technology] at 08:17 31 October 2014
chamber has two parts: the top, where drying occurs, made
of polymethyl methacrylate (PMMA) with a diameter of
250 mm and volume of 0.0158 m3, and the bottom, made
of stainless steel and with diameter of 220 mm and volume
of 0.008 m3, where condensation due to vapor released by
the samples collects. The top is transparent, allowing visual
observation of the samples during processing. The two
chambers are separated by a perforated plate made of
PMMA that has a structural function. The vacuum is pro-
duced by a vacuum pump (model RC.8D, D.V.P., Vacuum
Technology, Italy), that can reach a final pressure of 0.200 
0.005 mbar within 10 min after the start of the operation.
The modified part of this equipment is the upper chamber
cover and the heating plate. The cover was made of PMMA,
with a diameter of 270 mm and thickness of 22 mm, enough
to support the pressure difference between the inside and out-
side of the vacuum chamber. The hermetic coupling of the
cover was achieved with the use of an O-ring with a diameter
of 4 mm. The cover is used to support the weight measure-
ment system (single-point load cell) and the heating plate that
holds the samples during the freeze-drying operation.
The single-point load cell (model GL, Alfa Instrumen-
tos, Brazil), coupled to a metallic support, has a nominal
capacity of 2 kg and sensitivity of 0.1 g and was connected
to a signal conditioning system (model 3101C, Alfa Instru-
mentos), which is in turn connected to a computer. The
sample holder plate (SHP) is made of aluminum with a
diameter of 210 mm and thickness of 10 mm and was con-
nected to the load cell by a rigid stem (the weight of the
SHP is approximately 1 kg). The plate is heated by an elec-
tric resistance and its temperature is measured by a T-type
thermocouple and controlled by a proportional–integral–
derivative control system. Another T-type thermocouple
connected to a data acquisition system (model 34970A,
Agilent, Malaysia) was used to measure the sample tem-
perature. Both temperature sensors were calibrated against
a mercury-in-glass thermometer (model ASTM, Incoterm,
Brazil) in the temperature range used in the experiments.
Connection of the thermocouple, load cell, and electrical
resistance wires was made with copper screws passing
through the cover, sealed with epoxy resin. The connection
of the electric resistance was separated from the connection
of the measurement system to avoid any possible interference.
Calibration of the load cell was carried out under a
vacuum. The system was tested under freeze-drying operat-
ing conditions, without samples, to assess the operational
behavior of the weighing system; that is, to detect possible
effects of the vacuum on the behavior of the load cell
during the operation. Several freeze-drying cycles of at
least 15 h were carried out at different SHP temperatures.
Experimental Determination on the Freeze-Drying
Kinetics of Banana Slices
Bananas (Musa sapientum L., Prata variety) were
acquired in a local market (Florianópolis, SC, Brazil).
The fruits were selected based on their ripeness, which
was evaluated from the visual appearance, resistance to
penetration using a penetrometer (model FT 327-Ø 8 mm,
Effegi, Italy), and the soluble solid content using a digital
refractometer (model AR200, Reichert, USA). Banana
samples were selected when the penetration test results in
6  1 N and the soluble solid content was 23.1  1.4  Brix.
Selected fruits were manually peeled and cut into slices of
10 mm thickness, avoiding the edges of the fruit where the
diameter of the slice is reduced. Before and after each
freeze-drying process, the moisture content of the samples
was determined in triplicate by the gravimetric method.[12]
Before freeze drying, 120  2 g of banana slices was
frozen by placing the samples on a polyester film in direct
contact with the condensation surface for 2 h, until it
reached a core temperature of 50  2 C, as measured by
a thermocouple. Frozen samples were quickly transferred
to the SHP connected to the load cell, the system was closed,
and the vacuum pump was started. After 10 min the cham-
ber pressure reached an operating pressure of about 0.2
mbar. After 15 h of drying, the vacuum pump was switched
off and atmospheric pressure was restored. The samples
were removed and carefully weighed to verify the reliability
of the on-line weighing system, and the final moisture
content was determined. The temperature of the SHP
during the freeze-drying process was set at three levels: 20
and 30 C and unheated (in this case the temperature was
not constant). The experiments were performed in triplicate
for each SHP condition. The average value of the moisture
content (before and after processing) and the sample weight
curves were used to calculate the moisture content (dry
basis) during the process and to plot the drying curves
related to each freeze-drying process. To compare the data
obtained from the developed system with those obtained by
removing the samples from the freeze dryer, experiments
were carried out in the unheated condition. Samples
were removed from the vacuum chamber after 1, 2, 3, 4,
6, 10, and 15 h of drying. To avoid the interference that
interruption of the process could affect the results, a
 ADAPTING A LAB-SCALE FREEZE DRYER 1121
Downloaded by [Queensland University of Technology] at 08:17 31 October 2014

FIG. 1. Experimental device used to investigate the kinetics of freeze drying.

destructive approach was used, starting from frozen sam-
ples for each experimental point studied. The Savitz-Golay
Matlab function was fitted to each experimental drying
curve in order to smooth the data and perform the deriva-
tives that allowed calculation of the drying rate curves.
RESULTS AND DISCUSSION
Validation of the On-Line Weighing System
Several freeze-drying blank tests were run at different
temperatures to verify the reliability of the weighing system
installed in the vacuum chamber. Figure 2a shows a blank
test of 15 h with the SHP with a 123.5-g metal sample,
and Fig. 2b shows the results for the SHP with no sample.
The pressure in the vacuum chamber dropped to 0.2 mbar
in about 10 min. In this period, the weighing system showed
a decrease of about 1.2 g, probably due to the air flow
caused by the chamber evacuation. Once operating pressure
was reached in the vacuum chamber and the air flux
decreased, the system quickly returned to the original
weight. During the 15-h test, the maximum variation
 1122 TRIBUZI AND LAURINDO
recorded by the weighing system was 0.5 g, showing that
the load cell behavior was not significantly affected by the
vacuum condition. Considering that in this work 120 g of
fruit was used, a weight variation of approximately 80 g
during the whole drying process was expected. Therefore,
the maximum error for the final weight was approximately
0.6%. Moreover, the vibration of the recorded weight,
which could cause some lack of accuracy, can be easily
removed by applying a smoothing filter on the curve before
performing the data analysis. Because the capacity of the
load cell was 2 kg (weight of the SHP with samples), it is
possible to increase the amount of fruit sample, thus
increasing the amount of sublimated water and decreasing
the relative error of the measurement. Moreover, the use
Downloaded by [Queensland University of Technology] at 08:17 31 October 2014
of a load cell in this kind of device is very flexible, because
load cells with different capacities and sensitivities are
available.
Rovero et al.[11] reported that the reliability of a weighing
system can be affected by its temperature. Thus, to verify
the variation of the temperature of the load cell during
processing, the thermocouple tip (Fig. 1, component 7)
was fixed to the base of the load cell and a complete freeze-
drying cycle was carried out. The temperature of the load
cell reported in Fig. 2c remained stable at the 20  2 C
during the whole process. The variation of 2 C could be
FIG. 2. Validation of the weighing system installed in the freeze dryer
vacuum chamber, with an SHP (a) with a 123.5-g metal sample and (b)
without samples. (c) Load cell temperature during the test.
ascribed to the variability in the room temperature and
radiation heat transfer effects. The stability of the tempera-
ture of the load cell could be explained considering that it
was positioned 30 cm from the condenser and 15 cm from
the SHP, enough to avoid any influence on the load cell
temperature. This result is an important advantage
with respect to other weighing systems reported in the
literature.[8,10,11] Other important parameters influence the
accuracy of the measured weight, such as the electrical
instability and vibrations transmitted to the system. There-
fore, if the electrical network presents instabilities, the
weighing system should be connected to an electrical
stabilizer and the freeze dryer should be placed far from
the vacuum pump or other sources of vibration.
Experimental Freeze-Drying Curves
Figure 3 shows the freeze-drying curves for banana slices
recorded at different SHP temperatures (20 C, 30 C, and
unheated). The experimental data recorded by the on-line
system presented very good reproducibility, especially when
the SHP was set at 20 and 30 C. The curves related to the
unheated condition had a greater influence of the room
temperature and caused a small differences among the
curves due to radiation heat transfer.
The SHP temperature significantly affected the drying
curves. The moisture content of about 0.1 g water=g dry
solids was reached after 10.45, 12.33, and 14.80 h, respect-
ively, for temperatures of 30 and 20 C and the unheated
condition. These results indicate a reduction of about 30%
in the drying time when the SHP was heated to 30 C
compared to the unheated condition. This reduction was
approximately 16% when the temperature of the SHP was
20 C. These results show that higher plate temperatures
caused significant reductions in the drying time due to the
energy supplied for the ice sublimation and for desorption
of bound water. It is important to find the maximum tem-
perature at which the product does not present any sensible
degradation of its sensory and nutritional quality. In a first
approximation, the operating temperature of 20 C could
be used in the freeze-drying process for a given product.
Figure 3 also shows the data obtained by weighing the
banana slices discontinuously, interrupting the process and
removing the samples from the vacuum chamber. These
results present the same behavior as those obtained by the
on-line weighing system, confirming that the results obtained
by the developed system were acceptable. On the other hand,
the discontinuous approach presents some disadvantage
with respect to the on-line weighing system, such as the small
number of experimental points obtained and the time
required to obtain one drying curve, considering that the
experiment must be restarted for each experimental point.
Figures 4a and 4b show, respectively, the temperature
profiles of the SHP and the samples during freeze
drying. The sample temperatures (Fig. 4b) were recorded
 ADAPTING A LAB-SCALE FREEZE DRYER 1123

by inserting the thermocouple tip into the center of the

banana slice. Thus, the recorded temperature should be
considered as an average temperature. The behavior of
the sample temperature during freeze drying indicates the
drying rate behavior.
The drying rates against time for the three investigated
conditions are shown in Fig. 5. Two falling rate periods
were observed during the freeze-drying processes. The
drying rate fell strongly during the first 3 h of processing,
whereas the second falling rate period has a lower slope.
Classically, the first phase of a freeze-drying process is con-
sidered to be governed by two transport mechanisms: the
heat transfer that supplies the latent heat of sublimation
of ice (approximately 2,805 kJ=kg, at temperatures ranging
Downloaded by [Queensland University of Technology] at 08:17 31 October 2014

from 21 to 30 C) and the mass transfer of the water

vapor from the sublimation surface through the dried

FIG. 3. Freeze-drying curves of banana slices at sample holder plate

temperatures of 20 and 30 C and an unheated condition (in triplicate)
obtained by the on-line weighing system (solid and dashed lines). ^
represent the data obtained by removing the samples at different times FIG. 4. Temperature of the (a) sample holder plate and of (b) samples
(unheated condition). during freeze drying of banana slices.
 1124 TRIBUZI AND LAURINDO
FIG. 5. Freeze-drying rate as function of time of banana slices at sample
holder plate temperatures of 20 and 30 C and unheated.
Downloaded by [Queensland University of Technology] at 08:17 31 October 2014
product, coupled to its transfer to the drying chamber and
to the condenser.[13] The second drying phase involves the
removal of bound water that did not freeze (about
10–35% of the initial moisture content, depending on the
characteristics of the product and on the velocity of the
freezing stage). In a real process with foods, this second
phase is not totally independent of the first; a small amount
of bound water is removed by desorption from the dried
layer during the primary drying phase.[4] In the freeze-
drying process studied in this article, the latent heat
required for ice sublimation was provided by conduction
(SHP) and radiation (SHP and environment). As drying
process proceeded, a drying front formed from the sample
surface, which behaved as an insulating material, reducing
the contribution of the radiation heat transfer on the heat
transfer to the sublimation front.
These results, assessed with the weighing system adapted
to the freeze dryer, showed the usefulness of this device for
investigating the different conditions of dehydration of a
given food.
CONCLUDING REMARKS
The on-line weighing system adapted to a lab-scale freeze
dryer is a useful tool for investigating freeze-drying
processes. This is a low-cost, flexible, and easy-to-assemble
device, adaptable to preexisting freeze dryers. Moreover,
the use of a load cell as the weighing system offers the
possibility of changing the sensibility and the capacity of
the weighing system, adapting the system to different needs.
On the other hand, the heated sample holder plate allows
investigating the influence of the temperature on the
freeze-drying rate and process optimization.
FUNDING
The authors thank FINEP=Brazil and CAPES=Brazil
for financial support.
REFERENCES
1. Ibarz, A.; Barbosa-Cánovas, B. Unit Operations in Food Engineering;
CRC Press: Boca Raton, FL, 2003.
2. Ratti, C. Freeze and vacuum drying of foods. In: Drying Technologies in
Food Processing; Chen, X.; Mujumdar, A., Eds.; Blackwell Publishing:
Singapore, 2008; 225–243.
3. Singh, R.; Heldman, D. Introduction to Food Engineering, 4th ed.;
Academic Press: London, 2009.
4. Liapis, A.; Bruttini, R. Freeze drying. In Handbook of Industrial
Drying, 3rd ed.; Mujumdar, A., Ed.; CRC Press: Boca Raton, FL,
2006; 257–271.
5. Guiné, R.D. Influence of drying method on density and porosity of
pear. Food and Bioproducts Processing 2006, 84(C3), 179–185.
6. George, J.; Datta, A. Development and validation of heat and mass
transfer models for freeze drying of vegetable slices. Journal of Food
Engineering 2002, 52(1), 89–93.
7. Chakraborty, R.; Saha, A.; Bhattacharya, P. Modeling and simula-
tion of parametric sensitivity in primary freeze drying of foodstuffs.
Separation and Purification Technology 2006, 49(3), 258–263.
8. Chakraborty, R.; Bera, M.; Mukhopadhyay, P.; Bhattacharya, P.
Prediction of optimal conditions of infrared assisted freeze drying
of aloe vera (Aloe barbadensis) using response surface methodology.
Separation and Purification Technology 2011, 80(2), 375–384.
9. Barresi, A.; Pisano, R.; FIssore, D.; Rasetto, V.; Velardi, S.; Vallan,
A.; Parvis, M.; Galan, M. Monitoring of the primary drying of a
lyophilization process in vials. Chemical Engineering and Processing:
Process Intensification 2009, 48(1), 408–423.
10. Menlik, T.; Özdemir, M.; Kirmaci, V. Determination of freeze drying
behaviors of apples by artificial neural network. Expert Systems with
Applications 2010, 37, 7669–7677.
11. Rovero, G.; Ghio, S.; Barresi, A. Development of a prototype capaci-
tive balance for freezee-drying studies. Chemical Engineering Science
2001, 56, 3575–3584.
12. Association of Official Analytical Chemists. Official Methods of
Analysis, 17th ed.; Association of Official Analytical Chemists:
Washington, DC, 2000.
13. Oetjen, G.; Haseley, P. Freeze Drying; Wiley-VCH Verlag GmbH and
Co. KGaA: Weinheim, Germany, 2004.