Environmental Chemistry and Ecotoxicology 2 (2020) 107–114

Contents lists available at ScienceDirect

Environmental Chemistry and Ecotoxicology

journal homepage: www.keaipublishing.com/en/journals/environmental-chemistry-
and-ecotoxicology/

Fabrication of improved cellulose acetate-based biodegradable films for food

packaging applications
A. Rajeswari, E. Jackcina Stobel Christy, E. Swathi, Anitha Pius
⁎
Department of Chemistry, The Gandhigram Rural Institute – Deemed to be University Gandhigram, Dindigul 624 302, Tamil Nadu, India

A R T I C L E I N F O A B S T R A C T

Article history: Biodegradable polymers based food packaging films can replace the non-biodegradable synthetic polymers in the
Received 14 May 2020 way of low cost and also which creates a positive outcome on both environmentally and economically. For the
Received in revised form 25 June 2020 first time naturally occurring alginate and carrageenan which is extracted from seaweeds and cellulose acetate
Accepted 12 July 2020
(CA) blended novel food packaging films were fabricated by solvent casting technique. All the films such as
Available online 18 July 2020
bare CA (F1), polysaccharides incorporated films (F2 and F3) have been characterized using scanning electron mi-
Keywords:
croscope (SEM), thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy (FTIR). Addition
Food packaging of polysaccharides such as sodium alginate (SA) and carrageenan (CG) greatly increased the tensile strength
Biodegradable and thermal stability of the prepared films. The surface morphologies indicated better homogenization of biopoly-
Seaweeds mers like F2 and F3. Antibacterial activity of the film was studied. The prepared polysaccharide films inhibit the
Casting technique growth of certain type of microorganisms. Biodegradability tests were also carried out which indicated that the
Film prepared films were biodegradable in nature.

1. Introduction
For the past 20 years, uses of plastics in daily life have been enormously
increased [1–3]. Plastics in food packaging have been widely used and also
in some other industries for packaging applications because they are not
often damaged in everyday use. But increasing ecological concern due to
adverse environmental impact of plastics is contributing to the growth of
the biodegradable materials. Food packaging materials plays a vital role
in food preserving throughout the distribution chain. It has to protect
food from contamination and mechanical damage during marketing. In re-
cent times to develop materials having antimicrobial properties which
could an improve shelf-life, perishable food and its safety.
Most promising method for active packaging systems is antimicrobial
packing [4–6]. Labuza et al. [7] described an innovative active packaging
to enhance the shelf life of food processed and also to meet consumer satis-
faction and demands by producing quality products with freshness and
safety. An utilization of such packing enhanced food safety from the growth
of spoilage microorganisms and pathogens. Microbial pathogens can con-
taminate human food and water which cause ill effects after their toxins
are consumed [8–10].
To enhance the shelf life of food products, various research groups
[11–13] have been focusing on natural compounds like biopolymers,
plant extracts, essential oils etc., as an alternative for synthetic compounds.
It is well known cellulose as a natural biopolymer and it is used as a substi-
tute for traditional plastics found to have an attracting interest. Cellulose
derivates posses better applicability than cellulose. Among the cellulosic
derivates, CA has gained greater interest because as it has a properties of
biodegradability, biodegradable polymer, has excellent optical property,
high toughness and can produce films either by melting or solvent-casting
techniques [14,15]. CA showed low moisture barrier properties and should
be either modified for film production [16]. Moreover, as biopolymer, CA
exhibits hydrophilicity, which would limit its adjustment to food packaging
application [17].
Seaweed has received much interest and attention in applications re-
lated to energy, food, tissue engineering and biosensors [18]. Similar to
other polysaccharide sources, seaweed is also a green, abundantly available
and inexpensive source of polysaccharide harvested from the sea [19]. Algi-
nate, carrageenan and agar are common products which are derived from
seaweeds that exhibit interesting film forming properties [20–22]. Novelty
of this study is fabrication of biodegradable CA based food packaging films

⁎ Corresponding author.
E-mail address: dranithapius@gmail.com. (A. Pius).

http://dx.doi.org/10.1016/j.enceco.2020.07.003
2590-1826/© 2020 The Author. Production and hosting by Elsevier B.V. on behalf of KeAi Communications Co., Ltd. This is an open access article under the CC BY license
(http://creativecommons.org/licenses/by/4.0/).
A. Rajeswari et al. Environmental Chemistry and Ecotoxicology 2 (2020) 107–114

Fig. 1. Schematic set up of fabrication process.

Fig. 2. SEM images of (A) SA (B) CG (C) F1 (D) F2 and (E) F3.

by adding naturally occurring sodium alginate (SA) and carageenan (CG)

extracted from seaweeds which may greatly increase the surface morphol- 2. Experimental
ogy, thermal, tensile properties etc. Also both bare CA film (F1) and poly-
saccharides like SA and CG mixed films such as CA/SA (F2) and CA/SA 2.1. Materials
(F3) were characterized to evaluate efficiency for the application of food
packaging. The area of Rameshwaram is 51.8 sq. Km and a small island and major
pilgrim centre in the Gulf of Mannar, Tamilnadu, India. It is connected to

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Fig. 3. FTIR spectrum of pure SA, CG, F1, F2 and F3.
the mainland by Pamban Bridge. Olaikuda beach is one kilometre away
from the principal shrine of Rameshwaram. It is surrounded by seaweeds
and coral reefs. Brown seaweeds (Sargassum wightii-S. wightii) and red sea-
weeds (Gracilaria Corticata-G. Corticata) were obtained from the above
coastal area. Chemicals such as CA, acetone, potassium hydroxide, formal-
dehyde, sodium carbonate, hydrochloric acid and sodium hydroxide were
purchased from Sigma Aldrich.
2.2. Extraction of sodium alginate from brown seaweed
The collected brown seaweeds (S. wightii) were washed thoroughly with
distilled water and dried at room temperature. The dried seaweeds were
ground well and sieved to get uniform fine powder. The powdered seaweed
sample was weighed and treated with formaldehyde for about 24 h. Then it
was filtered and obtained residue was washed 2–3 times with distilled
water. Further it was treated with HCl solution and it was kept for 24 h at
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Environmental Chemistry and Ecotoxicology 2 (2020) 107–114
room temperature. Then it was filtered and washed with distilled water.
The obtained residue was treated with sodium carbonate for about 24 h.
The extract obtained was filtered and then treated with 5% v/v HCl to
form precipitated alginate which was separated by centrifugation method.
The precipitate was washed with distilled water, dried, powdered weighted
and stored for further use [23].
2.3. Extraction of carrageenan from red seaweed
The collected red seaweeds (G. corticata) were washed thoroughly with
distilled water, dried at room temperature and grounded well to obtain uni-
form fine powder. The powdered seaweed was soaked with distilled water
to remove the dissolved impurities then it was added to the potassium hy-
droxide (KOH) which was used as a solvent extractor when the temperature
reached 85 °C maintained in water bath. To maintain constant ratio of the
seaweed weight to solvent volume was obtained by adding hot water.
A. Rajeswari et al. Environmental Chemistry and Ecotoxicology 2 (2020) 107–114

Fig. 4. a) TGA and b) DTG spectra of F1, F2 and F3 films.

The extraction process was continued further 45 min. Then the extract was at atmospheric temperature which was filtered and to remove air bubbles
cooled and filtered to obtain the residue which was further treated with eth- the above solution allowed to stand for some time. Homogeneous CA solu-
anol immediately to gain polysaccharide precipitate. The product carra- tion was transparent and it was uniformly casted using casting instrument.
geenan was dried in oven and use for further studies [24]. The resulting film was immersed in coagulant bath and then dried [25].

2.4. Preparation of CA film 2.5. Preparation of CA/polysaccharide film

CA was dissolved in acetone which is a casting solution. To form a ho- The extracted polysaccharides such as SA and CG were separately dis-
mogeneous solution the above solution was blended using magnetic stirrer solved in water. To this above polysaccharide solutions, CA solution was

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Table 1 properties were measured with a 50 kN load cell at ambient conditions.

TGA and DTG values of F1, F2 and F3 films. 12.5 mm/min is the cross-head speed and samples were tested 3 times,
Film Thermal Tonset Tendset Weight DTA the average values were plotted.
degradation (°C) (°C) loss characteristics
step (%) 2.6.3. Biodegradation tests
F1 I 30 263 68.5 Exothermic As described in the literature the biodegradation tests were carried out
II 264 348 9.7 [26]. The regular shaped films were making free from moisture and taken
F2 I 30 292 72.5 Exothermic
weight (W0). Within a compact atmosphere the weighed films (F1, F2 and
II 293 397 12.4
F3 I 30 278 69.2 Exothermic F3) were deposited into a soil for 60 days. The above setup was carried
II 279 375 11.3 out at room temperature by adding water regularly. Changes occurred in
the above setup were follow-up gravimetrically. Deposited films were
taken out and cleaned. Further, the cleaned films were dried and weighed
added separately and stirred to get a homogenous solution. Coacervate CA (Wt) to average the weight loss (% WL) [27]. The above procedures were ex-
(F1), CA/SA (F2) and CA/CG (F3) solutions were uniformly casted using ecuted in three times and to found % WL values using Eq. (1).
casting instrument. The obtained films were dipped in coagulant bath and  
then dried [25]. Schematic representation of preparation method is W0 −Wt
%WL ¼  100 ð1Þ
shown in Fig. 1. W0

2.6. Characterization details and analysis

The morphologies of pure SA,CG, bare CA (F1), CA/SA (F2) and CA/CG
(F3) films were analysed by SEM (Model: TESCAN Vega3). Characteristic
stretching frequencies of pure SA,CG, F1, F2 and F3 films were compared
by using FTIR (JASCO FTIR-460 plus). Water contact angles of the prepared
films were estimated by goniometry (rame- hart instrument. Co, USA).
2.6.4. Antibacterial test
Agar diffusion method was employed for antimicrobial activity for the
prepared bare and polysaccharide films. The circular shaped polysaccha-
ride films were placed on agar plates. Plates were seeded with inoculums
containing indicator microorganisms which are incubated. The inhibitory
zone was calculated around the circular films in agar phase [28].

3. Results and discussion

2.6.1. Thermogravimetric analysis (TG-DTA)
Weight loss and DTA (derivate thermogravimetric analysis) were deter-
mined by SEIKO model TG/DTA 6200 for F1, F2 and F3 films from room
temperature (RT) to 600 °C temperature in N2 atmosphere. The weight
losses at different stages were recorded.
2.6.2. Mechanical stability test
Tensile strength as well as elongation-at-break for all films (bare F1, F2
and F3) was tested using Tinius Olsen 50ST instrument. In that, tensile
3.1. SEM analysis
SEM micrographs of A) SA, B) CG, C) bare F1, D) polysaccharide films
F2 and E) F3 are shown in Fig. 2.A to E
Fig. 2A and B were exhibit surface morphologies of SA and CG powder
which showed a distinct cube and aggregated spherical structures respec-
tively. The morphology of bare F1 film (Fig. 2.C) indicated porous and
cracked nature. While Fig. 2.D and E showed that the polysaccharides

Fig. 5. Contact angle of a) F1 b) F2 and c) F3.

Fig. 6. A) Tensile strength (TS) and B) Elongation at break (E) of a) F1 b) F2 and c) F3.

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Peaks of sodium alginate observed at 3416, 1024, 1626 and 1415 cm−1
were ascribed to –OH, C-O-C, asymmetric and symmetric stretching of car-
boxylate groups respectively [30]. Moreover, peaks around 1315, 1088,
898 and 1130 cm−1 correspond to CO and CC stretching. All these confirm
polysaccharide structure of SA as reported [31]. Pure carrageenan shows
several absorption peaks at 1377, 1068, 922 and 844 cm−1 indicated the
presence of sulphate ester, glycosidic linkage, 3,6- anhydro-d-galactose
and D-galactose-4-sulphate respectively. Similar results were registered in
literature [32,33].
Few significant changes were observed in F2 and F3 spectrum as com-
pared to the F1 spectrum. In addition, there was remarkable shifts noted
at 3480, 2957, 1738 cm−1 and 3497, 2955, 1730 cm−1 in F2 and F3 re-
spectively. While some characteristic peaks were introduced at 1636,
608 cm−1 and at 835, 794 cm−1 in F2 and F3 respectively. These shifts
and formation of new peaks may be due to the impregnation of SA and
CG onto CA film.

3.3. TGA analysis

TGA is considered as the most important method for studying the ther-
mal stability of polymers. Derivative thermogravimetric (DTG) curves and
Fig. 7. Degradation weight loss of the a) F1 b) F2 and c) F3 films.
TGA curves of neat F1 and polysaccharides impregnated F2 and F3 blend
films are depicted in Fig. 4.
were well embedded onto the CA films. Moreover SA and CG incorporated The first degradation step in bare F1 film was found to be in the range of
F2 and F3 films were relatively smooth, flat, showed an unbroken matrix in 30–263 °C with 68.5 wt% weight loss. In the case of polysaccharides such as
the absence of pores with better arrangement. Hence, the prepared SA and SA and CG incorporated films first degradation was noted between room
CG were mixed and dispersed onto the CA film. temperature to 292 (73.3 wt%) and 278 °C (69.2 wt%) respectively. This
could be the loss of absorbed water molecules present in the prepared
films which was supported by exothermic peak in DTA.
3.2. FTIR analysis However the second degradation of bare CA (F1) and modified CA (F2)
and (F3) films occurred in the range of 263–352 °C (9.7 wt%), 292–397 °C
FTIR analysis of SA, CG, F1, F2 and F3 was carried out and are depicted (12.5 wt%) and 278–375 °C (11.3 wt%) which corresponds to the decom-
in Fig. 3. The above F1 spectrum in Fig. 3, showed functional group peaks position of compounds present in the prepared films like cellulose acetate
for CO, OH, CH3 and ether C–O–C at 1736, 3443, 1374/1216 and and polysaccharide thereafter remained stable upto 600 °C. Similar obser-
1032 cm−1 respectively. This agrees with literature data [29]. vations had been reported in literature [34,35]. The thermogravimetric
characteristic values of bare (F1) and polysaccharide incorporated films
Table 2
(F2, F3) are shown in Table 1
Bacterial inhibitory zone for a) SA b) CG c) F1 d) F2 and e) F3 against E. coli, S. au-
reus and P. syringae. 3.4. Wettability test
Sample Inhibitory zone inhibitory zone inhibitory zone diameter
diameter for E. coli diameter for S. aureus for P. syringae (mm) Wettability test is a measurement of water molecules absorbed by the
(mm) (mm) sample. It is broadly defined the wettability character of the surface either
SA 13.8 15.2 14.6 the sample is hydrophilic or hydrophobic. The contact angle results of a) F1
CG 13.4 15.5 15.9 b) F2 and c) F3 are shown in Fig. 5.
F1 14.6 14.9 14.7 The contact angle degrees are 85o, 109o and 102° for bare F1, F2 and F3
F2 19.7 17.8 18.9 respectively. The contact angle was lower for F1 film than modified F2 and
F3 15.2 17.3 16.2
F3 films. Hence F1 film absorbed water which was allowed to spread in the

Fig. 8. Comparative test of tomatoes uncovered (right) and covered by F1 polysaccharide film (left).

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substrate and making it hydrophilic. But the polysaccharides such as SA and
CG incorporated films were hydrophobic in nature.
3.5. Mechanical properties
Tensile properties like tensile strength (TS) and elongation at break (E
%) of F1, F2 and F3 films, are exhibited in Fig. 6.
On comparing with F1 film, polysaccharides added F2 and F3 films ex-
hibited increase in TS but decrease in E %. This was due to the cooperative
physical cross-linking caused by hydrogen bond formation between SA and
CG with the CA chain and the brittleness of the films. Comparable results
were recorded in literature [2].
3.6. Biodegradation tests
The monitoring of degradation for the differently composed films such
as a) F1 b) F2 and c) F3 were proceeded for 60 days deposited in soil. The
atmospheric condition of the setup was kept constant. Fig. 7 explained
the percentage of weight loss in each film.
Percentage of weight loss was plotted against the degradation time.
From the results bare F1 film degrades after 58 days (65 wt%) at the
same time polysaccharides incorporated film like F2 and F3 were also de-
grades 55 and 50 wt%, respectively.
From this investigation, it is expected that the prepared films are biode-
gradable in soil within 3 months. The percentage weight loss of F2 and F3
film is less compared to bare F1 film. Hence the prepared films are biode-
gradable in nature.
3.7. Antibacterial activity
Inhibitory effect of a) SA b) CG c) F1 d) F2 and e) F3 against common
bacterial strains like Escherichia coli (E. coli), Staphylococcus aureus (S. au-
reus) and Pseudomonas syringae (P. syringae) micro organisms are shown
in Figs. S1·I(a)-(e), II(F)-(J) and III (K)-(O) respectively. According to the
disc as well as solution clear zone measurement the inhibitory effect was
calculated. (see Table 2).
If there is no clear zone surrounding the polysaccharide film, it is as-
sumed that there is no inhibitory zone. In terms of surrounding clear
zone, the polysaccharide films showed inhibitory effect against all tested
microorganisms. Incorporation of polysaccharide onto the CA film revealed
good antimicrobial effect. The inhibitory zones were markedly high for F2
and F3 films against E.coli, S. aureus and P. syringae compared bare F1 film.
From the observation, the addition of SA added polysaccharide film (F1) in-
creases the antibacterial activity.
3.8. Packaging of tomato
Tropically famous fruit is tomato which belongs to solanaceae family.
Compare to other fruits tomato ripens fast. Since the respiration is slow
when they are picked from the plant and also the shelf life of tomato is
short. The perfectly ripe tomato gets wrinkle and become rotten even
within two days. The food packaging polysaccharide film was used to
cover the seasonal fruit tomato. The appearance of tomato at the beginning
and 2nd, 3rd and 4th day was verified and shown in Fig. 8. The uncovered
tomatoes began to decay on the surface in 2 days, but the appearance of
covered tomatoes even on the 4th day was better than the uncovered
ones at the 2nd day. These results pointed out that the polysaccharide
film covering could delay the decay of tomatoes and showed a prolonged
shelf life.
4. Conclusions
In this investigation, cellulose acetate based biodegradable polysaccha-
ride films were prepared, characterized and applied for the food packaging
application. The prepared biodegradable polysaccharide film is desirable
considering environmental and economic aspects. Addition of
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Environmental Chemistry and Ecotoxicology 2 (2020) 107–114
polysaccharides such as sodium alginate and carrageenan greatly increased
the tensile strength and thermal stability of the films. The surface morphol-
ogies indicated better homogenization of biopolymers like F2 and F3. Anti-
bacterial activity of the film was studied. The prepared polysaccharide films
inhibit the growth of certain type of microorganisms like E. coli, S. aureus
and P. syringae. Biodegradation test carried out in laboratory scale and
found that the prepared films were biodegradable. It can be concluded
that the prepared polysaccharides incorporated F2 and F3 films can be effi-
ciently used to enhance shelf life of food materials.
Acknowledgements
The first author would like to thank the University Grants Commission,
Government of India for the financial support (ref. No. - F.No.25-1/2014-
15/ (BSR)/7-225/2008/(BSR), dt: 7th October 2015) and all authors thank
the authorities of Gandhigram Rural Institute –Deemed to be University for
the encouragement.
Appendix A. Supplementary data
Supplementary data to this article can be found online at https://doi.
org/10.1016/j.enceco.2020.07.003.
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