Microwave Drying of Gelatin Membranes and Dried Product

Properties Characterization

Abstract

Insufficient wound treatment procedures can cause serious repercussions on patients and constitute a
significant health economic burden across the world. Nowadays, biosynthetic polymers like gelatin are
popular due to its outstanding biodegradability, biocompatibility and economical friendly. Gelatin is a
collagen derivative that has comparable qualities as collagen with antibacterial properties. In constructing
gelatin as a wound dressing, drying is one of the essential procedures in fabricating gelatin membranes.
Some drying methods have been applied including freeze drying and convective oven drying. Nevertheless,
these drying methods were limited due to their extended drying duration, adequate quality and most
importantly not cost-effective. This study investigated the feasibility of microwave as an efficient drying
method for the production of gelatin membranes due to its rapid drying time, enhanced product quality and
cost-efficiency. In this research, microwave drying of gelatin membranes was conducted at three microwave
power (180 W, 300 W and 450 W). Results showed that drying kinetics (moisture content and drying rates)
decreased the quickest at the highest microwave power and the slowest at lower microwave power. Five
semi-empirical models were used to describe the thin layer drying kinetics include Newton, Logarithmic,
Page, Verma and Hii and Law models. Hii and Law model was the best in characterising the thin-layer
microwave drying kinetics. The effective diffusivity (Deff) coefficients, activation energies, and specific
energy consumption were also determined. FTIR analysis proved that microwave drying successfully
exposed hydrophobic groups in gelatin and improved its amphiphilicity. FESEM analysis certified that
microwave drying failed to create rough surfaces on the gelatin membranes.

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1. Introduction

1.1. Background

Gelatin is a biopolymer with intriguing features that have sparked the interest of many
biomedical researchers, due to its mild antigenicity, cost efficiency, excellent biodegradability, and
physiological biocompatibility (Dias et al., 2017). Gelatin membranes exhibit excellent wound
dressing capabilities because they contain collagen which is the major component of the
extracellular matrix involved in scar formation as a secondary process of healing after wound
contraction (Rittié, 2016). Drying is one of the most important steps in preparing gelatin
membranes and several methods such as convective oven drying and freeze drying have been
utilized in the treatment of gelatin membrane (Martucci et al., 2012; Sghayyar et al., 2020).
Nonetheless, these drying processes have a few drawbacks which include prolonged drying period,
mediocre quality, unappealing color/appearance, problematic flavor/aroma, and relatively pricey.
This leads to the research of another drying method which is microwave drying with high
efficiency and has been quite popular lately. Drying of gelatin membrane is essential to improve
its weak mechanical strength and degradation in vivo as well as modifying the state of molecular
interactions between polymer chains to regulate its physiochemical properties, especially in
microwave drying (Haider et al., 2008; Kuang et al., 2021). Microwave drying has some
dominances over conventional drying methods including enhanced drying rates, less energy
consuming and better product quality (Demiray et al., 2017; Hii et al., 2021). Therefore, microwave
drying of gelatin membranes was attempted in this study in which the drying kinetics of the
membranes were studied in detail. This was the novelty of the current study.

1.2. Literature review

Microwave-assisted techniques can be employed as a thermal cross-linking in treating gelatin

(Kuang et al., 2021). Microwave radiation is transferred to the materials, transformed into
molecular kinetic energy, and dispersed by molecules because of the inertial, elastic, and frictional
forces of the surroundings. Microwave-assisted technique has been proposed as one of the most
effective ways for improving the molecular and physicochemical properties of gelatin such as gel
strength, viscosity, melting point, and gelling point (Mirzapour-Kouhdasht et al., 2019). Moreover,
the application of microwave treatment is much less time consuming compared to other
conventional methods. The parameters affecting microwave-assisted cross-linking include
microwave power and microwave exposure time (Kuang et al., 2021). The higher the power of the
microwave, less irradiation time is required. Further heating of microwave can cause the gelatin
membrane to be burnt and stiff. Therefore, optimization of these parameters is essential to
synthesize gelatin membrane with desirable properties for enhanced wound healing.
The drying kinetics of gelatin membranes can be determined from their transport properties
which involve thermal conductivity, thermal diffusivity, moisture diffusivity and interface heat,
and mass transfer coefficients (Demiray et al., 2017). Microwave drying kinetics has been
evaluated on several studies such as drying of bamboo shoot slices (Bal et al., 2010), drying of
onion slices (Demiray et al., 2017), drying of green soybean (Cao et al., 2017), and drying of shallot
(Hii et al., 2021).
The drying rate was crucially affected by microwave output power in the study of drying of
onion slices (thickness of 7 ± 1 mm) by Demiray et. where greater microwave output power
resulted in quicker drying process. Similar findings were found in drying of shallot (thickness of
6.5 ± 0.5 mm) by Hii et. and drying of bamboo shoot slices (thickness of 3.4 ± 0.2 mm) by Bal et.
. The drying curves in these studies presented that higher microwave output gave more distinct
falling rate period than that at lower microwave output. Figure 1 represents a drying curve diagram
of microwave treatment with each stage indicated. It can be observed that the rate of conventional
drying of sample decreases after it passes the constant rate zone, which requires more time to dry
the samples completely. With the assist of microwave treatment, the drying rate of sample can

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remain constant after it passes the constant rate zone. Therefore, the duration of drying process can
be reduced.

Figure 1. Effect of microwave treatment on drying curve (Pusat et al., 2016)

There are several mathematical models of drying curves for the samples which include Page’s
model, Newton’s model, Logarithmic model, and Two-term model. These thin layer models
provide some understanding of the transport processes during the falling rate period (Mühlbauer
& Müller, 2020). The shape of the samples must be idealized as a sphere, slab, cylinder, or cuboid
in order to solve the equation (Mühlbauer & Müller, 2020).The drying curve shows how moisture
varies over time, whereas the drying rate curve shows how the drying ratio (moisture change per
unit time) changes over time. According to Hii et al. and Demiray et al., the most excellent
mathematical model fitting curve for their samples was Page’s model.
The effective moisture diffusivity of the drying processes can be determined using the Fick’s
second law. The determination of effective diffusivity is essential to develop the mathematical
modelling of drying process as well as analysing, designing and optimizing the heat and mass
transfer (Khan et al., 2016). The study by Hii et al. and Bal et al. showed that higher microwave
power output resulted in higher effective diffusivity values. Additional heating energy enhanced
the activity of water molecules at higher microwave power, resulting in greater effective moisture
diffusivity (Demiray et al., 2017).

1.3. Problem statement

Treatments of both chronic and acute wounds have become condemnatory menaces for
healthcare systems globally. They require adequate medical treatment to avoid microbial infections
and other unfavorable circumstances that might cause delayed wound healing. In 2018, The cost
of wound treatment for chronic injuries in the United States was 20 billion USD annually
(Aderibigbe & Buyana, 2018). In 2019, the global market cost of chronic wound care was $10.12
billion USD and was predicted to surge to 16.36 billion USD by 2027 (Ndlovu et al., 2021). These
data show the devastating socio-economic effects of wound treatment over the world, highlighting
the urgent need to produce cost-effective wound dressings.
Interactive/artificial wound dressings are frequently formulated from synthetic polymers and
biopolymers (Ndlovu et al., 2021) which are originated from gelatin, alginate, chitosan, and etc.
They are typically made up of transparent polymeric films and structures that are permeable to
water vapor and oxygen but not to germs (Ndlovu et al., 2021). Gelatin membranes as a wound
dressings have the advantages of being affordable and efficient, as well as having a longer life span
(Moeini et al., 2020). The success of this study can aid in the creation of wound dressings applying

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microwave as post-treatment of gelatin membrane is less expensive and more biocompatible which
lead to reduce in financial and mental toll that chronic and acute wounds had on patients (Kuang
et al., 2021).
Amidst the ease of fabrication as a wound dressing material, gelatin membrane has limitations
where its high hydrophilicity and low mechanical strength restrict its broad application in tissue
engineering (Beishenaliev et al., 2019). In specific, extended exposure to dampness can
compromise its structural integrity. As an outcome, the gelatin membrane will completely degrade
and lose its functionality. Thus, post-treatment such as thermal crosslinking is needed to increase
mechanical strength and decrease the degradation rate of gelatin membrane.

1.4. Objectives

The primary goal of this research is to dry gelatin membranes using microwave and to model
the drying kinetics. The study of drying kinetics is required to determine effective drying
technologies and to control the drying process. It aids in understanding the progress of moisture
removal and determining the best drying settings without the need of full-scale studies (Delfiya et
al., 2021). Thus, research was conducted by drying gelatin membranes using a microwave oven
with the following objectives:
 To determine the microwave drying kinetics of gelatin membranes.
 To model the drying of gelatin membranes using thin later drying models.
 To determine the effective diffusivities and activation energies of microwave drying of
gelatin membranes.
 To determine the specific energy consumption of microwave drying of gelatin
membranes.
 To study the effect of microwave drying on the functional groups of gelatin membranes.
 To characterize the surface morphology of the gelatins after microwave drying.

2. Materials and Methods

2.1. Drying experiment

Gelatin (R&M Chemicals) was purchased from R&M Chemicals in Malaysia. Three different
concentrations of gelatin (10 wt%, 15 wt% and 20 wt%) were prepared in this study. The gelatin
powder was dissolved in distilled water by using a hotplate and a magnetic stirrer at 45˚C and 500
rpm.
Subsequently, the gelatin solution was transferred into a 240-mL round plastic container and
subjected to microwave drying. The drying experiments were performed using a programmable
microwave oven (Model C-103FL, Samsung) which has a cavity with a dimension of 0.34 m ×
0.34 m × 0.22 m. The samples were placed on the rotating glass turntable and the microwave
drying was performed at three power settings (180 W, 300 W and 450 W). The drying was
conducted until equilibrium moisture content was achieved (constant weights) at 180 W, 300 W
and 450 W correspondingly. All the experiments were replicated thrice to acquire the mean values.

2.2. Drying kinetics

The weight of the gelatin membranes was evaluated by measuring the membrane every 1 min.
The gelatin membranes were weighed using an analytical balance (Metler Toledo, USA). Moisture
content (Mt) of each membrane was determined using Equation (1) (Hii et al., 2009).

𝑀𝑎𝑠𝑠 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒 (𝑔) − 𝐵𝑜𝑛𝑒 𝑑𝑟𝑦 𝑚𝑎𝑠𝑠 (𝑔)

𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝑐𝑜𝑛𝑡𝑒𝑛𝑡: 𝑀𝑡 = (1)
𝐵𝑜𝑛𝑒 𝑑𝑟𝑦 𝑚𝑎𝑠𝑠 (𝑔)

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 Bone dry mass was obtained by subjecting the final dried samples in an air ventilated oven
(Model Oven 100-800, Memmert) at 105 ˚C for 18 hours.
Drying rates (g water/g dry solid.hr) for the membranes were obtained by taking the gradient at
each data point along the moisture content profile.

2.3. Mathematical modelling

Thin layer modelling were executed using Newton, Logarithmic, Page, Verma and Hii and Law
models (Hii et al., 2009) as shown in Table 1. The purpose for employing these models was to
assess the accuracy of fitting based on the number of constants in the models which was three
constants (‘a’, ‘k’, and ‘c’ in Logarithmic), two constants (‘k’ and ‘n’ in Page), three constants
(‘a’, ‘k1’, and ‘k2’ in Verma), one constant (‘k’ in Newton) and five constants (‘a’, ‘b’, ‘k’, ‘g’,
and ‘n’ in Hii and Law). Hii and Law model was a new model developed in the study of cocoa
bean drying which combine Page and two-term drying models (Hii et al., 2009).

Table 1. Semi-empirical thin layer drying models.

Model Equation
Logarithmic 𝑀𝑅 = 𝑎. 𝑒𝑥𝑝−𝑘𝑡 + 𝑐 (2)
−𝑘𝑡 𝑛
Page 𝑀𝑅 = 𝑎. 𝑒𝑥𝑝 (3)
−𝑘1 𝑡 −𝑘2 𝑡
Verma 𝑀𝑅 = 𝑎. 𝑒𝑥𝑝 + (1 − 𝑎)𝑒𝑥𝑝 (4)
Newton 𝑀𝑅 = 𝑎. 𝑒𝑥𝑝−𝑘𝑡 (5)
Hii and Law −𝑘𝑡 𝑛 −𝑔𝑡 𝑛 (6)
𝑀𝑅 = 𝑎. 𝑒𝑥𝑝 + 𝑏. 𝑒𝑥𝑝

where MR = moisture ratio, Mi = initial moisture content and Me = equilibrium moisture content
as presented in Equation (7).

𝑀𝑡 − 𝑀𝑒
𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 𝑟𝑎𝑡𝑖𝑜: 𝑀𝑅 = (7)
𝑀𝑖 − 𝑀𝑒

Non-linear regression studies were carried using Excel SOLVER (MS office, USA) to assess and
identify the constants (‘a’, ‘b’, ‘c’, ‘g’, ‘k’, ‘k1’, ‘k2’, ‘g’, and ‘n’) of the designated models by
minimizing the sum of the squared residuals (SSR) as given in Equation (8). The studies were
carried out on the mean moisture ratio values calculated from the experimental moisture content.
As stated in Equations (9) - (11), the models were examined for root mean square error (RMSE),
coefficient of determination (R2), and Chi square (Χ2). The finest model preferred was the one
with least RMSE and Χ2 while having the greatest R2 value.
𝑁
𝑆𝑆𝑅 = ∑ (𝑀𝑅𝑝𝑟𝑒 − 𝑀𝑅𝑒𝑥𝑝 )2 (8)
𝑖=1

∑𝑁
𝑖=1(𝑀𝑅𝑝𝑟𝑒 − 𝑀𝑅𝑒𝑥𝑝 )
2
𝑅2 = 1 − (9)
∑𝑁 ̅̅̅̅̅
𝑖=1(𝑀𝑅𝑝𝑟𝑒 − 𝑀𝑅𝑒𝑥𝑝 )
2

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 2
∑𝑁
𝑖=1(𝑀𝑅𝑝𝑟𝑒 − 𝑀𝑅𝑒𝑥𝑝 )
2
𝛸 = (10)
(𝑁 − 𝑧)
1
1 𝑁 2
𝑅𝑀𝑆𝐸 = [( ) ∑ (𝑀𝑅𝑝𝑟𝑒 − 𝑀𝑅𝑒𝑥𝑝 )2 ] (11)
𝑁 𝑖=1

where subscripts exp and pre signify experimental and predicted values at each drying time
correspondingly. The number of observations and constants are expressed as N and z respectively.

2.4. Effective diffusivity and activation energy

The thicknesses of the membranes were required in estimating effective diffusivity coefficients
in the study and they were measured using micrometer. Fick’s second law which is presented in
Equation (12) was applied to determine effective moisture diffusivity by assuming the geometry
as an infinite slab (Westwater & Drickamer, 1975).

8 ∞ 1 −(2𝑛+1)2 𝜋2 𝐷𝑒 𝑡
𝑀𝑅 = 2 ∑ 𝑒𝑥𝑝 4𝐿2 (12)
𝜋 (2𝑛 + 1) 2
𝑛=0

where L is the half thickness of sample (m) and De is the effective diffusivity (m2/s).

By applying the first term (n = 0) to the equation as well as implementing natural log on both
sides of the equation, Equation (12) can be simplified as Equation (13) (Yap et al., 2020).

8 𝜋 2 𝐷𝑒 𝑡
ln 𝑀𝑅 = ln − (13)
𝜋2 4𝐿2

The value of De was obtained from the slope of the linear graph as illustrated in Equation (14).

𝜋 2 𝐷𝑒 𝑡
𝑆𝑙𝑜𝑝𝑒 = (14)
4𝐿2
Once the effective diffusion rate was investigated, the value of the activation energy could be
determined from the slope of the line. Activation energy is defined by the water molecules crossing
over the energy barrier when there is a moisture transfer within the product (Çelen, 2019). In the
drying process, lower activation energy values resulted in higher moisture diffusion values. The
rise in average energies of water molecules caused a reduction in the activation energy of
the process (Çelen, 2019). The activation energy was calculated using Arrhenius equation as
shown in Equation (15) (Zarein et al., 2015).

𝐸𝐴 𝑚
𝐷𝑒 = 𝐷𝑜 𝑒𝑥𝑝 (− ) (15)
𝑃
where Do is a constant equivalent to diffusivity at the infinite temperature (m2/s), EA is activation
energy (W/g), and m (g) is the mass of the raw product.
By applying natural log on both sides of the equation, Equation (15) can be simplified as
Equation (16).

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 𝑚
ln𝐷𝑒 = ln𝐷𝑜 − 𝐸𝐴 ( ) (16)
𝑃

2.5. Specific energy consumption and drying energy performance

The investigation of specific energy consumption is one of the forms to represent the
performance of a drying system. Specific energy consumption is known as the relation between
supplied energy (can be fuel and electrical) and the mass of evaporated water (Jokiniemi et al.,
2016). Specific energy consumption is a highly advantageous and practical number in energy
analysis (Azmi et al., 2019). Equation (17) was used to compute the microwave drying energy
consumption, whereas Equation (18) was used to determine the specific energy consumption
(Darvishi et al., 2013).

𝐸𝑐 = 𝑃 × 𝑡 (17)
𝑃 × 𝑡 × 10−6
𝐸𝑠 = (18)
𝑚𝑒𝑣
where Es is the specific energy consumption (MJ/kg water), P is the microwave power (W), t is
the drying time (s), and mev is the total mass of evaporated water (kg).

2.6. Fourier transform infrared analysis of gelatin membranes

Fourier transform infrared spectroscopy (FTIR; PerkinElmer, USA) in attenuated total reflection
(ATR) mode was used to confirm the existence of functional groups in gelatin membranes before
and after microwave drying. FTIR functions by exposing gelatin membranes to infrared radiation
throughout a wavenumber range of 400 to 4000 cm-1 utilizing 16 scans at a resolution of 8 cm-1.
The molecules in the samples specifically absorbed light of a certain wavelength, leading them to
transition from their ground state to excited state. This activity is represented by an infrared
spectrum which is defined as transmittance or absorbance against wavenumber where the
wavenumber of the peak identifies the presence of chemical compounds. Prior to the analysis, a
tiny piece of gelatin membrane (1 cm x 1 cm) was cut and placed on the sample loading area.
Gelatin powder was also examined using FTIR to confirm its functional groups.

2.7. Surface morphology of gelatin membranes

The surface morphology of gelatin membrane was examined by using a field emission scanning
electron microscope (FESEM; Quanta 400F, FEI, USA) in low vacuum mode and at an
accelerating voltage of 5 to 20 kV. A FESEM is a high-magnification electron microscope that is
used to visualize the surface morphology of an item. It scans an item by using electrons from a
field emission source and accelerating them in a high electrical field gradient. The secondary
electrons released from each point of the item will be caught by a detector, resulting in an electrical
signal that will be analyzed using Image J software (version 1.51u) to produce pictures depending
on the angle and velocity of these electrons. Prior to the analysis, a gelatin membrane was taped to
a sample holder using conductive carbon tape. Approximately four areas of the gelatin membrane
were viewed.

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3. Results and Discussion

3.1. Drying kinetics

Figures 2,3 and 4 illustrate the changes in moisture contents of gelatin membranes of 10 wt%,
15 wt% and 20 wt% respectively during microwave drying. They show similar trend of the falling
moisture contents over the time at 3 different designated powers. It could be noticed that within
the recorded drying time which ranged from 5 to 15 min, the moisture content diminished
exponentially. Drying gelatin at 450 W resulted in the least drying time when compared to those
at 180 W and 300 W. This is mostly owing to the elevated excitement of water molecules at higher
microwave power. Additionally, rapid heating rate facilitates improved heat transfer within the
membranes and allows the internal moisture to evaporate to the surface. This inevitably improves
mass transfer which results in a faster drying time (Haghi & Amanifard, 2008). A study related to
microwave drying kinetics of onion slices by Demiray et al. also gave similar curves where the
higher microwave output power generated steeper curve compared to those at lower microwave
output power. As the microwave output power was reduced from 450 W to 180 W, the curves
generated became shallower which proved that lower microwave output power required longer
drying duration.

0.80

0.70
180 W
0.60 300 W
MOISTURE CONTENT

450 W
0.50

0.40

0.30

0.20

0.10

0.00
0 2 4 6 8 10 12 14 16
TIME (MIN)

Figure 2. Variation of moisture contents of gelatin membrane of 10 wt% against microwave drying time.

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 0.80

0.70 180 W
300 W
0.60
450 W
MOISTURE CONTENT

0.50

0.40

0.30

0.20

0.10

0.00
0 2 4 6 8 10 12 14
TIME (MIN)

Figure 3. Variation of moisture contents of gelatin membrane of 15 wt% against microwave drying time.

0.70

0.60 180 W
300 W
0.50
MOISTURE CONTENT

450 W

0.40

0.30

0.20

0.10

0.00
0 2 4 6 8 10 12 14 16
TIME (MIN)

Figure 4. Variation of moisture contents of gelatin membrane of 20 wt% against microwave drying time.

Figures 5,6 and 7 display the changes in moisture contents of gelatin membranes of 10 wt%, 15
wt% and 20 wt% concentration consecutively during microwave drying. They show similar trend
of rate periods over the time at 3 different designated powers. It could be observed that microwave
drying at 450 W and 300 W exhibited a more noticeable falling rate periods in contrast to that at

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180 W. Higher microwave power revealed greater overall drying rate which means that microwave
drying at higher power can boost drying rates especially at the beginning of the drying process
where the product moisture content was larger, and the gelatin membranes were able to absorb
more microwave radiation to speed up the drying process. The findings from Demiray et al. on the
drying of onion slices (thickness of 7 ± 1 mm) showed similar curves where higher microwave
output power produced more obvious falling rate periods when compared to those of lower
microwave output power.

-2.50

-2.00
Drying Rate (g/min)

-1.50
180 W
300 W
-1.00 450 W

-0.50

0.00
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80
Moisture Content

Figure 5. Variation of drying rates with moisture contents for microwave drying of 10% concentration of
gelatin.

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 -2.50

-2.00
Drying Rate (g/min)

-1.50
180 W
300 W
-1.00 450 W

-0.50

0.00
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70 0.80
Moisture Content

Figure 6. Variation of drying rates with moisture contents for microwave drying of 15% concentration of
gelatin.

-2.50

-2.00
Drying Rate (g/min)

-1.50
180 W
300 W
-1.00 450 W

-0.50

0.00
0.00 0.10 0.20 0.30 0.40 0.50 0.60 0.70
Moisture Content

Figure 7. Variation of drying rates with moisture contents for microwave drying of 20% concentration of
gelatin.

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3.2. Mathematical modelling

Tables 2 – 10 manifest the drying constants as well as the statistical parameters (R2, Χ2 and
RMSE) obtained from regression analyses. The R2 values for all models range from 0.9717 to
0.9991, whereas Χ2 and RMSE values range from 0.0002 to 0.0048 and 0.0105 to 0.0554
progressively. It can be observed that Hii and Law model showed the greatest R2 values and the
least Χ2 and RMSE values in all drying experiments. This implies that Hii and Law model
surmounted other models and is the finest in designating the thin layer drying kinetics of the gelatin
membranes. Other findings such as microwave drying of onion slices (thickness of 7 ± 1 mm) by
Demiray et al. and microwave drying of shallot (thickness of 6.5 ± 0.5 mm) by Hii et al. concluded
that Page model had the best fittings in thin layer modelling. However, their studies didn’t apply
Hii and Law model as their nominated semi-empirical thin layer models. Moreover, findings by
Bal et al. on the drying of bamboo shoot slices (thickness of 3.4 ± 0.2 mm) came to terms that
Wand and Singh model is the most suitable thin layer drying model among other models including
Page model and excluding Hii and Law model. Therefore, it can be said that every divergent
method of drying or subject to be dried might has different befitting thin later drying kinetics.

Table 2. Results of mathematical modelling (10 wt% concentration gelatin; MW power = 180 W).
Model Constant R2 Χ2 RMSE
Logarithmic a = 1.065, c = 0.000, k = 0.222 0.9805 0.0025 0.0448
Page k = 0.116, n = 1.339 0.9964 0.0004 0.0193
Verma a = 0.000, k1 = 0.001, k2 = 0.210 0.9759 0.0031 0.0498
Newton k = 0.210 0.9759 0.0026 0.0498
Hii and Law a = 0.966, b = 0.005, g = 0.108, k = 0.100, n= 1.401 0.9970 0.0004 0.0176

Table 3. Results of mathematical modelling (10 wt% concentration gelatin; MW power = 300 W).
Model Constant R2 Χ2 RMSE
Logarithmic a = 1.055, c = 0.000, k = 0.391 0.9808 0.0030 0.0464
Page k = 0.232, n = 1.399 0.9982 0.0003 0.0143
Verma a = 8.519, k1 = 0.673, k2 = 0.749 0.9972 0.0004 0.0177
Newton k = 0.374 0.9775 0.0028 0.0501
Hii and Law a = 0.985, b = 0.003, g = 0.216, k = 0.222, n= 1.424 0.9983 0.0003 0.0137

Table 4. Results of mathematical modelling (10 wt% concentration gelatin; MW power = 450 W).
Model Constant R2 Χ2 RMSE
Logarithmic a = 1.034, c = 0.000, k = 0.605 0.9837 0.0032 0.0444
Page k = 0.429, n = 1.419 0.9991 0.0002 0.0106
Verma a = 9.179, k1 = 1.086, k2 = 1.206 0.9984 0.0003 0.0139
Newton k = 0.589 0.9823 0.0024 0.0462
Hii and Law a = 0.997, b = 0.000, g = 0.376, k = 0.425, n= 1.424 0.9991 0.0002 0.0105

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 Table 5. Results of mathematical modelling (15 wt% concentration gelatin; MW power = 180 W).
Model Constant R2 Χ2 RMSE
Logarithmic a = 1.064, c = 0.000, k = 0.237 0.9784 0.0029 0.0476
Page k = 0.123, n = 1.355 0.9960 0.0005 0.0205
Verma a = 1.162, k1 = 0.257, k2 = 17.120 0.9853 0.0020 0.0393
Newton k = 0.224 0.9736 0.0030 0.0526
Hii and Law a = 0.966, b = 0.005, g = 0.116, k = 0.107, n= 1.420 0.9967 0.0005 0.0187

Table 6. Results of mathematical modelling (15 wt% concentration gelatin; MW power = 300 W).
Model Constant R2 Χ2 RMSE
Logarithmic a = 1.050, c = 0.000, k = 0.424 0.9786 0.0038 0.0503
Page k = 0.259, n = 1.407 0.9975 0.0004 0.0171
Verma a = 8.830, k1 = 0.736, k2 = 0.816 0.9963 0.0006 0.0207
Newton k = 0.407 0.9755 0.0033 0.0538
Hii and Law a = 0.986, b = 0.002, g = 0.252, k = 0.250, n= 1.429 0.9977 0.0004 0.0166

Table 7. Results of mathematical modelling (15 wt% concentration gelatin; MW power = 450 W).
Model Constant R2 Χ2 RMSE
Logarithmic a = 1.029, c = 0.000, k = 0.658 0.9828 0.0045 0.0477
Page k = 0.487, n = 1.419 0.9990 0.0004 0.0113
Verma a = 0.596, k1 = 0.643, k2 = 0.643 0.9816 0.0048 0.0492
Newton k = 0.643 0.9816 0.0029 0.0492
Hii and Law a = 0.998, b = 0.000, g = 0.371, k = 0.484, n= 1.422 0.9990 0.0002 0.0113

Table 8. Results of mathematical modelling (20 wt% concentration gelatin; MW power = 180 W).
Model Constant R2 Χ2 RMSE
Logarithmic a = 1.072, c = 0.000, k = 0.251 0.9772 0.0031 0.0494
Page k = 0.121, n = 1.405 0.9969 0.0004 0.0182
Verma a = 1.192, k1 = 0.277, k2 = 14.289 0.9856 0.0019 0.0393
Newton k = 0.236 0.9717 0.0033 0.0550
Hii and Law a = 0.967, b = 0.005, g = 0.107, k = 0.106, n= 1.468 0.9975 0.0004 0.0165

Page | 13
 Table 9. Results of mathematical modelling (20 wt% concentration gelatin; MW power = 300 W).
Model Constant R2 Χ2 RMSE
Logarithmic a = 1.046, c = 0.000, k = 0.438 0.9772 0.0044 0.0523
Page k = 0.275, n = 1.402 0.9966 0.0005 0.0202
Verma a = 7.083, k1 = 0.750, k2 = 0.853 0.9953 0.0009 0.0237
Newton k = 0.422 0.9744 0.0035 0.0554
Hii and Law a = 0.985, b = 0.002, g = 0.265, k = 0.265, n= 1.426 0.9968 0.0005 0.0197

Table 10. Results of mathematical modelling (20 wt% concentration gelatin; MW power = 450 W).
Model Constant R2 Χ2 RMSE
Logarithmic a = 1.028, c = 0.000, k = 0.735 0.9797 0.0055 0.0526
Page k = 0.537, n = 1.518 0.9990 0.0002 0.0120
Verma a = 7.478, k1 = 1.392, k2 = 1.623 0.9982 0.0005 0.0158
Newton k = 0.720 0.9787 0.0035 0.0539
Hii and Law a = 0.998, b = 0.000, g = 0.367, k = 0.534, n= 1.527 0.9990 0.0002 0.0119

Figures 8 – 16 represent fitting of the experimental data to the diverse thin layer models. It can
be observed that Page and Hii and Law models fitted the experimental data the best among all
other models. Despite that, Hii and Law model outmatched Page model based on the values of R2,
Χ2 and RMSE values.

1.0
0.9
0.8
0.7
0.6
MR

0.5
0.4
0.3
0.2
0.1
0.0
0 2 4 6 8 10 12 14 16
Time (min)

180 W Logarithmic Page

Verma Newton Hii and Law

Figure 8. Variation of thin layer model fittings to experimental data (10 wt% concentration gelatin; MW
power = 180 W).

Page | 14
 1.0

0.9

0.8

0.7

0.6
MR

0.5

0.4

0.3

0.2

0.1

0.0
0 2 4 6 8 10 12
Time (min)

300 W Logarithmic Page Verma Newton Hii and Law

Figure 9. Variation of thin layer model fittings to experimental data (10 wt% concentration gelatin; MW
power = 300 W).

1.0

0.9

0.8

0.7

0.6
MR

0.5

0.4

0.3

0.2

0.1

0.0
0 1 2 3 4 5 6 7 8
Time (min)

450 W Logarithmic Page Verma Newton Hii and Law

Figure 10. Variation of thin layer model fittings to experimental data (10 wt% concentration gelatin; MW
power = 450 W).

Page | 15
 1.0

0.9

0.8

0.7

0.6
MR

0.5

0.4

0.3

0.2

0.1

0.0
0 2 4 6 8 10 12 14
Time (min)

180 W Logarithmic Page Verma Newton Hii and Law

Figure 11. Variation of thin layer model fittings to experimental data (15 wt% concentration gelatin; MW
power = 180 W).

1.0

0.9

0.8

0.7

0.6
MR

0.5

0.4

0.3

0.2

0.1

0.0
0 1 2 3 4 5 6 7 8 9
Time (min)

300 W Logarithmic Page Verma Newton Hii and Law

Figure 12. Variation of thin layer model fittings to experimental data (15 wt% concentration gelatin; MW
power = 300 W).

Page | 16
 1.0

0.9

0.8

0.7

0.6
MR

0.5

0.4

0.3

0.2

0.1

0.0
0 1 2 3 4 5 6
Time (min)

450 W Logarithmic Page Verma Newton Hii and Law

Figure 13. Variation of thin layer model fittings to experimental data (15 wt% concentration gelatin; MW
power = 450 W).

1.0

0.9

0.8

0.7

0.6
MR

0.5

0.4

0.3

0.2

0.1

0.0
0 2 4 6 8 10 12 14 16
Time (min)

180 W Logarithmic Page Verma Newton Hii and Law

Figure 14. Variation of thin layer model fittings to experimental data (20 wt% concentration gelatin; MW
power = 180 W).

Page | 17
 1.0

0.9

0.8

0.7

0.6
MR

0.5

0.4

0.3

0.2

0.1

0.0
0 1 2 3 4 5 6 7 8
Time (min)

300 W Logarithmic Page Verma Newton Hii and Law

Figure 15. Variation of thin layer model fittings to experimental data (20 wt% concentration gelatin; MW
power = 300 W).

1.0

0.9

0.8

0.7

0.6
MR

0.5

0.4

0.3

0.2

0.1

0.0
0 1 2 3 4 5 6
Time (min)

450 W Logarithmic Page Verma Newton Hii and Law

Figure 16. Variation of thin layer model fittings to experimental data (20 wt% concentration gelatin; MW
power = 450 W).

Page | 18
3.3. Effective diffusivity and activation energy

Table 11 demonstrates the effect of thickness of the gelatin membranes on diffusion coefficients
where both increased collaterally. The thicknesses of the membranes measured were 4.5 × 10-6 m,
6.0 × 10-6 m, and 8.0 × 10-6 m for 10 wt%, 15 wt% and 20 wt% of gelatin membranes respectively.
It can also be seen that effective diffusivity improved in conjunction with the microwave power
and this finding is similar to another study which was about the effect of microwave drying on
energy efficiency in the drying of apple slices by Zarein et. . The calculated effective diffusivity
coefficients in this study ranged from 9.74 × 10-15 m2/s at 180 W to 1.12 × 10-13 m2/s at 450 W.
The calculated rate of diffusions were much lower than those estimated by Çelen in the microwave
drying of Trabzon persimmon (thickness of 5, 7 and 9 mm) which gave effective diffusivity
coefficients ranging from 2.97 × 10-8 m2/s at 120 W to 4.10 × 10-6 m2/s at 460 W. Similarly, the
calculated diffusions rate in this study was also lower than those reported by Hii et al. microwave
drying of shallot (thickness of 6.5 ± 0.5 mm) which generated rate of diffusions ranging from 0.70
× 10-5 m2/s at 180 W to 3.69 × 10-5 m2/s at 450 W. Furthermore, the activation energy in this study
was determined from the change of lnDeff in compliance with m/P as illustrated in Figure 17. The
calculated activation energies were 60.475 W/g, 51.853 W/g, and 53.645 W/g and they were
greater than those reported by Çelen. The microwave drying of Trabzon persimmon (thickness of
5, 7 and 9 mm) in their study were 32.820 W/g, 18.640 W/g, and 12.800 W/g correspondingly.

20% gelatin 15% gelatin 10% gelatin

0.01 0.015 0.02 0.025 0.03 0.035

-25.5

-26

-26.5
ln Deff

-27

-27.5

-28

-28.5
m/P (g/W)

Figure 17. The effects of microwave power on effective diffusion coefficients.

Page | 19
Table 11. The diffusion rates and activation energy of the gelatin membranes at different thicknesses and
powers.
De (m2/s)
Microwave Power (W)
4.5 × 10-6 m 6.0 × 10-6 m 8.0 × 10-6 m
180 9.74 × 10-15 1.75 × 10-14 3.62 × 10-14
300 2.01 × 10-14 3.34 × 10-14 5.79 × 10-14
450 3.33 × 10-14 4.98 × 10-14 1.12 × 10-13
EA (W/g) 60.475 51.853 53.645

3.4. Specific energy consumption and drying energy performance

Figures 18 and 19 depict the overall energy consumption and specific energy consumption of
microwave drying of gelatin membranes. At varying powers, membrane with thickness of 4.0 ×
10-6 m consumed 0.045 to 0.053 kWh, membrane with thickness of 6.0 × 10-6 m consumed 0.038
to 0.040 kWh, while membrane with thickness of 8.0 × 10-6 m consumed 0.035 to 0.042 kWh. As
the power of the microwave increased, the drying time of gelatin membranes was also reduced.
The findings from Demirel & Ismail and Çelen also stated that higher microwave power led to
declination of drying duration and energy consumed. The specific energy consumption for 10 wt%,
15 wt% and 20 wt% gelatin membranes bound from 29.908 to 34.594 MJ/kg water, 25.978 to
27.817 MJ/kg water, and 25.575 to 30.607 MJ/kg water at different powers. This study also
showed that 10 wt% gelatin consumed more energy compared to 15 wt% and 20 wt% gelatins
because more water content demanded to reach evaporation temperature and the energy drained
on evaporation surged (Çelen, 2019).

0.06
0.05
Ec (kWh)

0.04
0.03
0.02
0.01
0
180 300 450
Microwave Power (W)

10 wt% gelatin 15 wt% gelatin 20 wt% gelatin

Figure 18. Energy consumption of microwave drying of gelatin membranes of different concentration at
different powers.

Page | 20
 40
35

Es (MJ/kg water)
30
25
20
15
10
5
0
180 300 450
Microwave Power (W)

10 wt% gelatin 15 wt% gelatin 20 wt% gelatin

Figure 19. Specific energy consumption of microwave drying of gelatin membranes of different
concentration at different powers.

3.5. Fourier transform infrared analysis of gelatin membranes

The FTIR analysis was performed on pure gelatin powder and gelatin membranes after
microwave drying at different microwave power. Figure 20 illustrates the FTIR spectrum of pure
gelatin powder where it gives strong peaks at 1520 cm-1 (amide II) and 1626 cm-1 (amide I).
Distinct bands were also found at 1080 cm-1, 1238 cm-1 (amide III), 1336 cm-1, 1454 cm-1, 2932
cm-1, 3072 cm-1 (amide B) and 3262 cm-1 (amide A). The characterization of the infrared bands
was based on the study of FTIR spectroscopic analysis of protein secondary structures conducted
by Kong & Yu in 2007. The peaks at 3262 cm-1 and 3072 cm-1 were generally attributed to N–H
stretching of the amide A and B band proportionately, the peak at 1626 cm-1 was specified to a
characteristic of amide I band which resulted from C=O stretching vibration, C–N stretching or
N–H bending of gelatin, and the peaks at 1520 cm-1 and 1238 cm-1 were credited to N–H bending
or C–N stretching vibration of the amide II and III band of gelatin (Ma et al., 2017). The
observation on the functional groups of the pure gelatin in this study issues similar characteristics
of those discovered by Hossan et. al in the study of preparation and characterization of gelatin-
hydroxyapatite composite for bone tissue engineering.

Page | 21
 3262 2932
%T

3072 1080
1336

1454
1626
1238
1520

4000 3600 3200 2800 2400 2000 1600 1200 800 400
Wavenumber (cm-1)

Figure 20. FTIR spectrum of pure gelatin powder

Figure 21 represents that the spectra of all gelatin membranes of different concentrations
subjected to microwave drying at three different microwave powers are quite similar to that of
gelatin powder. As the microwave power increased, the peak of amide A band of the gelatin
membranes at three different concentrations shifted to greater wavenumber (3264 to 3278 cm-1)
which stipulate that less N–H groups engage in hydrogen bond formation, making it difficult to
generate a three-helix shape during gel formation (Chen et al., 2018; Zhang et al., 2019). On the
other hand, the peak of amide I band of all gelatin membranes bore to smaller wavenumber (1634
to 1620 cm-1) as the microwave power went up, disrupting molecular conformation of
gelatin which forged more intramolecular hydrogen bonds and strengthened the disordered
structure of gelatin, enabling it easier to expose hydrophobic groups in gelatin and enhance its
amphiphilicity (Ahmad & Benjakul, 2011; Chen et al., 2018). These findings were supported by
the research of the effect of microwave extraction temperature on the chemical structure and oil-
water interface properties of fish skin gelatin performed by Feng et. al (2021) where they reported
that the peak of amide A band switched to higher wavenumber (3370 to 3426 cm-1) and the peak
of amide I band switched to a lower wavenumber (1654 to 1638 cm-1).

Page | 22
 Amide A band Amide I band

Gelatin Powder
10 wt% Gelatin (180 W)
10 wt% Gelatin (300 W)
10 wt% Gelatin (450 W)
%T

15 wt% Gelatin (180 W)

15 wt% Gelatin (300 W)
15 wt% Gelatin (450 W)
20 wt% Gelatin (180 W)
20 wt% Gelatin (300 W)
20 wt% Gelatin (450 W)

4000 3600 3200 2800 2400 2000 1600 1200 800 400
Wavenumber (cm-1)

Figure 21. FTIR spectra of gelatin membranes of different concentrations subjected to microwave drying
at 180W, 300W and 450W.

3.6. Surface morphology

The surface morphology of all gelatin membranes was presented in Figure 22 (a – i). It can be
observed that microwave drying create rough surface on the gelatin membranes and this opposed
to the finding reported by Sundaram et. al in the study of porous scaffold of gelatin-starch with
nanohydroxyapatite composite processed via novel microwave vacuum drying. They successfully
created porous surface on their gelatin composite scaffolds by creating a pressure differential
between the inside and exterior of the tissue via the use of microwave vacuum drying (Sundaram
et al., 2008). Physical activity of the material through the microwave field can enable
electromagnetic energy absorption in microwave vacuum drying. The microwave energy is
immediately absorbed by the material. If this procedure is carried out in vacuum condition, the
material may dry quickly, and pores can form (Scaman & Durance, 2005; Sundaram et al., 2008).
Another opposition was also reported by Sghayyar et al. in the study of fish biowaste gelatin coated
phosphate-glass fibres for wound-healing application utilising freeze drying as the drying method.
Their gelatin coatings seemed to be smooth with huge pores which were resulted by the removal
of ice crystals via sublimation during freeze-drying (Sghayyar et al., 2020).

Page | 23
(A) (B) (C)

10 μm 10 μm 10 μm

(D) (E) (F)

10 μm 10 μm 10 μm

(G) (H) (I)

10 μm 10 μm 10 μm

Figure 22. Surface morphology of gelatin membranes. (A) 10 wt% gelatin 180 W. (B) 10 wt% gelatin
300 W. (C) 10 wt% gelatin 450 W. (D) 15 wt% gelatin 180 W. (E) 15 wt% gelatin 300 W. (F) 15 wt%
gelatin 450 W. (G) 20 wt% gelatin 180 W. (H) 20 wt% gelatin 300 W. (I) 20 wt% gelatin 450 W.

Page | 24
4. Conclusions

Drying of gelatin membranes (10, 15 and 20 wt%) were conducted using microwave at 180 W,
300 W and 450 W. Drying rates were deemed to be the greatest in the 450 W microwave power
output, followed by 300 W and finally 180 W. Hii and Law model was shown to be the most
plausible in describing the thin layer drying behaviors of gelatin membranes. The effective
diffusivity (Deff) coefficients ranged from 9.74 × 10-15 to 1.12 × 10-13 m2/s at microwave power of
180 W and 450 W respectively. The activation energies for gelatin membranes with thicknesses
of 4.5 × 10-6, 6.0 × 10-6, and 8.0 × 10-6 m were 60.475, 51.853, and 53.645 W/g sequentially. The
specific energy consumption for gelatin membranes of 10 wt%, 15 wt% and 20 wt% ranged from
29.908 to 34.594 MJ/kg water, 25.978 to 27.817 MJ/kg water, and 25.575 to 30.607 MJ/kg water
at 180W, 300W and 450W respectively. As the concentration of the gelatin was reduced, the
gelatin absorbed more energy because more water content required to reach evaporation
temperature and the energy wasted on evaporation ascended. Increment in microwave power
shifted the peak of amide A band of the gelatin membranes to greater wavenumber (3264 to 3278
cm-1) which specified that less N–H groups engaged in hydrogen bond formation,
causing difficulty in generating three-helix shapes during gel formation. Moreover, the peak of
amide I band of all gelatin membranes switched to smaller wavenumber (1634 to 1620 cm-1) as
the microwave power boosted where it allowed the hydrophobic groups in gelatin to be exposed
securely and improved its amphiphilicity. Notwithstanding, microwave drying failed to create
porous surfaces on the gelatin membranes where the surfaces of the membranes were rough after
drying.

Page | 25
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