Chemical Engineering Communications

ISSN: 0098-6445 (Print) 1563-5201 (Online) Journal homepage: https://www.tandfonline.com/loi/gcec20

A Simple Data Processing Approach for Drying

Kinetics Experiments

Luís M. M. N. Castro & M. N. Coelho Pinheiro

To cite this article: Luís M. M. N. Castro & M. N. Coelho Pinheiro (2016) A Simple Data
Processing Approach for Drying Kinetics Experiments, Chemical Engineering Communications,
203:2, 258-269, DOI: 10.1080/00986445.2014.993468

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Chemical Engineering Communications, 203:258–269, 2016
Copyright # Taylor & Francis Group, LLC
ISSN: 0098-6445 print/1563-5201 online
DOI: 10.1080/00986445.2014.993468

A Simple Data Processing Approach for Drying

Kinetics Experiments
LUÍS M. M. N. CASTRO1,2 and M. N. COELHO PINHEIRO1,3
1
Departamento de Engenharia Quı́mica e Biológica, Instituto Superior de Engenharia do Instituto Politécnico de Coimbra,
Rua Pedro Nunes, Quinta da Nora, Coimbra, Portugal
2
GERST–DCE=FST, Group on Environment, Reaction, Separation and Thermodynamics, Department of Chemical Engineering,
Faculty of Sciences and Technology, University of Coimbra, Rua Sı́lvio Lima, Pólo II, Coimbra, Portugal
3
Centro de Estudos de Fenómenos de Transporte, Faculdade de Engenharia da Universidade do Porto, Rua Dr. Roberto Frias,
Porto, Portugal

A simple mathematical approach is proposed to be applied to drying kinetics raw data processing. The data collected in a drying
experiment of powder cork under constant air drying conditions served as case study to present the methodology. Two functions
(linear and third-degree polynomial) were used to fit solid moisture content in the constant drying rate and the falling rate periods.
The drying rate curve was obtained by differentiation and the time at which the drying rate period’s transition occurs was
determined iteratively until virtually continuous functions were achieved. The critical moisture content was easily identified and
two falling drying rate periods were detected.
The powder cork moisture decrease was also used to test several semiempirical models available in the literature. The Logarithmic,
Midilli, and Page Modified I models were the ones that revealed the best correlations performance. When the methodology proposed
was applied using these models, the critical moisture content was underpredicted.
The effective moisture diffusivity and the activation energy were also obtained for powder cork after the proposed mathematical
approach has been applied on the raw data obtained in experiments performed at different air drying temperatures.
Keywords: Constant drying conditions; Drying kinetics; Drying rate curve; Effective moisture diffusivity; Powder cork; Raw
data processing

Introduction The raw data is commonly in the form of solid moisture

Scaleup from laboratory=pilot experiments to a real dryer
requires a great volume of data obtained under different
operation conditions. Rapid and efficient methodologies
for processing data collected during drying kinetics experi-
ments are essential for the scaleup phase.
As referred by Kemp et al. (2001), drying kinetics data
may be obtained using different methodologies: periodic
sampling (or weighing), continuous weighing, and intermit-
tent weighing. Besides these direct methods, an indirect
method can also be used, where the humidity of the air-
stream at the drying chamber outlet is measured and then
from back calculation the water evaporation rate from the
solid is obtained (Kemp et al., 2001).
Address correspondence to M. N. Coelho Pinheiro,
Departamento de Engenharia Quı́mica e Biológica, Instituto
Superior de Engenharia do Instituto Politécnico de Coimbra,
Rua Pedro Nunes, Quinta da Nora, 3030-199 Coimbra,
Portugal. E-mail: mnazare@isec.pt
Color versions of one or more of the figures in the article
can be found online at www.tandfonline.com/gcec.
content calculated from weighing measurements. When data
acquisition is used in the drying experiments for continuous
wet solid weighing a large volume of information is available
for processing. Useful curves are obtained directly from data
and the drying rate curve (or Krischer curve) obtained after
mathematical treatment are useful curves, that are the basis
for the scaling up process.
Several approaches for processing drying kinetics raw
data are compiled in the work of Kemp et al. (2001). Raw
data could be used directly, with or without removing spuri-
ous values, or applying an averaging or smoothing method
over adjacent values. Additionally, the drying curve could
be fitted to an equation with theoretical support or simply
using the best fit curve to correlate data. The drying
rate curve is derived from the moisture curve using finite
differences or differentiating the fitted curve. Commonly,
the moisture curve is smoother than the drying rate curve
which presents random values typically for very low drying
rates. An important point outlined by Kemp et al. (2001)
is that raw data should not be discarded but always used
as a comparison for the smoothed curves processed.
A simple mathematical approach is proposed in this
study to deal with raw data acquired during drying kinetic
Drying Kinetics Experiments
experiments. The approach is applied to data collected dur-
ing a constant drying conditions experiment performed to
dry wet powder cork.
Cork is the bark of a special tree, the cork oak (Quercus
suber L), that grows in the Mediterranean regions, and parti-
cularly in Portugal, which is the world leader of cork oak
forests (more than 736 thousand hectares, 34% of total forest
area) with an average annual cork production of 100,000
metric ton (49.6% of worldwide production) (APCOR,
2013). Portugal is also the world leader in the cork sector
in terms of exports (in 2012, it took a share of 64.7%), which
represents 1.6% of the Industrial Gross Value Added of the
country (APCOR, 2013).
In the cork sector, the most important and prized product
is the cork stopper for the wine industry, which represents
68.4% by value, of the sector production (2012 data,
APCOR, 2013).
To produce cork stoppers, several mechanical operations
are required to transform the cork plank into the final product.
During this process, cork powder is produced, a solid waste
that is usually valorized as fuel in the biomass boilers or used
as filler in the production of colmated cork stoppers (natural
cork stoppers with their pores sealed with cork powder).
During the cork stoppers fabrication, the product
undergoes several drying operations: drying of cork planks
after harvesting and after the cork cooking process, drying
of cork stoppers after washing procedures and surface
treatment, and drying of cork powder to be used in the
production of colmated natural cork stoppers.
Over recent decades, research studies on drying food
products, such as fruit and vegetables, have been published
on a large scale. However, scientific publications concerning
drying studies of natural products such as cork are still
rather scarce, despite the importance of this unit operation
to the cork sector.
In fact, just recently a few studies of the drying process of
natural cork slabs as the main objective have been published:
Carpintero et al. (2014) evaluated the feasibility of applying
a kiln drying technique to cork planks and compared this
procedure with the traditional drying process of cork slabs;
Costa and Pereira (2013) studied the drying process of raw
cork planks in a cork pile in the field, under natural sun
drying conditions. Before that, Belghit and Bennis (2009)
studied the drying kinetics of small cork slabs in a laboratory
dryer with controlled conditions and Magalhães and
Pinho (2008) characterized the drying performance of cork
stoppers in a laboratory scale spouted bed under several
operating conditions.
The main contribution of this study is to provide the
scientific=industrial community with a simple methodology
for the processing of drying kinetics data. The mathematical
approach proposed is easy to implement and has revealed to
be efficient in the identification of the different convective
drying periods. Moreover, the main purpose of this work
contributes also to diminish the lack of information
available about cork powder drying kinetics and drying
parameters, since this natural product was used as case study
to exemplify the methodology described.
259
Materials and Methods
Materials and Sample Preparation
The cork powder used in the experiments was produced
during the transformation of cork planks into stoppers
and it was obtained by courtesy from a Portuguese cork
stoppers industry. The cork powder was stored in a bag until
it was been used in the drying experiment. Physical charac-
teristics of the powder, like particle size and size distribution,
specific surface area, and bulk density were evaluated.
Because the solid material used in the drying process is in
powdered form, the sample encompasses a collection of fine
particles and its volume includes the solid material volume,
the pores volume and the interparticle void volume. Follow-
ing the ASTM (American Society for Testing and Materials)
definition, this is designated by bulk volume and gives rise to
the bulk density. The bulk volume depends on the size and
shape of the individual fine particles and also on the level
the particles were packed. The obtained value for the bulk
powder density without packing was (67.3  0.9) kg=m3.
The characterization of the cork powder’s size
distribution was obtained by (wet) laser diffraction (Malvern
Mastersizer 3000 with the Hydro MV dispersion unit).
A suspension of powder in ethanol was prepared for the
measurement. The analysis was performed using the
Fraunhofer scattering model. The volume median diameter
obtained was 79.3 mm. Two others common percentiles,
10% and 90%, were also reported from the analysis with
values of 16.4 and 270 mm, respectively. The volume moment
mean, which reflects the size of the particles constituting the
bulk of the sample volume, is also a relevant parameter
for the powder cork sample and have a value of 116 mm.
A specific surface area of 184.1 m2=kg was obtained from
the laser diffraction analysis.
The sample preparation started with the cork powder
immersion in water during 24 h. Then, the cork was
separated from the excess of water by filtration and trans-
ferred to the tray. In this step, care was taken to guarantee
a uniform thickness (about 0.01 m) of wet solid material in
the tray before placing it into the drying chamber.
Experimental Procedure and Conditions
The drying kinetics experiments of cork powder were
performed in a laboratory scale tray dryer (Armfield Ltd,
model UOP8) which is schematically presented in Figure 1.
The drying unit consists of a floor-standing tunnel equipped
with an axial flow fan and heating elements near the
entrance. The drying chamber, which might be accessed by
a transparent door, contains a metallic structure suspended
from a balance mounted outside on the top of the dryer
body. The metallic structure has four shelves to accommo-
date four trays. Only one tray in the upper shelf was used
in this experimental work. The tray (0.275 m  0.185 m and
0.015 m depth) is made of stainless steel.
The fan with adjustable speed gives a range of air
velocities from 0.3 to 1.8 m=s in the drying chamber.
A power control adjusts the heater power up to 3 kW varying
260 L. M. M. N. Castro and M. N. Coelho Pinheiro

Table I. Initial characteristics of wet cork powder and mean

airstream drying parameters measured during the experiment
Xi (kgwater=kgdry solid) 7.12

Solid load (kgwet solid) 0.09500

Air at the dryer Temperature ( C) 19.98  0.23
entrance Humidity (% relative) 57.19  1.44
Air downstream the Temperature ( C) 45.52  0.27
drying chamber Humidity (% relative) 13.90  0.29
Air upstream the Temperature ( C) 42.94  0.28
drying chamber Humidity (% relative) 15.84  0.79
Mean air velocity (m=s) 0.77  0.01

Fig. 1. Sketch of the tray dryer used in the drying kinetics

experiments of cork powder. 1. Fan speed controller; 2. heater
power controller; 3. balance; 4. upstream location of the
humidity=temperature sensor; 5. trays; 6. downstream location
of the humidity=temperature sensor.
the temperature of the airstream up to 80 C (for smaller air
flow rates).
A digital balance OHAUS (Adventurer Pro AV8101)
with a maximum load of 8.1 kg and an accuracy of measure-
ment of 0.1 g was used. Two holes in the tunnel, located
upstream and downstream of the drying chamber, were used
to insert two humidity=temperature sensors (HigroClip2
from Rotronic) which are external probes of the data logger
HygroLog HL-NT3. Another HigroClip2 probe measures
the ambient humidity and temperature. The readings from
the balance and humidity=temperature probes were acquired
(with an acquisition frequency of 0.025 Hz (period of 40 s)),
using the HiperTerminal emulator for the connection to
a computer.
The velocity of the airstream at the outlet of the tunnel
was measured with an anemometer from Airflow Develop-
ments (LCA6000). In order to have a representative value
for the velocity, the anemometer was located at each quarter
of the tunnel cross section and the local velocity value was
measured. An average value was calculated to represent
a mean value of the air velocity over the entire cross section
at the tunnel outlet. The velocity of the airstream flowing
over the upper surface of the tray in the drying chamber
was calculated from the continuity principle.
The initial moisture content of the cork powder was
obtained by drying a small amount of the wet solid in
an oven at 104  1 C followed by cooling in a desiccator
containing silica gel to balance temperature and weighing.
The cycle of drying, cooling with desiccating, and weighing
was repeated until a constant weight was obtained. A high
precision digital balance (Mettler Toledo PB3002) with an
accuracy of 0.0001 g was used in this determination.
The fan speed and the heat power control were selected in
order to have the air conditions (flow rate and temperature)
required to dry the cork powder. At the beginning of the
experiment, the temperature and humidity at the airstream
downstream and upstream of the drying chamber were
periodically measured in order to verify when the steady-state
conditions will be reached. An equal procedure was applied to
the air flow rate.
Once the steady state conditions were reached, the wet
solid already in the tray was placed in the drying chamber
and its weight started to be acquired during the drying.
During the experiment, the air conditions were measured
in order to verify that the airstream humidity and flow rate
were virtually constant and also to have an average value to
represent the drying air conditions. Table I shows the initial
moisture content of the wet powder cork to be dried, the
humidity and temperature average values for the air at three
different locations (entrance of the tunnel dryer, down-
stream, and upstream of the drying chamber), and the mean
air velocity at the tunnel dryer outlet. The dispersion from
the average values that occur during the experiment are
depicted in Table I by the standard deviations associated
to the variables.
The drying process was interrupted when the solid
weight remained constant for a considerable period of time,
indicating that the equilibrium moisture was reached. At the
end of the drying process, it was not noticed appreciable
shrinkage of the sample.
In addition to the experiment described in detail that will
be used as case study to present the proposed mathematical
methodology for processing drying kinetics data, others
experiments at different air drying temperatures were carried
out. The main purpose of these experiments was to obtain
two important parameters for drying processes: the effective
moisture diffusivity and the activation energy.
Moisture Content Curve
With the weight of the wet cork powder acquired during the
drying process, the moisture content of the solid (X) was
obtained in a dry basis
W  Ws
X¼ ð1Þ
Ws
where W is the weight of the wet solid at instant t and Ws is
the weight of the dry solid. The value of Ws was calculated
with the weight of the wet powder cork at instant t ¼ 0, Wi,
and the initial moisture content Xi obtained from the sample
dried in the oven until constant weight (as referred before) as
Wi
Ws ¼ ð2Þ
1 þ Xi
Drying Kinetics Experiments
The moisture content curve was obtained after the compu-
tation of X for all data acquired during the experiment.
Drying Rate Curve
The convective drying rate (R) as a function of moisture
content is derived from the drying curve and this is usually
done by applying a finite difference method (Mujumdar,
2006) to have
Ws dX Ws DX
R¼ ffi ð3Þ
A dt A Dt
As referred before, every 40 s a value of the wet solid weight
was acquired by the data acquisition system. As a result, a
large quantity of data was obtained (see plot in Figure 2)
which can include random scatter due, for example, to the
uncertainty associated to the mass measured by the digital
balance or due to vibration of the tray with the wet solid
caused by the airstream. In order to reduce these uncertain-
ties, time intervals of 200 s were used to apply Equation (3)
and calculate the moisture content change of the wet solid
during the drying process. With this procedure, the balance
uncertainty becomes insignificant relative to the weight
change in the amount of wet cork powder, at least over
a large period of the total drying process, but a considerable
amount of raw data was not used in the calculations.
The work of Kemp et al. (2001), as referred before, is
a useful tool for experimental drying kinetics data processing
because the authors review the methods usually applied. The
authors referred that the more irregular the moisture content
versus time curve is, more smoothing techniques should be
used before trying to obtain the drying rate curve. The
moisture content curve is irregular when the signal to noise
ratio is low, which is observed when an external periodic
weighing sample procedure is used or a small mass of wet
solid is dried. High hot air flow rates could also cause
Fig. 2. Moisture content curve for the experiment performed
with wet cork powder. Air drying conditions: 45.52  0.27 C
and 0.77  0.01 m=s.
261
periodic oscillations (noise) in the weighing data acquired
continuously or intermittently due to vibrations in the
dryer trays. Care was taken to avoid sources of noise in
the weighing data acquired during the drying experiments
performed. Figure 2 shows that the moisture content curve
obtained in this work for the drying process of cork powder
is very smooth and no further smoothing techniques are
necessary. In the next section, a mathematical approach will
be described in order to obtain the drying rate curve directly
from the moisture content curve with a smoothing appear-
ance and without discarding the raw data.
Mathematical Approach
Very often from the decrease of moisture content during
the drying period, it is evident (after a small unsteady state
period in which the solid adjusts its temperature to the
airstream conditions) the existence of two characteristic
periods of convective drying: the constant drying rate period
and the falling drying rate period.
If the equations fitted to both periods are X ¼ at þ b for
the constant drying rate period and X ¼ ct3 þ dt2 þ et þ f
for the falling drying rate period, the correspondent
equations for the convective drying rates are obtained
applying Equation (3). The former period will be described
by a constant value of drying rate, Rc, defined as
Ws dX Ws
Rc ¼  ¼ a ð4Þ
A dt A
and the falling rate period is given by
Ws dX Ws  2 
R¼ ¼ 3c t þ 2d t þ e ð5Þ
A dt A
For instant tc corresponding to the instant where critical
moisture, Xc, was reached both values of the drying rate
determined by the Equations (4) and (5) must be equal,
which allow the determination of the critical time from the
next equation:
pffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
2d þ 4d 2  12cðe  aÞ
tc ¼ ð6Þ
6c
The transition between both drying rate periods was
obtained iteratively. At the beginning of the iterative pro-
cedure, the transition between the two periods was visually
determined. Afterwards, a new estimate of tc using Equation
(6) was possible from the best fit equations obtained and this
procedure continued until consecutive values of tc do not
differ significantly. Finally, after optimization of the fitted
equations for each drying period the convective drying rate
curve was obtained using Equations (4) and (5).
The values of R were calculated for all the instants t
correspondent to the acquisition rate used in the experiments,
which means that intervals of time of 40 s were used.
262 L. M. M. N. Castro and M. N. Coelho Pinheiro

The Semiempirical Models Describing Drying Kinetics Table II. Semiempirical models used in this experimental study
to model cork powder drying kinetics
The models available for convective drying processes
were developed with two different approaches. Theoretical Model Equation
models based on the mathematical description of the
physical phenomena driving heat and mass transfer, with Lewis MR ¼ expðktÞ Equation ð7Þ
or without solid shrinkage effects, and empirical models Page MR ¼ expðktn Þ Equation ð8Þ
based on drying kinetics observations. Empirical models
became widespread during recent decades because the Handerson & MR ¼ A expðktÞ Equation ð9Þ
application of theoretical models had been hindered by the Pabis
lack of physical transport parameters as effective moisture Logarithmic MR ¼ A expðktÞ þ B Equation ð10Þ
diffusivity in the solid and thermal conductivity. However,
Two-terms MR ¼ A expðk0 tÞ þ B
a large amount of data is required to obtain empirical
models with carefully designed experiments carried out at expðk1 tÞ Equation ð11Þ
different temperature and air velocity conditions.
The time-consuming procedure to obtain empirical and Wang & Singh MR ¼ 1 þ k0 t þ k1 t2 Equation ð12Þ
semiempirical (or semitheoretical) models has been used to n
Modified Page I MR ¼ exp½ðt=kÞ  Equation ð13Þ
describe food drying processes and several models are now
n
available. According to Erbay and Icier (2009), the semiem- Midilli MR ¼ A expðkt Þ þ Bt Equation ð14Þ
pirical models can be divided into two major classes,
depending of the law through which they were derived: Verma MR ¼ A expðktÞ þ ð1  AÞ
Newton’s law of cooling or Fick’s second law for diffusion. expðgtÞ Equation ð15Þ
The models derived from Newton’s law of cooling include
the Lewis model (Lewis, 1921) (or Newton model) and the
Page model (Page, 1949). The first model was derived stating An extra term to the Henderson & Pabis model, which
that during the falling drying rate period of hygroscopic is time dependent was proposed by Midilli et al. (2002)
porous materials, the moisture content decreases with a rate (Equation (14)). A model with two exponential terms,
which is proportional to the existing driving force for moist- expressed by the Equation (15), was suggested by Verma
ure transfer. Constant air drying conditions are assumed to (1989).
obtain Equation (7) representing the Lewis model. The Page The semitheoretical models presented in Table II were
model, derived in 1949, is a modification of the Lewis model used to correlate the experimental data obtained during cork
which introduced a new dimensionless empirical parameter, powder drying at constant air drying conditions. The equa-
shown in Equation (8), in order to obtain a more accurate tions presented in Table II disregard the initial unsteady
model for drying shelled corns. state period and are more suitable to describe drying kinetics
The models obtained from Fick’s second law for diffusion during the falling rate period (Jayas et al., 1990; Sander,
include Handerson & Pabis, Logarithmic, Two-terms, Wang 2007). The independent variable, the moisture ratio (MR),
& Singh, and Midilli models, among others. The Handerson in the model equations represents the dimensionless solid
& Pabis model (Equation (9)) was obtained from the moisture content defined as:
analytical solution of the second Fick’s law for an infinite
slab (Crank, 1975) taking the drying time sufficiently long. X  Xe
In these conditions only the first term of the infinite series MR ¼ ð16Þ
Xi  Xe
of terms can be considered without significant loss of
accuracy. Later, Chandra and Singh (1995) proposed where Xe is the equilibrium moisture in the solid and Xi is its
a modification to the Handerson & Pabis model, including initial moisture content, as referred before.
a new empirical constant. This model (Equation (10)) is
known as Logarithmic model. Henderson (1974) proposed Table III. Different values of the moisture content of the solid
to use two terms of the infinite series of terms from Fick’s during drying (Xi, Xc, Xd, and Xe), the value of the constant
second law solution for modeling grain drying kinetics. drying rate Rc, and the duration of both drying periods,
The Equation (11) obtained is known as Two-terms model. for the experiment performed with the wet cork powder. Air
Wang and Singh (1978) presented an equation to describe drying conditions: 45.52  0.27 C and 0.77  0.01 m=s
a single layer drying kinetics of rough rice, which is known
as the Wang & Singh model (Equation (12)). Moisture content (X) Xi 7.12
Overhults and his team proposed in 1973 a modification kgwater=kgdry solid Xc 1.84
to the Page model when they wanted to describe the drying Xd 0.88
process of soybeans. The proposed equation is presented in Xe 0.16
Table III as Equation (13). Later, others modifications to Constant drying rate (Rc) 10.03
Page model were proposed by different authors and for that gwater=(min m2)
reason the modification proposed originally by Overhults Period duration min Constant drying rate 118.0
et al. (1973) is referred as Modified Page I. Falling drying rate 80.7
Drying Kinetics Experiments
A powerful statistical technique, the nonlinear regression,
was used to correlate data obtained in the drying experiment
of powder cork with the models presented in Table II. The
Regression add-on module of SPSS Statistics 21 provides
this technique and uses an iterative estimation algorithm
proposed and implemented in NPSOL1 by Gill, Murray,
Saunders and Wright to estimate the model parameters. This
software was used and for each model it gives the optimized
parameters estimations and also provides statistics in order
to analyze the differences between data and predictions
using the analysis of variance (ANOVA) technique. Differ-
ent statistical methods are applied to validate the models,
but the correlation coefficient (r2), the reduced chi-square
test (v2), and the root mean square error (RMSE) are gener-
ally accepted as good criterions to select the best model.
A value of r2 close to unity and a value of v2 and RMSE very
low (close to zero) indicate that a good fit exists between data
and predictions obtained from the model (Midilli et al., 2002;
Akpinar et al., 2003; Wang et al., 2007; Dissa et al., 2011;
Tunde-Akintunde, 2011; Demiray and Tulek, 2012).
Effective Moisture Diffusivity and Activation Energy
The effective moisture diffusivity and the activation energy
associated to the moisture transfer process are key para-
meters in drying modeling and dryer design. These drying
parameters can be found in the literature for a great variety
of materials: hydrogel films for pharmaceutical purposes
(Wong et al. 2014; Silva and Coelho Pinheiro, 2013),
fruits (Samadi and Loghmanieh, 2013; Ramos et al., 2010;
Xanthopoulos et al., 2009; Doymaz, 2008), vegetables (Ajala
et al., 2012; Zielinska and Markowski, 2010), agriculture
wastes (Chen et al., 2012a; Vega-Gálvez et al., 2010), and
forest products (Du et al., 2014; Chen et al., 2012b), etc.
Considering that during the falling rate period the
moisture transfer mechanism in the drying process is
governed by the Fick’s second law, it can be described by
@MR  
¼ r Deff ðrMRÞ ð17Þ
@t
where Deff is the effective moisture diffusivity. As referred by
Chen (2007) this parameter is used in Equation (17) with a
broader meaning in opposition to the fundamental concept
of liquid diffusion coefficient. In fact, it includes several
other mechanisms responsible for the moisture transfer
and the author suggested an alternative designation, ‘‘liquid
depletion coefficient’’ considering the effectiveness of the
effective moisture diffusivity in this approach.
If the material shrinkage during drying is negligible and
Deff is constant, the Equation (17) can be written as
@MR @ 2 MR
¼ Deff ð18Þ
@t @x2
for the one-dimensional nonsteady moisture transfer process
inside the solid sample; x represents the moisture transfer
direction through sample thickness. Considering that the
moisture is uniformly distributed at the beginning of the
263
‘‘diffusional’’ process, the solution of this problem is well
known (Crank, 1975) and is given by the following equation:
" #
8X 1
1 ð2n þ 1Þ2 p2 Deff t
MR ¼ 2 exp  ð19Þ
p n¼0 ð2n þ 1Þ2 4L2
where L stands for half of the sample thickness if symmetric
conditions of moisture ratio exists in sample surfaces or
represents the sample thickness if the surface at x ¼ 0 is an
impermeable surface (a moisture barrier).
The powder cork was in the tray during the drying pro-
cess with the upper surface exposed to the hot drying air-
stream which carries with it the evaporated moisture. The
other sample surface (in contact with the bottom of the tray)
behaves as an impermeable boundary since there isn’t moist-
ure flux across the tray wall.
The terms of the infinite series in the solution presented in
Equation (19) converge rapidly with the increasing time and
keeping just the first term results in small errors. So the
solution can be simplified and the useful approximation is
obtained:
 2 
8 p Deff t
MR ¼ exp  ð20Þ
p2 4L2
which can be used to estimate Deff from drying kinetics data.
A linear correlation will be obtained between ln MR and t
with slope equal to p2 Deff=4L2 and the value of Deff can
be calculated for the cork powder drying experiments.
Repeating the methodology described before with data
acquired in drying experiments performed at different
temperatures and assuming that an Arrhenius relation
describes the dependence of Deff with temperature,
 
Ea
Deff ¼ D0 exp  ; ð21Þ
Ru T
the drying activation energy (Ea) can be calculated using
Equation (21); D0 is a constant, Ru is the ideal gas constant,
and T is the drying (absolute) temperature.
Results and Discussion
The Mathematical Approach Proposed Applied to Drying
Kinetics Data
The evolution of X with the drying time, t, is represented in
Figure 2 to show the characteristic drying curve for the cork
powder under the constant air drying stream conditions used
in the experiment. From the decrease of moisture content
presented in Figure 2, it is evident that the three character-
istic periods of convective drying are present: the preheating
of the wet solid, the constant drying rate period and the fall-
ing drying rate period. After an unsteady state period in
which the solid initially at ambient temperature increases
its temperature to the wet bulb temperature of the drying
air, the moisture content of the wet cork powder decreases
linearly with time during approximately 124 min. For higher
264
drying times the decrease in the moisture content of the solid
was slower, indicative of the falling drying rate period.
After 210 min, the moisture content of the solid remains
approximately constant and the equilibrium with the air
humidity prevailing in the air drying stream is achieved
(Mujumdar, 2006). The dying process was interrupted.
The drying curve was obtained from the solid moisture
content information using Equation (3) for time intervals
of 200 s, as explained before. The resulting drying rate curve
is presented in Figure 3. Is evident that a significant random
scatter of data remains despite the effort made to reduce the
effect of mass uncertainty in the computed values of R
increasing the time interval considered in the finite difference
method. However, the three periods of convective drying are
evident from the plot. The preheating period, in which the
wet solid adapts itself to the air conditions, is not long and
for a moisture content of about 6.9 kgwater=kgdry solid the dry-
ing rate becomes almost constant. This period of constant
drying rate ends at 1.8 kgwater=kgdry solid, the critical moisture
content, and a period of decreasing drying rate starts. The
falling drying rate period seems to be nearly linear with
moisture content until a value of about 0.88 kgwater=kgdry
solid followed by a nonlinear period until the equilibrium
moisture content (0.16 kgwater=kgdry solid) was reached.
In order to obtain the drying rate curve directly from the
moisture content curve without discarding the raw data pre-
sented in Figure 2, the mathematical approach proposed was
applied. From Figure 2 is evident the existence of a constant
drying rate period followed by a falling rate period and for
that reason, different functions were fitted to data corre-
sponding to each period. The data in the first period was
fitted with a linear function and to the second period
a polynomial function of third degree was used to fit the
data. To obtain the instant in which the characteristic
periods change, when the critical moisture is attainted, an
iterative methodology was implemented, as described below.
For the first estimation of tc the transition between the
two periods was considered visually from data represented
in Figure 2. From the best fit equations obtained a new
Fig. 3. Drying rate curve for the experiment performed with wet
cork powder. Air drying conditions: 45.52  0.27 C and
0.77  0.01 m=s.
L. M. M. N. Castro and M. N. Coelho Pinheiro
estimation of tc is calculated using Equation (6) and after
that new equations X(t) were fitted to data considering the
new duration of both drying periods. This procedure was
repeated until the difference of successive values of tc was
lower than 1%.
The final fitted equations X(t) obtained after the iterative
methodology described and the respective correlations coef-
ficients were represented in Figure 4 with correlated data. As
can be observed, the functions used to derived rate equations
correlated very well the experimental data.
The values of R were calculated using Equation (4) for
t < tc and using Equation (5) when t  tc. It should be noted
that the computation of R was made with all data acquired
during the experiment, at time intervals of 40 s. The resulted
drying rate curve is presented in Figure 5. The values of X
(the x axis of the drying rate curve) are the experimental
values obtained for the instants t considered, to whom the
corresponding values of R are calculated. To make the com-
parison easier, in Figure 5 there are also represented the R
values calculated directly from the values measured during
the drying experiment depicted in Figure 3. The drying rate
curve resulting from the application of the mathematical
approach described has a very smooth appearance and all
the raw data is considered with the methodology proposed.
Moreover, the transition from the constant drying rate per-
iod to the falling drying rate period is very well defined and
the value of Xc could be easily obtained from the drying rate
curve. The evaporation rate, per unit area of the drying sur-
face, is constant and equal to 10.03 g=(min m2) until the criti-
cal moisture content of 1.84 kgwater=kgdry solid was attainted
during the drying process (see Figure 5). Beyond Xc, the
evaporation rate starts to decrease with the moisture content
in the solid and seems to present a linear dependency until a
moisture content Xd of nearly 0.88 kgwater=kgdry solid was
reached, followed by a falling drying rate period no linear.
The evaporation rate becomes zero for a moisture content
Fig. 4. Moisture content curve for the experiment performed
with wet cork powder with the functions fitted to data in order
to describe the drying kinetics. Air drying conditions:
45.52  0.27 C and 0.77  0.01 m=s.
Drying Kinetics Experiments 265

the wet solid layer and is followed by a period of intraparticle

Fig. 5. Drying rate curve resulted from the mathematical
approach proposed and values obtained from data acquired
during the experiment performed with wet cork powder. Air
drying conditions: 45.52  0.27 C and 0.77  0.01 m=s.
of 0.16 kgwater=kgdry solid indicating that the equilibrium
moisture in the solid Xe was reached. In Figure 5 is repre-
sented the best linear fit to the first falling drying rate period
observed in the drying rate curve and as expected a very
good correlation was obtained (R2 ¼ 0.9982). Probably, this
period corresponds to the evaporation of the moisture exist-
ing between the small particles constituting the cork powder
(i.e., interparticle moisture content) at the inferior level of
moisture content reduction.
Table III shows the initial moisture content of the wet
cork powder to be dried, the moisture content of the solid
Xc, Xd, and Xe, the constant drying rate Rc and the duration
of both drying periods, for the experiment performed with
the wet cork powder.
The methodology proposed was presented using the
powder cork drying kinetics data where two functions (linear
and third-degree polynomial) were enough to correlate
the decrease of moisture content successfully. However, the
shape of the moisture content curve depends on the nature
of the wet solid to be dried and more and=or different
functions shall be used to correlate data accurately, but
the mathematical approached presented is still valid.
Semiempirical Models Adjustment
The data collected during the drying experiment were fitted
using semiempirical models reported in the bibliography
and presented in Table II. Table IV shows the parameter
estimations obtained for the semiempirical models tested
with the respective correlation indicators (r2, v2, and
RMSE). The nonlinear regression was applied to the data
acquired during the falling rate period of the cork powder
drying experiment because following the suggestion of
several authors, as referred before, the models used are
more suitable to describe drying kinetics during that period.
In order to verify this suggestion, the nonlinear regression

Table IV. Model parameters obtained from nonlinear regression and values of r2, v2, and RMSE to evaluate the adjustment of data
to the models during the falling rate period
Correlation Reduced chi-square Root mean square
Model Parameter coefficient (r2) test (v2) error (RMSE)

Lewis k ¼ 0.0002511 s1 0.6561 0.001840 0.04272

Page k ¼ 1.761E-10 sn 0.9934 0.00003555 0.005913
n ¼ 2.555
Handerson & Pabis k ¼ 0.0006234 s1 0.9789 0.0001137 0.01057
A ¼ 27.39
Logarithmic k ¼ 0.0004081 s1 0.9970 0.00001657 0.004020
A ¼ 6.221
B ¼ 0.04930
Two-terms k0 ¼ 0.0006235 s1 0.9789 0.0001156 0.01057
k1 ¼ 0.0006235 s1
A ¼ 10.25
B ¼ 17.14
Wang & Singh k0 ¼ 0.0001392 s1 0.9776 0.0001210 0.01091
k1 ¼ 4.575E-09 s2
Modified Page I k ¼ 6579.1 s 0.9936 0.00003468 0.005841
n ¼ 2.587
Midilli k ¼ 0.0001528 sn 0.9969 0.00001728 0.004088
A ¼ 5.1728
B ¼ 0.000003172 s1
n ¼ 1.1066
Verma k ¼ 4.021 s1 0.9789 0.0001146 0.01057
g ¼ 0.0006235 s1
A ¼ 26.39
266
was also applied to the data acquired during all the experi-
ment and for all models used (see Table II) and the reduced
chi-square test (v2) presented higher values and the
correlation coefficient (r2) values are lower for all models
(with exception to the Lewis’ model) indicating a not so
good correlation of data.
Analyzing the values of r2, v2, and RMSE used to evalu-
ate the adjustment of data to the models shown in Table II,
it is observed that Logarithmic model shows the best fit
between data in the falling rate period and predictions,
followed by the Midilli and Modified Page I models that
present also good correlations. The MR data is plotted
versus t in Figure 6 together with the result of the regression
analysis performed with the three models with best levels of
correlation, the Logarithmic, Midilli, and Modified Page I
models. Figure 6 shows that in general a good fitting
between data and predictions from the models are obtained.
For values of moisture ratios corresponding to the beginning
of the falling rate period (the first 2 min), average deviations
between data and models of 2.8% and 4.2%, respectively,
for Logarithmic=Midilli and Modified Page I, are found.
However, for small moisture ratios, the deviations are
significant for Modified Page I model and Midilli and
Logarithmic models cannot predict this region where the
solid moisture approaches the equilibrium moisture content.
The Mathematical Approach Proposed Applied to
Semiempirical Models Describing Drying Kinetics
As the information obtained from the drying rate curve has
a relevant practical interest, the iterative mathematical
approach proposed was applied to the equations describing
Logarithm, Midilli, and Modified Page I models. These
models are those that fitted better data obtained during
the experiment performed with wet cork powder, as
Fig. 6. Moisture ratio curve for the experiment performed
with wet powder cork and moisture ratio curves predicted from
Third-degree polynomial, Logarithmic, Modified Page I, and
Midilli models. The curves correspond to the falling rate period.
Air drying conditions: 45.52  0.27 C and 0.77  0.01 m=s.
L. M. M. N. Castro and M. N. Coelho Pinheiro
Fig. 7. Drying rate curve resulted from the mathematical
approach proposed applied to data, to the predictions obtained
from Logarithmic, Modified Page I, and Midilli models and to
the values obtained from data acquired during the experiment
performed with wet cork powder under constant air drying
conditions (45.52  0.27 C and 0.77  0.01 m=s).
concluded in the previous section. The drying rate curves
obtained are represented in Figure 7 together with data
acquired during the experiment and using the third-degree
polynomial fit proposed in the presented analysis. Again,
the mathematical approach proposed in this study allows a
well-defined transition from the constant drying rate period
to the falling drying rate period. The values of Xc from the
three semiempirical models are close but clearly underpre-
dict the experimental value referred before (1.84 kgwater=
kgdry solid, to which corresponds a MR of 0.241).
From the drying rate curves obtained from Modified Page
I, Logarithmic, and Midilli models that are represented in
Figure 7, a single (linear) falling drying rate period seems
to be present during the process of drying of wet cork
powder unlike the data suggests.
Drying Parameters: Effective Moisture Diffusivity and
Activation Energy
The continuous weighing of the wet solid during drying
process results in a large amount of data useful in dryer
design, as mentioned previously. The effective moisture
diffusivity and the activation energy are essential parameters
not only in the design step but also in modeling the drying
process. The importance of these parameters justifies this
section devoted to present effective diffusivity values for
moisture in wet powder cork samples calculated from drying
experiments carried out at different temperatures.
After the critical moisture identification with the iterative
procedure proposed, the effective moisture diffusivity was
obtained correlating lnMR with t for data acquired in the
falling drying rate period in all experiments performed.
Reasonable linear correlations were obtained, with correlations
Drying Kinetics Experiments
Table V. Effective moisture diffusivity obtained for cork powder
drying at different temperatures
Temperature ( C)
29 39 42 48 52
Deff  109 (m2=s) 3.97 5.29 5.79 6.93 6.96
coefficients ranging from 0.88 to 0.93. As expected, the
calculated Deff values were greater when the powder cork
was dried at higher temperatures indicating that hindrance
to moisture depletion from the sample interior decreases
with the temperature increase. The calculated values varied
from 3.97  109 to 6.96  109 m2=s when the temperature
used in the drying process changed from 29 C to 52 C.
In Table V are indicated the Deff values obtained in all the
temperature conditions used.
The values encountered for powder cork in the present work
seem to be in accordance with the values of effective moisture
diffusivity for forestry and agricultural residues reported in the
bibliography ranging from 109 to 108 m2=s. Thakur and
Gupta (2006) presented values of Deff between 8.42  109
and 1.69  108 m2=s for rice husk and for temperatures from
30 C to 60 C, while Tirawanichakul (2008) using nearly the
same range of temperatures found values of Deff for moisture
in coconut husk ranging from 1  108 to 6  108 m2=s. The
moisture diffusivity in powdered peanut shell was evaluated
by Chen et al. (2012a) for a temperature range of 50–90 C
and they obtained values from 9.60  109 to 2.26 
108 m2=s. A team with some of the previous authors
(Chen et al., 2012b) determined also the Deff in poplar
sawdust for similar temperatures (50–90 C) and they found
values between 9.38  1010 to 1.38  109 m2=s.
Magalhães and Pinho (2008) calculated the effective
moisture diffusivity in cork stoppers from data obtained in
spouted bed drying processes over a temperature range of
40–70 C. The authors encountered values from 1.36  109
to 4.44  109 m2=s when the drying temperature varied
from 40 C to 70 C. Abdulla et al. (2010) in order to evaluate
the impact of an instant controlled pressure drop treatment
(usually referred as DIC) on the cork granules drying
with hot air determined the effective moisture diffusivity
in untreated samples. For the smallest granules used
(0.5–1 mm mean diameter) the value of Deff increased
from 2.60  109 to 4.50  109 m2=s when the air drying
temperature changed from 50 C to 70 C.
The value obtained in this work for the convective drying
of a thin layer of powder cork at 39 C (5.29  109 m2=s) is
higher than the value obtained by Magalhães and Pinho
(2008) for cork stoppers dried at a similar temperature.
In fact, it was expected that essentially interparticle (but also
intraparticle) moisture transfer resulted in a facilitated
process when compared with the depletion of intraparticle
moisture in cork stoppers. The same behavior was observed
when comparing the Deff obtained in this study at 48 C
(6.93  109 m2=s) with the value presented by Abdulla
et al. (2010) for cork granules calculated for intraparticle
moisture transfer at 50 C.
267
Fig. 8. Plot of lnDeff versus 1=T resulting from the
Arrhenius-type relationship between effective moisture diffusiv-
ity and temperature for powder cork.
In order to obtain the activation energy for powder cork
drying the logarithmic form of the Arrhenius equation
(Equation (21)) was used to correlate the data presented in
Table V. The performance of the linear relationship of lnDeff
versus 1=T is evident from Figure 8. From the slope of the
best linear fit (Ea=Ru), it was obtained an activated energy
of 24.04 kJ=mol. This value is smaller than the one achieved
by Magalhães and Pinho (2008) for cork stoppers (28.72 kJ=
mol) indicating that a lower energy is required to initiate the
moisture transfer in a thin layer of powder cork than inside
of a cork stopper during the drying process. Although not so
noticeable, the activation energy obtained in this study was
also smaller than the value reported by Abdulla et al.
(2010) for cork granules with 0.5–1 mm of mean diameter
(25.29 kJ=mol).
Conclusions
The simple mathematical approach proposed to process raw
data obtained in drying kinetics experiments was applied
successfully to the set of wet solid weight values acquired
continuously during the convective drying of powder cork.
Although the case study of powder cork was presented,
the methodology was also tested with success to other wet
solids (sand, vegetables, and fruits).
The three periods of convective drying (the constant dry-
ing rate period and two falling drying rate periods) observed
in the drying rate curve obtained from the powder cork raw
data were clearly identified after application of the math-
ematical approach. The optimization of the polynomial
functions fitted to the solid moisture content data, resulting
from an iterative procedure, allows the prediction of the
critical moisture content for the powder cork, which is cor-
roborated by the experimental data. The transition from
the linear falling rate period to the second falling rate period
could be also easily identified. The Logarithmic, Midilli, and
Modified Page I models correlated adequately the raw data
during the falling drying rate period but the parameters used
to evaluate the adjustment of data to the models indicated
the third-degree polynomial function as the best choice for
the case study presented. When the proposed methodology
was applied using the previous semiempirical models to
268 L. M. M. N. Castro and M. N. Coelho Pinheiro

correlate data, the critical moisture content of the powder Greek Symbols
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