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ro/
Journal of
Journal of Agroalimentary Processes and Agroalimentary Processes and
Technologies 2023, 29 (3), 191-202 Technologies

The influence of heat treatment conditions on the water vapor

barrier properties of polyvinyl alcohol-based films
Iulia Benko*1, Anca Mihaly Cozmuta1, Camelia Nicula1, Leonard Mihaly
Cozmuta1, Goran Drazic2 and Anca Peter1
1Technical University of Cluj Napoca, Faculty of Sciences, Victoriei 76, 430072 Baia Mare, Romania
2National Institute of Chemistry, Hajdrihova 19 POBox 660 SI-1001 Ljubljana, Slovenia
____________________________________________________________________________________
Abstract
The purpose is to develop polyvinyl alcohol (PVA)-based formulations with water vapor permeability
(WVP) comparable to polyethylene (PE). Seventeen samples were created by modifying PVA with
beeswax, citric acid and surfactant, varying heat treatment conditions. Characterization involved optical
and electron microscopy, elemental analysis, WVP and biodegradability assessments. Sample B9, with
3% citric acid, heat-treated at 125°C for 30 minutes, exhibited the lowest WVP (0.673 x 10 -10 g/s m Pa).
B9 was tested as a bread packaging material, displaying similar crust hardness behavior to PE after 1
day and 26.4% higher hardness than PVA after 4 days. B9 matched PE in dry matter preservation after
2 days. Thus, the modification with citric acid, bee wax and by heat treatment, led to an 88% reduction
in PVA's water vapor permeability compared to unmodified PVA. The findings suggest B9's potential
as an effective alternative packaging material with improved barrier properties and bread preservation
capabilities.
Keywords: polyvinyl alcohol-based films; water vapor barrier properties; citric acid; thermal treatment;
beeswax;
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1.Introduction the chemical bonds of the polymer into smaller
fragments. Microorganisms recognize these
Food packaging plays a crucial role in protecting
fragments and assimilate them, using them as a food
and maintaining the quality of food products. In this
source to support their growth and metabolism.
context, polyvinyl alcohol (PVA) film has gained
Finally, the mineralization process converts polymer
increased attention due to its barrier properties
fragments into end products, such as carbon dioxide
against water vapor and its ability to prevent
and water, which integrate into the surrounding
undesired moisture exchanges between packaged
environment, contributing to reducing
products and the surrounding environment.
environmental impact. Biodegradation is an
However, in the production process of packaging
important aspect in the development of ecological
materials, the heat treatment represents a critical
materials, such as biodegradable packaging, to
stage [1].
reduce plastic waste and promote sustainability in
Biodegradation is an essential process in the life the industry [2].
cycle of polymeric materials, involving their
Polyvinyl alcohol (PVA) is a synthetic, colorless
transformation into simpler components such as
polymer soluble in water, primarily used in textile
carbon dioxide, water, methane, or biomass under
and paper treatment. It is represented as a unique
the influence of microbial activity or other
polymer because it consists of chemical compounds
biological factors. This decomposition occurs in
and large molecules with multiple units, as it is not
several well-defined stages, starting with
built through polymerization reactions but from
biodeterioration, where microorganisms colonize
precursor molecules with a single unit known as
the material's surface and secrete enzymes to
monomers [1].
degrade the polymer's structure. Next is the
depolymerization stage, where enzymes break down
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* Corresponding author: Iulia Benko - iulia_benko@yahoo.com
 Iulia Benko et.al./ Journal of Agroalimentary Processes and Technologies 2023, 29(3)

PVA is a common polymer that exhibits important for 105 days of post-harvest, followed by a
characteristics such as water solubility, ease of use simulated commercialization period of 7 days, all
and film-forming properties. It is used for preparing covered fruits successfully recorded a reduction in
blends and composites with various renewable weight loss, decomposition and softening rate.
natural polymers, including chitosan, nanocellulose Therefore, it can be considered that chitosan-
or starch. This polymer presents significant beeswax with pollen grains represents a safe and
potential as a biodegradable matrix in effective option for fruit preservation [4].
environmentally friendly composites. It can be a
The purpose of this study is to investigate the
sustainable alternative to composites made from
influence of the heat treatment conditions on the
non-biodegradable or non-recyclable fillers like
water vapor barrier properties of polyvinyl alcohol-
carbon fibers [3].
based films modified with beeswax, designed for
According to the literature data, smart films have food packaging. This aspect is becoming
been found suitable for food packaging, provided increasingly important in the food industry as there
they possess good physical and mechanical is a constant search for ways to enhance the
properties. In this context, a chitosan and beeswax- durability and safety of food products on the
based film was used to preserve "Le Conte" pears market.
after harvesting. These films were characterized
2. Materials and Methods
using methods such as X-ray diffraction, Fourier-
Transformed Infrared Spectroscopy and Scanning 2.1.Preparation of Polyvinyl Alcohol-Based
Electron Microscopy. All films demonstrated good Formulations
abilities, with mechanical resistance (elongation) A total of 17 formulations of polyvinyl alcohol
values ranging from 86.7 to 96.3 cm-1. The film (PVA) modified films were prepared. The mass
treated with pollen grains showed a better water ratio of PVA (Merck, Germany) to beeswax (from a
contact angle compared to the chitosan film. The local beekeeping store in Baia Mare) to glycerin
chitosan-beeswax film with pollen grains recorded a (Chemical Company, Romania) to vegetable
WVP value twice as low as the chitosan film and surfactant (Cocamidopropyl betaine, Mayam,
exhibited a tendency to increase the film rigidity. Romania) was 10:16:8:1. Table 1 presents the
The percentage of elongation at break decreased process for obtaining each sample.
from 35.81 to 14.09 cm-1. During the cold storage

Table 1. Procedure for obtaining the modified PVA-based formulations

Sample Code Description of the sample
B0 It was obtained through heat treatment for 10 minutes when the oven reached a temperature of 125°C
B1 It was obtained through heat treatment; the sample was introduced into the oven when it was still cold
(20℃) and was kept for 10 minutes from the moment the temperature reached 125℃.
B2 It was obtained through heat treatment; the sample was introduced into the oven when it was still cold
(20℃) and was kept for 20 minutes from the moment the temperature reached 125℃.
B3 It was obtained through heat treatment; the sample was introduced into the oven when it was still cold
(20℃) and was kept for 30 minutes from the moment the temperature reached 125℃.
B4 The film was kept hot for 20 minutes from the moment the oven reached 125 ℃.
B5 The film was kept hot for 30 minutes from the moment the oven reached 125 ℃.
B8 The film was kept warm for 10 minutes from the moment the oven reached 125 ℃, and citric acid was
added at 2.83%.
B9 The film was kept warm for 30 minutes from the moment the oven reached 125 ℃, and citric acid was
added at 2.83%.
B10 The film was kept warm for 10 minutes from the moment the oven reached 125℃, and the surfactant
solution, that is, the tenside, has a concentration of 15g/L.
B11 The film was kept warm for 30 minutes from the moment the oven reached 125℃
B12 The film was kept warm for 50 minutes from the moment the oven reached 125℃, and the surfactant
solution is 15g/L.
B13 The film was kept warm for 70 minutes from the moment the oven reached 125℃, and the surfactant
solution is 15g/L.
B14 The film was kept warm for 10 minutes from the moment the oven reached 125℃, and 2.83% citric acid
was added, with a surfactant solution concentration of 15g/L
B15 The film was kept warm for 30 minutes from the moment the oven reached 125℃, and 2.83% citric acid
was added, with a surfactant solution concentration of 15g/L
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B16 The film was kept warm for 50 minutes from the moment the oven reached 125℃, and 2.83% citric acid
was added, with a surfactant solution concentration of 15g/L
B17 The film was kept warm for 70 minutes from the moment the oven reached 125℃, and 2.83% citric acid
was added, with a surfactant solution concentration of 15g/L
Unmodified PVA The film contains only PVA dissolved in the surfactant solution and was kept warm for 10 minutes when
the oven reached 125℃

2.2. Characterization of Polyvinyl Alcohol-Based

2.2.3. Biodegradability
Formulations
The biodegradability of the films was evaluated by
2.2.1 Morphological Characterization via Electron
introducing a known mass piece of film into
Microscopy and Elemental Analysis
approximately 500 g of garden soil, constantly
The morphology of the samples was determined moistened and periodically monitoring the mass
using scanning electron microscopy (SEM) with a decrease of the film. Every 15 days, the film piece
Jeol ARM 200 CF SEM Cs system. The samples was extracted from the soil, washed with distilled
were positioned on a Ni-modified carbon grid. For water, dried at 60 0C and weighed. Biodegradability
elemental analysis (EDXS), an energy-dispersive X- (BIO) was expressed as a percentage.
ray spectrometer (SDD) was employed, specifically
mi  m f
the Jeol Centurion model. The working potential BIO(%)  100
was set to 80 kV. mi (Eq. 3)
2.2.2 Mass Increase and Water Vapor Permeability
Where: - - initial mass of the film (g); - final
A piece of material (9 cm2) was fixed to a plastic mass of the piece (g)
flask with section 1cm/1cm containing anhydrous
silica gel. The assembly was weighed, then 2.2.4. Evaluating the Most Efficient PVA-Based
introduced into a container with water vapor. The Formula as Bread Packaging Material
assembly was weighed at intervals until equilibrium The bread was wrapped in the most efficient
was reached. modified PVA formula (which exhibited the best
The mass increase (MI) was calculated using the barrier properties against water vapor) and stored at
formula: 22℃. Unpackaged bread, bread packaged in PE and
bread packaged in unmodified PVA were
(Eq. 1) considered as reference samples and were also
analyzed. The characterization of the bread during
Where: - -- initial mass of the flask (g); - storage consisted in performing the organoleptic
final mass of the flask (g) analysis, determination of crust hardness and dry
matter content.
Water vapor permeability (WVP) was calculated
using the formula: The hardness of the bread crust was monitored
using a Wagner penetrometer and was expressed in
w x
WVP ( g / s  m  Pa)  kg.
t  A  P (Eq. 2) The dry matter content of the bread was determined
Where: w - mass increase due to the absorption of by the gravimetric method. In a weighing flask with
water vapor by silica gel until equilibrium is a known mass (m0), 1 g of finely crushed bread is
reached (g); x - thickness of the material (m); A - added and the entire assembly was weighed (m1). It
contact surface area (m²); t - analysis time required was dried in an oven at 102-105°C until the constant
to reach equilibrium (s); ΔP - difference between mass was reached (m2). The dry matter content
the partial pressure of the atmosphere with silica gel (DM) was determined by the formula:
and distilled water (2652 Pa at 40°C).
(Eq. 4)
where: m0 – mass of the weighing flask (g), m1 –
mass of the flask with bread before drying (g); m2 –
mass of the flask with bread after drying (g) [5].
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3. Results and Discussions The SEM images of the samples are presented in
Figure 2. The results showed that the surface of the
3.1. Morphology of PVA-Based Formulas
modified PVA formulas is non-homogeneous
The macroscopic images of formulas B0, B9 and (Figure 2a and b). This indicates that the dispersion
unmodified PVA are presented In Figure 1. It can be of beeswax in the material is unbalanced, due to the
observed that PVA is transparent, colorless, flexible inadequate mixing and insufficient stirring time. In
and has a glossy texture (Figure 1c). Formulas B0 contrast, the surface of the PVA sample is more
and B9 have a matte texture, they are flexible, homogeneous than that of the modified formulas
slightly elastic and display a yellowish-white color, (Figure 2c). However, holes also appeared in the
attributed to the beeswax (Figure 1a and b). The PVA film, due to the excessively thin layer of
other PVA-based formulas exhibit organoleptic material, which, after drying, created spaces. On the
characteristics like B0 and B9. According to the other hand, the PE sample has an extremely high
literature data, during macroscopic analysis, degree of surface homogeneity compared to the
spherical granules were observed on the surface of other samples (Figure 2d). Wang et al. (2013) have
the PVA polymer, with diameters ranging from 0.5 observed that the morphology of the PVA
to 1 μm, and the speed was reduced, leading to composite membrane was remarkably uniform. This
agglomeration [6]. is because the weak force of the PVA chains is not
sufficient to induce clustering at the molecular chain
level. As a result, the PVA composite membrane
should exhibit excellent uniformity [6].

(a)

(a)

(b)

(c)
Figure 1. Macroscopic image of formula B0 a), B9 b) (b)
and unmodified PVA c)
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(c) (a)

(b)
(d)
Figure 2. SEM images of sample B0 a), B9 b),
unmodified PVA c), and polyethylene (PE) d)

The results of the elemental analysis EDXS are

presented in Figure 3. In formula B0 (Figure 3a), C
and O are present, along with lesser amounts of Na
and Cl, originating from the vegetable surfactant. In
formula B9 (Figure 3b), C, O, Na, Mg, Si, Cl, and K
are found, also coming from the vegetable
surfactant, as well as from beeswax. Insignificant
amounts of Na, S, and Cl can be observed in the (c)
PVA sample (Figure 3c). C and tiny amounts of O
were found in the polyethylene sample (Figure 3d).
Abdel-Hady et al. (2019) have observed that the
modification of the PVA structure after adding TiO2
nanoparticles occurred and was established by
EDXS elemental analysis. In addition to the gold
sputtered peak (2.1 keV), two peaks associated with
O and C elements (0.2 keV) and O elements (0.5
keV) were observed, indicating characteristic
components of PVA. New peaks associated with Ti
elements (0.4 keV and 4.5 keV) and O elements (0.5 (d)
keV) were observed, indicating the presence of Figure 3. Elemental analysis by EDXS of sample B0 a),
characteristic components of TiO2 [7]. B9 b), Unmodified PVA c) and polyethylene (PE) d)

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3.2. Mass Increase and Water Vapor increase of B2 is lower than that of B4 by 2%,
Permeability indicating that introducing the film into the oven
already heated to 125°C is not optimal for reducing
Figure 4 illustrates the mass increase of the tested
barrier properties. Sample B5 shows a mass increase
PVA-based formulas compared to PVA and PE. The
of 12.7% at 13 days, lower than sample B4, with a
mass increase is significant for the PVA sample
difference of 0.8%. Sample B4 was kept for 20
(12%) and less pronounced for B0 (11.4%) and PE
minutes in the oven already heated to 125°C, while
(6.3%) after 55 days of analysis. The mass increase
sample B5 was kept for 30 minutes. Between these
for formulas B1, B2, and B3 is similar (between
two samples (B4 and B5), sample B5 performs
11.5% and 11.9% after 55 days), with statistically
better, suggesting that increasing the thermal
insignificant differences. Therefore, increasing the
treatment time favors barrier properties when the
thermal treatment time from 10 to 30 minutes did
oven is already warm at the introduction of the
not result in changes in the water vapor barrier
samples.
properties of the PVA samples with beeswax and
without citric acid, which were introduced into the By analyzing Figure 4c, it can be observed that
cold oven during the thermal treatment. sample B8 exhibits a pronounced mass increase
until day 15, after which the increase is reduced
In terms of mass increase, the PE sample is the most
(12.2% after 55 days of analysis), almost 1% higher
efficient, as it shows the lowest mass increase
than B0. The mass increase of B9 is 15.2% after 126
compared to the other four samples (Figure 4a).
days, indicating that sample B9 was the least
Comparing samples B2 and B4 (Figures 4a and 4b), permeable to water vapor.
it can be observed that after 55 days, the mass

(a)

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(b)

(c)

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(d)

(e)
Figure 4. Mass increase provided by samples B0-B3 a), B4 and B5 b), B8 and B9 c), B10-B13 d), and B14-B17 d)

In sample B10, a more concentrated surfactant enhance the water vapor barrier properties of the
solution (15g/L) was added compared to samples PVA-based formula.
B0-B9 (Figure 4d). Sample B10 shows a more
Samples B10-B13 differ in the duration of heat
pronounced mass increase (14.6% after 11 days)
treatment. By analyzing Figure 4d, it is noted that
compared to sample B1, which was prepared under
the lowest mass increase values were recorded for
the same conditions, but with a surfactant
samples B10 and B13, which were heat-treated for
concentration of 10g/L. Thus, it is observed that the
10 and 70 minutes, respectively.
increase of the surfactant concentration does not
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Therefore, the most advantageous is the heat water vapor barrier properties of films based on
treatment procedure for 10 minutes. PVA modified with beeswax. Through modification
(adding citric acid, heat treatment conditions), the
Samples B14-B17 contain citric acid at a
permeability to water vapor of PVA was reduced by
concentration of 2.83% and a surfactant with a
88% compared to unmodified PVA, while the
concentration of 15g/L, differing in heat treatment
barrier properties are 3 times lower than that of PE
time of 10, 30, 50, and 70 minutes, respectively. It
(considered nearly impermeable).
is observed that sample B14 has a mass increase of
15.2% after 55 days, and sample B15 has a mass The literature data showed that in the case of starch-
increase of 15.4% after 78 days. Sample B15 based films, the permeability to water vapor can be
reached equilibrium after the longest period, influenced by mass transfer mechanisms and by
indicating the lowest permeability for water vapor. interactions between the used solutions and the
polymers. Due to the irreversibility of the
Among all the tested samples, formulas B9 and B17
thermodynamic process, the difference in water
reached equilibrium after 126 and 120 days of
chemical potential is the driving force for water
storage in a water vapor environment, respectively
transfer through a film. When the process occurs at
(Table 2). Additionally, the permeability to water
constant temperature and pressure, the difference in
vapor was the lowest for these two formulas. This
water vapor concentration between the two faces of
demonstrates that the presence of citric acid at a
the film is proportional to the difference in chemical
mass concentration of 2.83% and the increase in
potential of water [8].
heat treatment time have an enhancing effect on the

Table 2. Time required to reach vapor equilibrium and water vapor permeability of PVA-based formulas
Formula cod Time required to reach vapor WVP(g/s m Pa) x 1010
equilibrium (days)
B0 52 5.19
B1 26 1.82
B2 26 1.77
B3 73 0.655
B4 35 1.47
B5 35 1.36
B8 84 0.744
B9 126 0.673
B10 55 1.44
B11 55 1.61
B12 55 1.18
B13 55 1.13
B14 55 1.58
B15 78 1.13
B16 55 1.42
B17 120 0.740
PVA 38 5.76
PE 184 0.218

3.3. Biodegradability
This is because unmodified PVA is a biodegradable
Biodegradability refers to the material's ability to synthetic polymer in environments with
naturally decompose in the surrounding microorganisms capable of breaking it down, such
environment under the influence of microorganisms as certain bacteria and enzymes, undergoing
and environmental factors such as heat, moisture, degradative processes. In the same conditions, PE
and light [9]. showed a biodegradability of 0.1% in 30 days of
analysis.
According to Figure 5, the highest biodegradability
was observed for the PVA-based formulas (~55%), According to studies on anaerobic biodegradability
with PVA unmodified exhibiting the highest of polyvinyl alcohol, it was found that the evolution
biodegradability among them. rate of CO2 from anaerobic degradation of PVA
decreased as the molecular weight increased.
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Figure 5. Biodegradability of PVA-based formulas

These results suggested that PVA is biodegraded by

anaerobic microbes, but a longer time is required for
the biodegradation of high-molecular-weight PVA
[9].
3.4. Evaluating the Most Efficient PVA-Based
Formula as Bread Packaging Material
The most efficient formula was B9, with a WVP
value of 0.673 x 10-11 (g/s m Pa), 101 times higher
than that of PE. Thus, this formula was used to store
bread and to determine the period during which it
maintains optimal organoleptic and physical-
chemical properties for consumption. The image of
bread samples packaged in the tested materials at
the beginning of the experiment is presented in (b)
Figure 6.

(a) (c)
Figure 6. Image of bread samples packaged in formula
B9 a), PE b), and unmodified PVA c)

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During the 4-day storage period, there were no with the B9 crust hardness being 26.4% higher than
changes in the color and smell of the bread samples the PVA-packaged bread after 4 days of storage.
stored in the packaging, only changes in
Crust hardness is strongly influenced by the WVP
consistency. The bread in PVA hardened after just 4
of the packaging film and can vary depending on
hours of packaging, while the one in B9 became
several factors, including the recipe used, the type
hard after the second day. In contrast, the bread in
of flour, the baking process, and the bread storage
PE retained its softness even after the fourth day.
time. The outer layer of the bread, known as the
The highest crust hardness (Figure 7) was measured crust, results from the formation of a dry and crispy
after 4 days for the bread in PVA packaging (3 kg surface during the baking process.
force), followed by the B9 formula (2 kg force),
Regarding the variation in the dry matter of bread
while the lowest was observed for the sample stored
(Figure 8), after 4 days of storage, the bread stored
in PE (0.1 kg force).
in PVA underwent the most intense dehydration
The crust hardness after one day in the B9 sample process (DM = 89%), followed by that in B9 (DM =
was identical to that of the bread in PE. After four 86%), while the least dehydrated was the bread in
days, the crust hardness of the bread in the B9 PE (DM = 74%).
sample was lower than that of the unmodified PVA,

Figure 7. Crust hardness of bread packaged in the tested materials

Figure 8. Variation in bread dry matter content during storage in the tested packaging

According to a study, the moisture content of bread minutes after baking) or packaged after being
was determined over the course of a year of storage sprayed with 0.2% calcium propionate 10 minutes
at 25℃. Two packaging methods for the bread after baking did not develop any mold over the
crumb resulted in a slower firming rate and lower storage period. However, the separation of the
equilibrium firmness. To prevent mold growth on crumb from the crust of fully baked bread 1 hour
bread, two packaging methods were tested. Bread after baking maintained the crumb moisture during
packaged in a sterilized bag while still hot (3 storage but did not prevent firming; nevertheless,
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the equilibrium firmness was much lower. Both Acknowledgements. The analyses were conducted at the
crumb firmness and crumb moisture played Research Center for Quality Control and Environmental
important roles in crumb firming, but other factors and Product Safety, within the Department of Chemistry
also contributed. Both crumb firmness and crumb and Biology, Technical University of Cluj-Napoca, and
at the Electron Microscopy Laboratory at the National
moisture reached equilibria after 30 days of storage
Institute of Chemistry, Ljubljana, Slovenia.
[10].
Conflict of Interest. Author has declared that no
4. Conclusions competing interests exist.
The analyses have shown that among the 17 Compliance with Ethics Requirements. Authors
formulas based on PVA modified with beeswax, declare that they respect the journal’s ethics
where citric acid content, surfactant concentration, requirements. Authors declare that they have no conflict
and thermal treatment time were varied, the least of interest and all procedures involving human / or
permeable to water vapor were the B3, B8, B9, B17 animal subjects (if exist) respect the specific regulation
samples. Therefore, by adding citric acid (2.83%) and standards.
and increasing the thermal treatment time (up to 70 References
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