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Research Paper

Determination of diffusion and convective transfer


coefficients in food drying revisited: A new
methodological approach

Francisco J. Arranz a, Tatiana Jimenez-Ariza b, Belen Diezma c,


Eva C. Correa d,*
a
Grupo de Sistemas Complejos, Departamento de Ingenierı́a Agroforestal, ETSI Agronomica Alimentaria y de
Biosistemas, Universidad Politecnica de Madrid, Av. Puerta de Hierro 2, 28040 Madrid, Spain
b
Facultad de Ciencias Ba sicas e Ingenierı́a, Universidad San Buenaventura, Carrera 8H # 172 e 20, Bogota,
Colombia
c
Laboratorio de Propiedades Fı́sicas y Tecnicas Avanzadas en Agroalimentacion (LPT_TAGRALIA), Departamento de
Ingenierı́a Agroforestal, ETSI Agronomica Alimentaria y de Biosistemas, Universidad Politecnica de Madrid, Av.
Puerta de Hierro 2, 28040 Madrid, Spain
d
Laboratorio de Propiedades Fı́sicas y Tecnicas Avanzadas en Agroalimentacion (LPF_TAGRALIA), Departamento de
Quı́mica y Tecnologı́a de Alimentos, ETSI Agronomica Alimentaria y de Biosistemas, Universidad Politecnica de
Madrid, Av. Puerta de Hierro 2, 28040 Madrid, Spain

article info
It is usual to determine diffusion and convective transfer coefficients using classical
Article history: approximate relationships involving dimensionless numbers. These approximate relation-
Received 3 January 2017 ships were developed in the past, in order to avoid the difficulties associated with calculations
Received in revised form of large series expansions and its corresponding expansion coefficients given by transcen-
9 July 2017 dental equations. However, the development of improved computing techniques has
Accepted 24 July 2017 removed these difficulties, such that currently such calculations can be easily performed. An
Published online 12 August 2017 iterative methodology is proposed that takes advantage of current computational capabil-
ities, avoiding to use approximate relationships. The proposed methodology is applied to
Keywords: generated data and also to experimental data from carrot drying. Additionally, a MATLAB®
Mass Biot number implementation of the proposed iterative methodology, along with the input data files cor-
Mass Fourier number responding to the results presented in this paper, is provided as supplementary material.
Iterative numerical methodology © 2017 IAgrE. Published by Elsevier Ltd. All rights reserved.
Carrot

conditions, the correct and accurate determination of the


1. Introduction physical parameters involved is a central issue. Especially
important in food engineering are heat and mass transfer
In the development of suitable models for complex processes processes, which are characterised by the corresponding
involving foods, which are applicable to a broad set of external diffusion and convective transfer coefficients.

* Corresponding author.
E-mail address: evacristina.correa@upm.es (E.C. Correa).
http://dx.doi.org/10.1016/j.biosystemseng.2017.07.005
1537-5110/© 2017 IAgrE. Published by Elsevier Ltd. All rights reserved.
b i o s y s t e m s e n g i n e e r i n g 1 6 2 ( 2 0 1 7 ) 3 0 e3 9 31

Nomenclature [z Half height of the sample (mm)


t Time (s)
Bi Biot number
ti The i-th time measured in the drying process (s)
D Effective diffusion coefficient (m2 s1)
v Air velocity induced by the extractor fan (m s1)
Di Effective diffusion coefficient calculated at the i-th
w0 Initial sample weight in the drying process (g)
iteration (m2 s1)
wdm Sample dry matter weight (g [dry matter])
F Mass flow (g [water] (m2 s1)
weq Sample weight at equilibrium in the drying
Fo Dimensionless time (Fourier number)
process (g)
M Dry basis moisture (g [water] g1 [dry matter])
wi Sample weight at each time ti in the drying process
M Position averaged moisture (g [water] g1 [dry
(g)
matter])
x Position across thin layer sample thickness (mm)
M0 Initial uniform moisture (g [water] g1 [dry
yi The i-th ordinate value corresponding to the
matter])
average dimensionless relative moisture at each
Meq Moisture at equilibrium (g [water] g1 [dry matter])
time ti in the drying process
M[ Moisture at food sample-air interface (g [water]
Di Convergence of first term approximation for the
g1 [dry matter])
i-th iteration
SD Generalised significant figures in diffusion
F Average dimensionless relative moisture
coefficient
FN The N terms series expansion approximation to
Sh Generalised significant figures in mass transfer
the average dimensionless relative moisture
coefficient
mn The n-th positive root of the characteristic
T Sample temperature ( C)
equation mntanmn ¼ Bi
a Intercept in the fitting to the straight line y ¼ a þ bt
r Sample dry matter density (g [dry matter] m3 )
b Slope in the fitting to the straight line y ¼ a þ bt
s2D Variance of the diffusion coefficient (m2 s1)
(s1)
s2h Variance of the mass transfer coefficient (m s1)
h Convective mass transfer coefficient (m2 s1)
s2i Variance corresponding to the i-th ordinate value
hi Convective mass transfer coefficient calculated at
yi in the drying process
the i-th iteration (m2 s1)
s2w Variance corresponding to the instrumental error
[ Half thickness of the sample (mm)
of the weighing device (g)
[y Half width of the sample (mm)

It is noteworthy that for industrial purposes, as is pointed the series expansion solution, diffusion coefficient can be
out by Zhao et al. (2014), foods are usually dried to remove the obtained from the corresponding slope (Karim & Hawlader,
moisture up to a certain level at which microbial spoilage and 2005; Mghazlia et al., 2017; Sampaio et al., 2017; Srikiatden &
deteriorative chemical reactions are minimised, and accurate Roberts, 2006). Additionally, by using approximate relation-
determination of diffusion and convective transfer co- ships involving dimensionless numbers, in particular the Biot
efficients is required in order to facilitate accurate designs. number, convective transfer coefficient is also obtained
Different methods have been described in the literature to (Dhalsamant, Tripathy, & Shrivastava, 2017; Guine , Cruz, &
obtain experimental values for these coefficients. Zhao et al. Mendes, 2014; Tripathy & Kumar, 2009). Note that, in order
(2014) used a trial-and-error method based on a comparison to obtain the correct values of the coefficients, it is important
of analytic and experimental drying curves, tuning the value that the experimental conditions correspond to the mathe-
of the diffusion coefficient until the matching of both curves is matical conditions under which the analytical solution was
reached approximately. In similar fashion, Białobrzewski obtained. However, it is not common to find in the literature
(2007) obtained both diffusion and convective transfer co- details explaining the drying experimental methodology
efficients by comparing numerical (as opposed to analytical) which could fulfil such conditions.
and experimental drying curves. Note that analytical solu- Moreover, it is important to determine the accuracy of the
tions are available only for some simple systems, whilst nu- resulting coefficients and the corresponding significant fig-
merical solutions are available for any system. Conversely, ures. Note that the instrumental error of the experimental
analytical solutions have arbitrarily high accuracy, but the data will propagate in the calculations when the coefficients
accuracy of numerical solutions is limited by numerical are obtained, such that the significant figures in the initial
approximation, especially in the case of partial differential experimental data will decrease (or at best remain the same)
equations. Also, in order to obtain the convective transfer in the calculated coefficients. In this regard, as is well known,
coefficient, the reaction engineering approach has been the calculability of diffusion and convective transfer co-
applied by considering drying as a competitive process be- efficients depends on the Biot number, therefore this issue
tween condensation and evaporation (Compaore et al., 2017). should be analysed in any method for the determination of
However, the most widely used method is the fitting of the diffusion and convective transfer coefficients.
experimental drying curves, in logarithmic form, to a straight In drying experiments, since the mass diffusion coefficient
line. For simple one-dimensional geometries, such as for sli- (and also convective mass transfer coefficient) depends on
ces or cylinders, by assuming the first term approximation in temperature, in order to calculate the mass diffusion
32 b i o s y s t e m s e n g i n e e r i n g 1 6 2 ( 2 0 1 7 ) 3 0 e3 9

coefficient (and convective mass transfer coefficient) by fitting solving, it can be identified the mismatching of experimental
to an analytical solution of mass diffusion equation where the conditions and mathematical conditions, and so, the unsuit-
diffusion coefficient (and convective mass transfer coefficient) ability of used data. As will be explained in detail below,
is assumed to be constant, it is mandatory to maintain the experimental data are first transformed to an asymptotic
sample with uniform temperature in its whole volume. In this linear form and then fitted to a straight line. The mathemat-
regard, as was shown by Srikiatden and Roberts (2006) when ical conditions under which the analytical solution is obtained
studying potatoes and carrot drying, when the initial tem- lead to a very narrow range for the intercept of this asymptotic
perature of the sample and target temperature differ, the straight line. So that, a fitting intercept value out of range
maintenance of surrounding air temperature at target tem- implies that experimental data have been obtained under
perature is not sufficient to achieve uniform temperature, experimental conditions that differs from mathematical
with temperature gradients occurring inside the sample. It is conditions, hence is unsuitable for the determination of
necessary firstly to heat the sample, using a microwave device diffusion and convective transfer coefficients.
which leads to uniform temperature, up to target tempera- The proposed methodology is applied to generated data, in
ture, and then maintain the surrounding air temperature at order to test its behaviour, and also to experimental data from
the target temperature throughout the drying assay. The likely carrot drying at different temperatures, including an unsuitable
reason for wrong determination of the mass diffusion coeffi- data set corresponding to non-isothermal drying, included in
cient is due to existence of temperature gradients inside the order to illustrate the detection of the unsuitability of data set.
sample, as was pointed out in the early literature (Chen & Additionally, a MATLAB® implementation of the proposed
Johnson, 1969; Chirife, 1983; King, 1968; Vaccarezza, iterative methodology, along with the input data files corre-
Lombardi, & Chirife, 1974). sponding to the results presented in the paper, is provided as
Additionally, aside from temperature, other conditions must supplementary material.
be controlled in order to correctly obtain mass diffusion and
convective mass transfer coefficients. Thereby, sample volume
is usually assumed constant in obtaining analytical solutions of
diffusion equation, so that shrinkage should be controlled in 2. Materials and methods
food samples (e.g., by taking drying data over the initial period,
when shrinkage is negligible). Besides, the asymptotic moisture 2.1. Determination of diffusion and convective transfer
value (i.e., sample moisture at infinite time) is also usually coefficients
assumed constant, so that the relative humidity of the sur-
rounding air should be maintained invariable. 2.1.1. Mathematical model
On the other hand, in the fitting of the corresponding It is assumed that, for a thin layer sample, food drying process
analytical solution to obtain mass diffusion and convective is well described by means of the one-dimensional diffusion
mass transfer coefficients, some approximations are usually equation
made. Firstly, in the infinite series expansion of the analytical  
vM v vM
solution, the first term approximation is taken, that is, solu- ¼ D ; (1)
vt vx vx
tion is approximated by taking only the first term in series
expansion. As is well known, this is a very accurate approxi- with uniform initial condition
mation only for large enough time (Crank, 1975; Luikov, 1968).
Mðx; t ¼ 0Þ ¼ M0 ; (2)
Time threshold is well defined in terms of dimensionless time,
but dimensionless time depends on the diffusion coefficient, and boundary conditions
so that some iterative process should be used. Secondly, the  
vM
logarithmic form of first term approximation leads to a ¼ 0; (3)
vx x¼0
straight line, so that the fitting process is straightforward.
Nevertheless, direct calculation of diffusion and convective and
transfer coefficients from fitting intercept and slope involves  
vM h 
the solving of a transcendental equation, so that different ¼  M[  Meq ; (4)
vx x¼[ D
approximate relationships involving dimensionless numbers
were developed in order to avoid this difficulty (Luikov, 1968; where M is the dry basis moisture, t is the time, x is the position
Pflug & Blaisdell, 1963). Despite that these difficulties being across thin layer sample thickness (with origin x ¼ 0 at internal
easily avoidable, due to the development of computers and centre), [ is the sample half thickness, and D and h are the
numerical methods, the approximate classical schemes are physical drying parameters, namely, effective diffusion and
still used (Guine  et al., 2014; Karim & Hawlader, 2005; convective mass transfer coefficients, respectively. Besides,
Srikiatden & Roberts, 2006; Tripathy & Kumar, 2009). M[ ¼ M(x ¼ [, t) is the moisture at food sample-air interface, and
In order to determine diffusion and convective transfer Meq ¼ Mðx ¼ [; t/∞Þ is the corresponding moisture at equilib-
coefficients from drying data, an iterative methodology is rium. Note that symmetric external conditions, i.e. the same air
presented that takes advantage of current numerical and conditions at both sides of the thin layer, have been assumed.
computational capabilities, avoiding to use the approximate Since initial condition in Eq. (2) is also symmetric, the whole
classical schemes, and numerically solving the corresponding system is symmetric, so that the mass flow F ¼ rD(vM/vx) given
transcendental equations. As an additional feature, from the by Fick's law, where r is the dry matter density, will be null at the
range of obtained parameters involved in this numerical internal centre, leading to the boundary condition in Eq. (3).
b i o s y s t e m s e n g i n e e r i n g 1 6 2 ( 2 0 1 7 ) 3 0 e3 9 33

Moreover, if food sample temperature is maintained con- FðFo; BiÞ in Eq. (9) must be calculated with sufficient accuracy,
stant during drying process, then the diffusion coefficient D i.e, by taking a large enough number of terms N in the series
can be assumed to be constant. Additionally, if the air velocity expansion leading to a high accuracy approximation
is constant, the convective transfer coefficient h can also be FN ðFo; BiÞ. For this purpose, the corresponding first N roots of
assumed constant. Finally, if the relative humidity of air is the transcendental equation in Eq. (10) need to be calculated
maintained constant, then the moisture at equilibrium Meq with high accuracy, too. However, since the roots are clearly
will be constant. Under these additional conditions, the so- bounded by the inequalities in Eq. (11), there exist different
lution of diffusion equation in Eq. (1) under initial condition in numerical algorithms that are able to calculate them very
Eq. (2), and boundary conditions in Eqs. (3) and (4), is given by efficiently. Specifically, the algorithm of Forsythe, Malcolm,
the following series expansion (Crank, 1975; Luikov, 1968) and Moler (1977) have been used, which is implemented in
 x   the MATLAB® function fzero.
Mðx; tÞ  Meq X ∞
2sinmn Dt
¼  cos mn exp  m2n 2 ; Moreover, it is well known that the series expansion in Eq.
M0  Meq n¼1
mn þ sinmn cosmn [ [
(9) converges rapidly and monotonically for high enough
(5)
values (depending on Biot number value) of the Fourier number
being mn the positive roots of the equation (Crank, 1975; Luikov, 1968), so that, as time increases, moisture
h[ curve tends asymptotically to the first term in the series, that is
mn tanmn ¼ ; (6)
D
lim FðFo; BiÞ ¼ F1 ðFo; BiÞ: (12)
ordered such that 0 < mn < mnþ1. The experimentally measur- Fo/∞

able overall moisture content M of the sample is obtained by In other words, for high enough values of the Fourier
averaging over the whole sample volume number, moisture time evolution FðFo; BiÞ is well described by
the first term approximation F1 ðFo; BiÞ, that expressed in
Z[
1 logarithmic form
MðtÞ ¼ Mðx; tÞdx; (7)
[  2 
0 2sin m1 m2 D
logFzlog  12 t; (13)
m1 ðm1 þ sinm1 cosm1 Þ [
so that, the overall content moisture corresponding to series
expansion in Eq. (5) will be takes the form of a straight line y ¼ a þ bt with intercept
   
MðtÞ  Meq X ∞ 2 2
2sin mn Dt 2sin m1
¼  exp  m2n 2 : (8) a ¼ log ; (14)
M0  Meq n¼1
mn ðmn þ sinmn cosmn Þ [ m1 ðm1 þ sinm1 cosm1 Þ

As is well known, the solutions of diffusion equation can be and slope


expressed in terms of dimensionless magnitudes (Crank, 1975;
m2 D
Luikov, 1968). In this way, the series expansion in Eq. (8) can be b ¼  12 : (15)
[
expressed as follows
So that, by taking a set of drying data {w0,w1,…,weq}, the
X

2Bi
2
  corresponding ordinate values can be calculated1
FðFoÞ ¼  2  exp m2n Fo ; (9)  
n¼1 m2n Bi þ Bi þ m2n wi  weq
yi ¼ log ; (16)
where F ¼ ½MðtÞ  Meq =ðM0  Meq Þ is the average dimension- w0  weq
less relative moisture, Fo ¼ Dt/[2 is the dimensionless time where w0 is the initial sample weight at t0 ¼ 0, wi is the sample
known as Fourier number, and Bi ¼ h[/D is the Biot number, weight at each time ti(i ¼ 1,2,…), and weq is the sample weight
which determines the relative importance between diffusion at equilibrium. Then, intercept a and slope b can be obtained
and convective transfer processes. Notice that, in dimen- by means of the least squares fitting to a straight line of the
sionless form, the coefficients mn are defined as the positive data pairs {ti,yi}(i ¼ 1,2,…).
roots of the equation It should be noted that, by using the logarithm function in
the ordinate values definition yi, the corresponding variances
mn tanmn ¼ Bi: (10)
s2i will increase with time, so that, a weighted least squares
If diffusion process is much faster than convective transfer fitting should be used in the obtaining of slope and intercept
process (external problem), then Bi/0 and the positive roots values. Indeed, assuming the same variance s2w for all weight
of Eq. (10) are given by mn ¼ (n  1)p. Conversely, if convective data wi, which is determined by the weighing device used
transfer process is much faster than diffusion process (inter- (instrumental error), the variances for the ordinate values
nal problem), then Bi/∞ and the corresponding roots are yi(i ¼ 1,2,…) are given by2
given by mn ¼ ð2n  1Þp=2. So that, when both processes are
simultaneously relevant (0 < Bi < ∞), the positive roots of Eq. 1
Note that, in order to calculate the average dimensionless
(10) are bounded by the two extreme cases, that is, relative moisture F from drying data, only weight data w are
needed, and no average moisture values M should be calculated,
ðn  1Þp < mn < ð2n  1Þp=2: (11) M M
since M0i Meq
w w
¼ w0i weq :
eq eq
2
Given a function f(x1,…,xN) of variables xk with variances
2.1.2. Iterative numerical methodology s2k ðk ¼ 1; …; NÞ, error propagation theory provides the following
In order to obtain the diffusion and convective transfer co-  2
P vf
formula for the variance s2 of the function f.s2 ¼ N k¼1 vxk s2k :
efficients from drying data, the dimensionless moisture
34 b i o s y s t e m s e n g i n e e r i n g 1 6 2 ( 2 0 1 7 ) 3 0 e3 9

!
1 1 1 manually water washed, peeled, and lengthwise sliced with a
s2i ¼ 2s2w  2 þ   þ 2 : kitchen slicer (Cooking, CASA International nv, Itegem, Ant-
wi  weq wi  weq w0  weq w0  weq
werpen, Belgium) in order to obtain constant thickness. The
(17)
samples were sliced from central part of carrots, and even-
The weighted least squares fitting was carried out by using tually cut into rectangular pieces. The dimensions of each
the algorithm of Strang (1986), which is implemented in the carrot sample were measured by means of a digital caliper
MATLAB® function lscov. gauge (DigitCal® Classic 05.30035, Swiss Instruments Ltd.,
After fitting process, the first root value m1 is calculated Mississauga, Ontario, Canada).
from Eq. (14). Notice that, as in the calculation of the roots of Before drying process, each carrot sample was heated in a
Eq. (10) discussed above, it is a transcendental equation, so microwave oven (PTMW 700, Electrodome sticos Taurus S.L.,
that the algorithm of Forsythe et al. (1977) has also been used. Oliana, Lerida, Spain), with the aim of achieving a uniform
Then, diffusion coefficient D is calculated from Eq. (15), temperature in the whole sample. With the purpose of
convective transfer coefficient h is calculated from Eq. (6), and determine diffusion and convective transfer coefficients at
Biot number Bi from Eq. (10). different temperatures, distinct heating periods were consid-
However, the coefficients thus obtained could be wrong, since ered to reach temperatures around 40, 50, 60, and 70  C. In
the first term approximation F1 ðFo; BiÞ is valid for high enough order to avoid the start of drying process throughout the
values (depending on the Biot number value) of the Fourier heating period, a small bowl with water was introduced into
number, and both Fourier and Biot numbers depend on diffusion microwave oven along with each sample.
and convective transfer coefficients. So that, in order to ensure After heating, sample temperature was measured in each
the correctness of the coefficients calculated, an iterative pro- case by using a type T thermocouple thermometer
cess is mandatory. Thus, iteratively, the (i1)-th data pair will be (HH2001TC, Omega Engineering Inc., Stamford, CT, USA),
deleted and the corresponding coefficients Di and hi recalculated giving temperatures of 40, 55, 64, and 72  C. Before each
by fitting of remaining data pairs, until the convergence of first sample was introduced into the weighing device, it was
term approximation within data accuracy, namely sandwiched between two metal grids in order to keep the slice
  shape. The setpoint temperature, corresponding to each
FN ðFoi ; Bii Þ  F1 ðFoi ; Bii Þ  si ; (18) measured temperature at which the parameters will be esti-
where the values of Fourier and Biot numbers are recalculated mated, was established in each case in the weighing device
at each iteration from fitting coefficients Di and hi. When the (AMB 300 moisture balance, Inscale Measurement Technology
condition in Eq. (18) is fulfilled, the corresponding coefficients Ltd., Bexhill, East Sussex, UK), and the sample weight
Di and hi can be considered the correct coefficients. Observe recording every 20 s was started. As shown in Fig. 1, the pro-
that, in order to verify the convergence of first term approxi- grammable weighing device comprises a chamber, with the
mation to exact values, we have used a high accuracy weighing pan inside, equipped with two halogen heaters, and
approximation FN ðFo; BiÞ that can be considered as exact also a RS-232 interface for connection to a computer, so that
within data accuracy. weighing data are automatically recorded in a file. The
Finally, notice that by applying the inequalities in Eq. (11) to instrumental error of the weighing device, which is required
the first root m1, the intercept a and the slope b of the fitted by the proposed iterative methodology in Eq. (17), is
straight line must necessarily fulfil the following conditions sw ¼ 0.001 g. Additionally, at the top of the chamber, there is a
ventilation grill. Observe that, in order to achieve the required
8 symmetric external conditions (i.e., the same air conditions at
log < a < 0; (19)
p2 both sample sides), the sample was raised on four feet above
and the sample pan.
Air temperature and also air relative humidity were
b < 0: (20)
monitored by means of an electronic logger (iButton® Hygro-
So that, the non-fulfilment of conditions above, when chron™ DS1923, Maxim Integrated Products Inc., San Jose , CA,
fitting a given data set, implies that the experimental setup USA) located into the weighing device chamber. In order to
breaks the model assumptions, and then the fitting co- prevent the increase of relative humidity in the sample sur-
efficients obtained will be wrong. In this regard, condition in roundings, an extractor fan (EVERFLOW F128025BU, SilverStone
Eq. (19) is particularly relevant since it establishes a very Technology Co. Ltd., New Taipei, Zhonghe, Taiwan) was
narrow range, a2(0.21, 0), for checking the suitability of mounted on the ventilation grill of the weighing device
experimental data set. chamber [see Fig. 1(a)]. Extracted air velocity was measured by
A MATLAB® implementation of the proposed iterative using a multifunctional precision manometer with Prandtl's
methodology, along with the input data files corresponding to tube (DC 100pro, Wo € hler Messgera € te Kehrgera€ te GmbH, Bad
the results presented in this paper, is available in the Wünnenberg, Paderborn, Germany).
supplementary material. Lastly, each carrot sample was entered into a drying oven
(Conterm Poupinel, JP SELECTA S.A., Abrera, Barcelona, Spain)
2.2. Experimental setup at 105  C until steady weight was achieved, and thereafter
sample dry weight was determined with a precision balance
The carrot samples were obtained from entire carrots (Daucus (ADP 720/L, Adam Equipment Co. Ltd., Kingston, Milton
carota L. cv. Nantes) purchased from local market, which were Keynes, UK).
b i o s y s t e m s e n g i n e e r i n g 1 6 2 ( 2 0 1 7 ) 3 0 e3 9 35

Fig. 1 e (a) Overview of the weighing device with the mounted extractor fan. (b) Section view of the weighing device with
the sample raised on four feet above the sample pan. (c) Detail of the sample sandwiched between two metal grids with the
four feet.

accuracy sw. Notice that convergence condition in Eq. (18) is


3. Results and discussion graphically represented in panel (h) of Fig. 2.
It is worth noting that we have verified in a heuristic
3.1. Determination of coefficients from generated data manner that, as is shown in Fig. 2 and summarised in Table 1
for the present case, diffusion and convective transfer co-
In order to test the behaviour of the proposed iterative efficients are obtained roughly with one significant figure less
methodology, the series expansion in Eq. (9) with original than the weighing values. Thus, the generated data set starts
coefficients D, h, and other conditions described in Table 1, with w1 ¼ 5.86 g and ends with w18 ¼ 3.01 g, corresponding to
was used to generate 18 sample weight data {w1, w2,…,w18} three significant figures, and diffusion and convective transfer
along drying process. By taking N ¼ 14 terms in series coefficients are obtained with two significant figures.
expansion, an accuracy of 0.001 g in the worst case Fo ¼ 0 was The number of significant figures obtained depends on the
achieved. Gaussian noise was introduced into generated data, Biot number, as well as the features of the experimental setup,
so that the final data set with weighing accuracy sw ¼ 0.01 g mainly the accuracy of the weighing data. In order to establish
was obtained. Pseudorandom values for Gaussian noise were the number of significant figures obtained in the calculation of
calculated by using the algorithms of Marsaglia (Marsaglia & diffusion and convective transfer coefficients under typical
Tsang, 2000; Marsaglia & Zaman, 1991) which are imple- conditions in drying experiments, we have carried out several
mented in the MATLAB® function randn. series of simulations by generating weighing data and fitting
The successive iterations corresponding to applying the generated data to obtain the coefficients, in a similar way to
proposed iterative methodology to generated data have been the example above. Sample half thickness [ ¼ 2 mm, weighing
depicted in panels (a)e(g) of Fig. 2. At each iteration, the first device accuracy sw ¼ 0.001 g with 4 significant figures, and
data point is deleted, and the remaining data fitted to a range 109  1012 m2 s1 for the order of magnitude of the
straight line leading to the corresponding values of diffusion diffusion coefficient are assumed as typical conditions in
Di and convective transfer hi coefficients. Note that, in the first drying experiments. Additionally, for each Biot number
iterations, the original fitting data points and the corre- Bi ¼ {0.001,0.01,0.1,1,10,100,1000} a set of 10 diffusion co-
sponding exact points obtained from Eq. (9) with the fitting efficients are randomly obtained, and for each random diffu-
coefficients Di and hi differ significantly. As iterative process sion coefficient 10 sets of weighing data are generated at
progresses both data sets get closer, and finally, when Fourier numbers Fo ¼ {0,0.1,0.2,…,1}. By comparing original
convergence is reached at i ¼ 7, they match within weighing diffusion and convective transfer coefficients with those
calculated from generated data sets, the value of the general-
ised number of significant figures SX is obtained. The gener-
Table 1 e Original and calculated diffusion and convective alised number of significant figures in X is defined by means of
transfer coefficients in the determination of coefficients the logarithmic difference
from generated data. Note that calculated coefficients
correspond to those in Fig. 2(g) rounded to two significant SX ¼ 1 þ log10 ðXÞ  log10 ðsX Þ; (21)
figures.
where X ¼ D, h is the value of the corresponding coefficient at a
Coefficients D (m2 s1) h (m s1) Bi
given Biot number, and sX is the standard deviation of the
Original 4.76$1011 2.74$107 11.5
coefficient from the different simulations (10 simulations in
Calculated 4.8$1011 2.7$107 11
our case) at that Biot number. Notice that, for the same Biot
Data generation conditions: [ ¼ 2 mm, w0 ¼ 6.47 g, weq ¼ 0.77 g, number but different random diffusion coefficient, somewhat
sw ¼ 0.01 g.ti ¼ {0.5, 1, 1.5,…,9 h}.
different values of SX will be obtained, which will be
36 b i o s y s t e m s e n g i n e e r i n g 1 6 2 ( 2 0 1 7 ) 3 0 e3 9

Fig. 2 e Iterative process for obtaining diffusion and convective transfer coefficients applied to generated data described in
Table 1. At each iteration (i ¼ 1,2,…,7), the logarithm of average dimensionless relative moisture F versus Fourier number Fo
has been depicted for fitting data (open circles), fitted straight line corresponding to first term approximation F1 ðFoi ; Bii Þ
(thick line), exact drying curve corresponding to high accuracy approximation FN ðFoi ; Bii Þ (thin line), and the points over
exact curve corresponding to Fourier numbers of fitting data (filled circles). (a) Initial fitting with all data. (b)e(g) Consecutive
fitting iterations, where the first datum is deleted at each iteration until reaching convergence. Fitting coefficients Di
(10¡11 m2 s¡1) and hi (10¡7 m s¡1) and also c each iteration are indicated. (h) Decimal logarithm of the difference
 
Di ¼ FN ðFoi ; Bii Þ  F1 ðFoi ; Bii Þ at convergence. Values corresponding to deleted data points (open circles) and used fitting
data (filled circles) are depicted. Data error at convergence s7 is represented in dotted line.

statistically characterised by the corresponding mean and


standard deviation.
The results of these simulations are shown in Fig. 3, where
the mean values and the standard deviation values of the
generalised significant figures corresponding to each generated
data set are represented as filled circles and error bars, respec-
tively. Observe that, as expected, optimal results for both co-
efficients jointly are obtained in the range 1  Bi  10. Moreover,
as Biot number increases the accuracy of diffusion coefficient
also increases, whilst the accuracy of convective transfer coef-
ficient falls quickly. Even so, at Bi ¼ 100 the accuracy of transfer
coefficient is not too low. On the other hand, as Biot number
decreases the accuracy of diffusion coefficient falls quickly, and
the accuracy of transfer coefficient also falls, although it de-
creases slower than the diffusion coefficient accuracy. This is
not a surprising behaviour, since the transfer coefficient value is
calculated through Eq. (6) by using the previously obtained
diffusion coefficient. However, until Bi ¼ 0.01 the accuracy of
calculated transfer coefficient is very good.
The iterative process shown in Fig. 2 can be reproduced,
and additional details obtained, by running the MATLAB® pro-
gram with the input data file corresponding to generated data
available in the supplementary material.
Fig. 3 e Generalised significant figures, SD and Sh, obtained
3.2. Determination of coefficients from experimental in the calculation of diffusion (thick line) and convective
data transfer (thin line) coefficients, respectively, as a function
of the Biot number Bi for different simulations performed
The proposed iterative methodology has been applied to under typical conditions in drying experiments (see text
experimental data corresponding to carrot drying for details).
b i o s y s t e m s e n g i n e e r i n g 1 6 2 ( 2 0 1 7 ) 3 0 e3 9 37

experiments. In order to establish the temperature depen- different drying behaviour of core and cortex parts in carrots
dence of diffusion and convective transfer coefficients, and the slightly different core-cortex ratio in each sample.
isothermal drying at different temperatures was performed. Notice that, in order to achieve the one-dimensional behav-
The final fitting at convergence is depicted for each tempera- iour for the thin layer samples, it was not possible to separate
ture in Fig. 4 (top panels) along with the corresponding core and cortex parts.
graphically represented convergence conditions (bottom In this regard, Srikiatden and Roberts (2006) obtained slightly
panels). The obtained diffusion and convective transfer co- higher values of the diffusion coefficient for core tissue than for
efficients are summarised in Table 2 in addition to some cortex tissue in carrots (D. carota L. cv. Red Core Chantenay) cut
sample parameters as Biot number Bi, thickness 2[, width 2[y, into cylindrical samples. Specifically, they found at tempera-
height 2[z, initial weight w0, equilibrium weight weq, and dry tures of 40, 50, 60, and 70  C, the values of 1.01, 1.32, 1.90, and 2.34
matter weight wdm. Note that, in this case, weighing data have (109 m2 s1) for core tissue, and values of 0.76, 0.92, 1.06, and
four significant figures, so that three significant figures have 1.36 (109 m2 s1) for cortex tissue, respectively. Taking into
been assumed for the obtained coefficients. By means of account that carrot samples of Srikiatden and Roberts corre-
simulations as those depicted in Fig. 3, the accuracy of the spond to a different cultivated variety than those used in the
obtained diffusion and convective transfer coefficients has present work, it can be considered that their results and our
been estimated, namely sD ¼ 0.03$109 (m2 s1) and results are in good agreement. Additionally, Markowski (1997)
sh ¼ 0.01$106 (m s1), respectively. found the value h ¼ 1.37$107 (m s1) for convective transfer
Since the main goal of this section is to illustrate the appli- coefficient of carrots (cv. not specified) at T ¼ 60  C and natural
cation of the proposed methodology, for the sake of clarity only convection. Considering that our results correspond to forced
one data set at each temperature has been considered. However, convection, albeit rather at a low air velocity, it seems reason-
in order to obtain a better estimation of the coefficients accu- able that our results are somewhat higher.
racy, accounting correctly for the experimental error, several Moreover, it is important to highlight that, since an
data sets at each temperature should be regarded, and the cor- analytical solution of the diffusion equation under certain
responding error calculated in standard manner. conditions is used, in order to obtain physical coefficients of
As is expected, both diffusion coefficient and convective carrots rather than unphysical best fit parameters, these
transfer coefficient mostly grow as temperature increases. conditions should be approximated in drying experiments, as
Nevertheless, as is shown in Table 2, diffusion coefficient much as possible. Thus, one-dimensional behaviour for the
decreases very slightly from the value at T ¼ 55  C and the thin layer samples is achieved by taking thin layer samples
value at T ¼ 64  C. We assume that this effect is due to the with width and height one order of magnitude greater than

Fig. 4 e Iterative process for obtaining diffusion and convective transfer coefficients applied to experimental data from carrot
slices drying summarised in Table 2. For different temperatures, the logarithm of average dimensionless relative moisture F
versus the Fourier number Fo has been depicted for fitting data (open circles), fitted straight line corresponding to first term
approximation F1 ðFoi ; Bii Þ (thick line), exact drying curve corresponding to high accuracy approximation FN ðFoi ; Bii Þ (thin
line), and the points over exact curve corresponding to Fourier numbers of fitting data (filled circles). (a)e(d) Final fitting at
convergence for temperatures T ¼ 40, 55, 64, 72  C, respectively. (e)e(h) Decimal logarithm of the difference
 
Di ¼ FN ðFoi ; Bii Þ  F1 ðFoi ; Bii Þ at convergence corresponding to temperatures T ¼ 40, 55, 64, 72  C, respectively. Values
corresponding to deleted data points (open circles) and used fitting data (filled circles) are depicted. Data error at
convergence for each temperature si (i ¼ 39,34,78,18) is represented in dotted line. Fitting coefficients Di (10¡9 m2 s¡1) and hi
(10¡6 m s¡1) and also the Biot number calculated at convergence are indicated.
38 b i o s y s t e m s e n g i n e e r i n g 1 6 2 ( 2 0 1 7 ) 3 0 e3 9

Table 2 e Diffusion and convective transfer coefficients obtained for carrot slices and additional sample parameters.
T ( C) D (m2 s1) h (m s1) Bi 2[ (mm) 2[y (mm) 2[z (mm) w0 (g) weq (g) wdm (g)
10
40 7.27$10 6.54$107 1.28 2.85 32.80 61.17 4.795 0.662 0.593
55 1.55$109 1.20$106 1.45 3.75 27.40 62.48 5.450 0.890 0.845
64 1.53$109 1.29$106 1.21 2.87 29.51 62.96 4.986 0.733 0.702
72 2.95$109 2.65$106 1.76 3.92 23.43 52.13 3.986 0.479 0.456

Obtained coefficients accuracy: sD ¼ 0.03$109 m2 s1, sh ¼ 0.01$106 m s1. Weighing device accuracy: sw ¼ 0.001 g. Air velocity: v ¼ 0.71 m s1.

thickness, as is shown in Table 2. Homogeneous initial


moisture M0 can be assumed for fresh carrots preserved in
moisture insulated atmosphere. Additionally, diffusion D and
convective transfer h coefficients must be constant. Since both
coefficients depend on temperature, carrot sample tempera-
ture should be uniform and constant. Sample temperature
homogeneity is achieved by using a microwave device in the
heating process, and it is kept constant by controlling sur-
rounding air temperature, which was monitored by means of
an electronic logger. Notice that convective transfer coeffi-
cient depends also on surrounding air velocity and carrot
sample shape, both conditions being kept constant as is
explained below. Besides, sample moisture at equilibrium Meq
must also be constant, which is achieved by controlling rela-
tive humidity of surrounding air. In order to avoid the relative
humidity increase due to drying process, an extractor fan at
very low velocity was used (generating constant air velocity),
and relative humidity was monitored through an electronic
logger. Finally, shape and size (volume geometry in diffusion
equation) must be constant along drying process. Carrot slices
were sandwiched between two metal grids in order to keep
Fig. 5 e Iterative process applied to unsuitable (non-
the slice shape. Nevertheless, shrinkage is an unavoidable
isothermal) experimental data from carrot slices drying.
effect in carrot drying, which changes size and also shape,
The logarithm of average dimensionless relative moisture
albeit most shrinkage occurs at the initial stages of drying
F versus time t has been depicted for fitting data (open
process, since it is strongly correlated with the moisture
circles), and for the corresponding fitted straight line
decrease. However, the proposed methodology discards initial
logðFÞ ¼ a þ bt (thick line). The unsuitability of data set is
data, where most shrinkage occurs.
detect at first step of process, since fitting intercept a is out
Additionally, a data set within a narrow moisture range has
of range, i.e., a;ð0:21; 0Þ.
been considered, so that shrinkage can be neglected. Notice
that, as verified, weighing data corresponding to a non-
negligible shrinking period lead to a convex (instead of
concave) drying curve, as in the case of non-isothermal drying analytical solution on which our methodology is based is a
described below, being detected by the proposed methodology concave curve (positive second derivative). As a consequence
as unsuitable data. of this feature, fitting intercept a is out of the required range
The sample temperature homogeneity is a remarkable (0.21, 0) in Eq. (19), being a positive value a > 0, and so
condition in order to obtain correct diffusion and convective detecting the unsuitability of data set.
transfer coefficients from drying data fitting. As it has been The iterative process corresponding to each experimental
shown by Srikiatden and Roberts (2006) in drying experiments data set at different temperatures shown in Fig. 4, as well as
with carrots and also with potatoes, convective hot air drying that corresponding to the unsuitable data set, can be repro-
with constant air temperature leads to non-isothermal drying, duced, and additional details obtained, by running the MATLAB®
since a temperature gradient is induced inside samples, giving program with the corresponding input data file available in
experimental drying curves that do not fit the corresponding the supplementary material.
analytical solution of diffusion equation with constant diffu-
sion and transfer coefficients. In this regard, an example of
checking of suitability of data set provided by the proposed 4. Conclusions
iterative methodology in Eq. (19) is shown in Fig. 5. Drying data
in Fig. 5 correspond to a carrot slice sample initially at room Physical drying parameters, namely, mass diffusion and
temperature (~20  C) that is drying at constant air temperature convective mass transfer coefficients, have a significant rele-
of 65  C. Observe that the drying curve given by experimental vance on proper determination of optimal drying conditions in
data is convex (negative second derivative), whilst the convective hot air food drying, in order to achieve the aims of
b i o s y s t e m s e n g i n e e r i n g 1 6 2 ( 2 0 1 7 ) 3 0 e3 9 39

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Appendix A. Supplementary data
determination of temperature dependent mass transfer
coefficients from drying kinetics: Application to solar drying.
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