Materials and Design 61 (2014) 264–269

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Materials and Design

journal homepage: www.elsevier.com/locate/matdes

Effect of carrageenan on properties of biodegradable thermoplastic

cassava starch/low-density polyethylene composites reinforced
by cotton fibers
Jutarat Prachayawarakorn a,b,⇑, Wanida Pomdage a
a
Department of Chemistry, Faculty of Science, King Mongkut’s Institute of Technology Ladkrabang, Ladkrabang, Bangkok 10520, Thailand
b
Advanced Materials Research Unit, Faculty of Science, King Mongkut’s Institute of Technology Ladkrabang, Ladkrabang, Bangkok 10520, Thailand

a r t i c l e i n f o a b s t r a c t

Article history: Applications of biodegradable thermoplastic starch (TPS) have been restricted due to its poor mechanical
Received 25 November 2013 properties, limited processability and high water uptake. In order to improve properties and processabil-
Accepted 18 April 2014 ity, thermoplastic cassava starch (TPCS) was compounded with low-density polyethylene (LDPE). The
Available online 9 May 2014
TPCS/LDPE blend was, then, modified by a natural gelling agent, i.e. carrageenan and natural fibers, i.e.
cotton fibers. All composites were compounded and processed using an internal mixer and an injection
Keywords: molding machine, respectively. It was found that stress at maximum load and Young’s modulus of the
Biodegradable polymer
TPCS/LDPE composites significantly increased by the addition of the carrageenan and/or the cotton fibers.
Cellulose fiber
Gelling agent
The highest mechanical properties were obtained from the TPCS/LDPE composites modified by both the
Thermoplastic starch carrageenan and the cotton fibers. Percentage water absorption of all of the TPCS/LDPE composites was
found to be similar. All modified composites were also degraded easier than the non-modified one. Fur-
thermore, all the composites were analyzed using Fourier-transform infrared spectroscopy (FTIR), X-ray
diffraction (XRD) and Scanning electron microscopy (SEM).
Ó 2014 Elsevier Ltd. All rights reserved.

1. Introduction
The excessive amount of disposable plastics has led to serious
demands for biodegradable materials made from renewable
resources. The use of biopolymers appears as an excellent alterna-
tive for reducing current environmental problems. Starch is an
important biopolymer in foods that is an attractive choice for pack-
aging materials. Starch consists primarily of linear and branched
chains of glucose molecules, named as amylose and amylopectin,
respectively. Amylose is essentially a linear molecule with a few
branches; whereas, amylopectin is a highly branched molecule [1].
Native starch can be transformed into thermoplastic materials
through disruption of its granular structure and plasticization by
the presence of plasticizers with the application of thermo-
mechanical energy in a heating process. Many studies have focused
on the preparation of melted starch with the presence of glycerol;
the materials are called thermoplastic starch (TPS). Unfortunately,
there are some limitations to the commercialization of TPS-based
⇑ Corresponding author at: Department of Chemistry, Faculty of Science, King
Mongkut’s Institute of Technology Ladkrabang, Ladkrabang, Bangkok 10520,
Thailand.
E-mail address: ksjutara@kmitl.ac.th (J. Prachayawarakorn).
products. TPS materials, based solely on starch, are highly moisture
sensitive and have rather limited mechanical properties [2–10].
Furthermore, high viscosity and poor flow properties of starch-
based materials present difficulties during injection molding; typ-
ical process for producing synthetic thermoplastic polymers.
Therefore, the processing techniques for TPS are mainly limited
to compression molding and extrusion [2,3,5–10]. In order to pro-
cess TPS using injection molding technique, a polymer blend
between natural TPS and synthetic thermoplastic is still necessary.
New approach to solve the limitations of TPS materials is to use
a natural gelling agent. Carrageenan is one of natural gelling agents
widely used in food industries. Carrageenan is a polysaccharide-
based and water-soluble polymer with a linear chain of partially
sulphated galactans, which represent high potentiality as film-
forming materials. The sulphated polysaccharide is extracted from
the cell walls of various red seaweeds (Phodophyceae) [11]. Carra-
geenan has been blended with other natural polymers for produc-
ing edible and biodegradable films [12–14]. It was reported that,
without plasticizer, carrageenan improved tensile properties of
the sodium caseinate film, although water vapor permeability val-
ues increased [12]. However, at low content of plasticizer, carra-
geenan promoted stiffness and reduce water vapor permeability
of the sodium caseinate film [12]. Mechanical and rheological

http://dx.doi.org/10.1016/j.matdes.2014.04.051
0261-3069/Ó 2014 Elsevier Ltd. All rights reserved.
 J. Prachayawarakorn, W. Pomdage / Materials and Design 61 (2014) 264–269
properties of the acid hydrolyzed hydroxypropylated pea starch/
carrageenan cast film were also studied. It was found that the stiff-
ness of the film increased with the addition of carrageenan [14].
The use of natural cellulose fibers to reinforce TPS is another
interesting approach to resolve drawbacks of TPS materials. Many
researchers reported results on the addition of natural cellulose
fibers, such as Eucalyptus wood pulp [2], winceyette [3], bacterial
cellulose [4], cotton [5], kapok [10], etc. into TPS materials. Most of
these works focused on mechanical properties and showed that the
incorporation of these cellulose fibers into TPS caused the increase
of tensile strength and elastic modulus but the decrease of elonga-
tion of TPS [2–10]. In addition, a significant improvement in water
resistance was also obtained by the addition of cellulose fibers [2–
6,8–10]. Moreover, thermal stability of TPS was stated to improve
by higher thermal resistance of cellulose fibers [2–5,9–10].
Due to the high viscosity and poor flow properties of the ther-
moplastic cassava starch (TPCS) materials; therefore, the TPCS
was blended with low-density polyethylene (LDPE) in order to
assist for the flowability during injection molding process. Because
of the hydrophilic nature of the TPCS, it is not compatible with the
hydrophobic characteristics of the LDPE, resulting in poor mechan-
ical properties of the TPCS/LDPE blend. Since either carrageenan or
cellulose fibers has been shown to improve properties of starch
films; thus, the TPCS/LDPE composites modified by the carra-
geenan and/or the cotton fibers were, in this study, injection-
molded and tested. It was expected that properties of the TPCS/
LDPE composites would be improved by good phase compatibility
due to the chemical structural similarity of polysaccharides of the
starch and the carrageenan including cellulose structure of the cot-
ton fibers. The modified TPCS/LDPE composites were, after that,
characterized by Fourier-transform infrared spectroscopy (FT-IR),
X-ray diffraction (XRD) and Scanning electron microscopy (SEM)
techniques. Moreover, physical and mechanical properties of the
composites were tested.
2. Experimental details
2.1. Materials
Cassava starch (11.5–13.0% moisture) was obtained from Thai-
tam (Chonburi, Thailand), containing 20 ± 1 wt% amylose and
75 ± 2 wt% amylopectin. Glycerol (plasticizer) was purchased from
Lab System Co. Ltd. (Thailand). Injection grade of LDPE (LD1603J)
with melt flow index (MFI) of 28 g/10 min (tested at 21.6 N and
190 °C) was obtained from Thai Polyethylene, Co., Ltd (Bangkok,
Thailand). Maleic anhydride-grafted-polyethylene (MAPE,
MB100D) with the MFI of 2.0 g/10 min was purchased from Chem-
ical Innovation, Co. Ltd. (Bangkok, Thailand). j-carrageenan (Food
grade) was obtained from Ruam Chemie 1986, Co. Ltd. (Bangkok,
Thailand). Cotton fibers was obtained locally and used as-received.
The L/D ratio of the cotton fibers was approximately 150:1.
2.2. Sample preparation
Cassava starch was firstly pre-mixed with glycerol in polyethyl-
ene bags. The weight ratio of the cassava starch and glycerol was
maintained at 70:30. Blending of the TPCS with the LDPE and MAPE
compatibilizer was then carried out using an internal mixer (Lab-
Tech Engineering, Thailand) at the temperature of 140 °C at the
rotor speed of 40 rpm for 5 min. After that, the TPCS/LDPE blend
was injected by an injection molding machine (Hitech Weltec,
TTI-220/80, Hong Kong) using the injection pressure and injection
flow speed of 30 bar and 50 rpm, respectively. The injection tem-
perature was in the ranged of 150–170 °C. The weight ratio of
the TPCS and LDPE was kept at 1:1 and The MAPE content was
265
maintained at 5% by weight of the LDPE. The property modification
of the TPCS/LDPE composite was carried out by the addition of dif-
ferent contents of carrageenan, i.e. 0%, 2%, 4%, 6%, 8% and 10% by
weight of the TPCS. By the use of the cotton fibers, it was fixed at
5% by the total weight of the TPCS/LDPE composites. It should be
noted that the abbreviations of CG and CF referred to 10% weight
of the carrageenan by the TPCS weight and 5% weight of the cotton
fibers by the TPCS weight, respectively.
2.3. IR spectroscopic study
FTIR spectrum of a sample was recorded on a Spectrum 2000 GX
spectrometer (Perkin Elmer, USA) using KBr disk technique with a
resolution of 4 cm1 in a spectral range of 4000–600 cm1 using 16
scans per sample.
2.4. X-ray diffraction
Wide angle X-ray diffraction measurements were carried out
using a D8 Advance X-ray diffractometer (Bruker, Madison, USA)
using Cu Ka radiation (wavelength of 0.1542 nm) operating at
40 kV and 35 mA. The scattering angle (2h) covered the range from
3° to 60° (h is the Bragg angle) with a step size of 0.02° and a sam-
pling interval of 10 s. Percentage crystallinity of a sample was
determined by the following equation
Crystallinity ð%Þ ¼ Ac =ðAc þ Aa Þ  100 ð1Þ
where Ac and Aa were the area of crystallinity region and the area of
amorphous region of a sample determined from a diffractogram,
respectively.
2.5. Morphology
A LEO 1455 VP scanning electron microscope (Oberkochen, Ger-
many) was employed to study the morphology of a sample. Each
tested sample was sputter-coated with a thin layer of gold to pre-
vent electrical charge during observation and a sample was
immersed into liquid nitrogen before being fractured.
2.6. Mechanical properties
Mechanical tests were conducted according to ASTM: D-638 at
the temperature of 23 ± 1 °C and relative humidity of 60 ± 5%. A
sample was conditioned at the temperature and relative humidity
of testing for 24 h prior to the test. A mechanical measurement of
each dumbbell-shaped specimen was carried out using a Universal
Testing Machine (Lloyd Instrument, LR 5 K, West Sussex, UK) with
a 100 N load; the crosshead speed was maintained at 40 mm/min.
It should be noted that the mechanical property results of different
composites were obtained by averaging the measurement results
of ten independent specimens. Hardness test was conducted
according to ASTM: D-2240 using Shore D hardness durometer.
Ten different measurements were carried out for a sample to
obtain average values of hardness.
2.7. Water absorption
Water absorption test was carried out according to ASTM: D-
570. Newly prepared sample was dried at 105 °C for 3 h and then
immersed in distilled water. The amount of water absorbed by a
sample was determined daily for 30 days. The percentage of water
absorption was calculated as followed:
Water absorption ¼ ðW 2  W 1 Þ=W 1  100 ð2Þ
where W2 and W1 were the wet weight and the dried weight of a
sample, respectively.
266 J. Prachayawarakorn, W. Pomdage / Materials and Design 61 (2014) 264–269
2.8. Biodegradation by soil burial test
A dumbbell sample was buried at approximately 10 cm under
the soil surface. The water content of the soil was in the range of
30–40% and the test was carried out for 0, 6 and 12 weeks. After
that, the tensile test of a soil-buried sample was conducted in com-
parison with an original sample.
3. Results and discussion
3.1. IR spectroscopic study
Fig. 1(a) shows the FTIR spectra of the non-modified TPCS/LDPE
composite. The main peak positions in the range of 3500–
3250 cm1, 3000–2800 cm1, 1640 cm1, 1465 cm1, 1300–
1000 cm1 and 1200–1000 cm1 were assigned for the O–H
stretching from the TPCS, C–H stretching of CH2 and/or CH3 of
the TPCS/LDPE and MAPE, O–H bending of water presented in the
TPCS, C–H bending of CH2 from the LDPE and MAPE, C–O–C
stretching from the TPCS and C–O–H bending of the TPCS, respec-
tively [15].
The FTIR spectrum in Fig. 1(b) showed that most peak positions
of the carrageenan-modified TPCS/LDPE composite were similar to
those obtained from the non-modified TPCS/LDPE composite
(Fig. 1(a)). This was due to the similarity of the chemical structure
of the carrageenan which was also based on polysaccharide, lead-
ing to the overlapped peak positions. However, the shift of the O–H
stretching peak to lower wavenumber was detected in the TPCS/
LDPE composites incorporated by the carrageenan, suggesting that
new hydrogen bonds were formed between the TPCS and the car-
rageenan with the presence of the LDPE.
The FTIR spectra of different TPCS/LDPE composites modified by
the cotton fibers (Fig. 1(c)) including by both the carrageenan and
the cotton fibers (Fig. 1(d)) appeared similar; however, the peak
position of the O–H stretching region also shifted to lower wave-
number. The results indicated that the new hydrogen bond forma-
tion was also found in the TPCS/LDPE composite reinforced by the
cotton fibers as well as in the carrageenan-modified TPCS/LDPE
composites reinforced by the cotton fibers. The shift of the IR peak
position of O–H stretching has also been reported for TPS
Fig. 1. FT-IR spectra of different TPCS/LDPE composites (a) TPCS/LDPE, (b) TPCS/LDPE/CG, (c) TPCS/LDPE/CF and (d) TPCS/LDPE/CG/CF.
reinforced by cellulose fibers [5,9–10] and claimed to be due to
hydrogen bonding existed between two compatibility polymers
[16].
3.2. X-ray diffraction
The XRD diffractogram of the non-modified TPCS/LDPE compos-
ite is presented in Fig. 2(a). The TPCS component showed the peak
at 2h of 19.6°, corresponded to the Vh-type pattern of starch due to
the amylose–lipid complex formation forming by the effective
starch gelatinization [17]. The LDPE component of the non-modi-
fied composite showed the peaks at 2h of 21.3°, 23.6° and 36.0°,
corresponded to the orthorhombic crystal structure of polyethyl-
ene [18]. In general, cotton fibers with cellulose I crystal structure
showed the main XRD peaks at 2h of 18.0°, 23.3° and 26.0° [19];
whereas, carrageenan showed the main peak at 2h of 12.5°, corre-
sponded to the double-helix triagonal unit cell [20]. It should be
noted that the crystallinity of the non-modified TPCS/LDPE com-
posite mainly resulted from the LDPE component since the LDPE
component caused the major peak intensity in the diffractograms.
For the TPCS/LDPE composites modified by the carrageenan
(Fig. 2(b)), by the cotton fibers (Fig. 2(c)) or by both the carra-
geenan and the cotton fibers (Fig. 2(d)), no change in the XRD dif-
fractograms was detected, indicating that the carrageenan and/or
the cotton fibers did not interfere the orientation and the crystal
formation of the TPCS/LDPE composites. The percentage crystallin-
ity values of different TPCS/LDPE composites obtained from the
XRD technique were found to be approximately 35% which showed
the insignificant change with the incorporation of the carrageenan
and/or the cotton fibers.
3.3. Morphology
Morphology of the non-modified TPCS/LDPE composite
obtained from SEM technique is shown in Fig. 3(a). The micrograph
revealed that the difference morphologies between the hydrophilic
TPCS phase and the hydrophobic LDPE phase were noticed. The
surfaces of the TPCS and LDPE components appeared smooth and
rough, respectively. With the use of the MAPE compatibilizer, some
 J. Prachayawarakorn, W. Pomdage / Materials and Design 61 (2014) 264–269
Fig. 2. X-ray diffraction patterns of different TPCS/LDPE composites (a) TPCS/LDPE,
(b) TPCS/LDPE/CG, (c) TPCS/LDPE/CF and (d) TPCS/LDPE/CG/CF.
phase separation between the TPCS and LDPE phases could still be
observed.
The modification of the TPCS/LDPE composite by the carra-
geenan led to more smooth and compatible surface as shown in
Fig. 3(b). In general, j-carrageenan chemical structure can be
destroyed by heating process and form gel during cooling process
[11]. The carrageenan would possibly aggregate and form gel with
the TPCS matrix during the cooling process due to the chemical
structural similarity of polysaccharides. Moreover, the addition of
Fig. 3. SEM micrographs of different TPCS/LDPE composites (a) TPCS/LDPE, (b) TPCS/LDPE/CG, (c) TPCS/LDPE/CF and (d) TPCS/LDPE/CG/CF.
267
the carrageenan into the TPCS/LDPE matrix caused less phase dif-
ference between the TPCS hydrophilic and the LDPE hydrophobic
phases.
For all the TPCS/LDPE composites reinforced by the cotton fibers
(Fig. 3(c) and (d)), the morphology revealed that the fibers were
randomly distributed in the TPCS/LDPE matrix. Furthermore, the
surface of the cotton fibers embedded in the TPCS matrix was cov-
ered by the TPCS matrix, indicating of good phase compatibility
between the cotton fibers and the TPCS matrix. As expected, when
the cotton fibers were embedded in the LDPE matrix, no sign of
surface wetting was observed.
3.4. Mechanical properties
The effect of the carrageenan contents on the mechanical prop-
erties of different carrageenan-modified TPCS/LDPE composites are
represented in Fig. 4. It was found that the stress at maximum load
(Fig. 4(a)), Young’s modulus (Fig. 4(a)) and hardness (Fig. 4(b)) of
the carrageenan-modified TPCS/LDPE composites were signifi-
cantly higher than those of the non-modified TPCS/LDPE compos-
ite. This was due to the new hydrogen bond formation (Fig. 1)
between the TPCS and the carrageenan resulted in the difficulty
of the mobility of the polymer chains. Besides, the improved phase
morphology shown in Fig. 3 also affected the mechanical property
results. The carrageenan-modified TPCS/LDPE composites were
apparently harder; consequently, the extendibility, expressed by
the strain at maximum load was dropped (Fig. 4(b)). The mechan-
ical property results were consistent with Lafargue et al. [14] who
reported about the tensile properties of casted starch film modified
by j-carrageenan.
The influence of the cotton fibers on the mechanical properties
of the non-modified and the carrageenan-modified TPCS/LDPE
composites is shown in Fig. 5. The results indicated that the
268 J. Prachayawarakorn, W. Pomdage / Materials and Design 61 (2014) 264–269
Fig. 4. Mechanical properties of the different TPCS/LDPE composites with different
carrageenan contents (a) stress at maximum load and Young’s modulus and (b)
strain at maximum load and hardness.
Fig. 5. Mechanical properties of different TPCS/LDPE composites modified by
carrageenan and/or cotton fibers.
addition of the cotton fibers into the composites caused the com-
posites stiffer but less elastic. It should be noted that the addition
of the cotton fibers into the TPCS/LDPE composites caused more
stiffness than that of the carrageenan. This could be due to the high
crystallinity of the cotton fibers [19,21]. It should be noted that the
Fig. 6. Water absorption of different TPCS/LDPE composites modified by carra-
geenan and/or cotton fibers.
TPCS/LDPE composite reinforced by both the carrageenan and the
cotton fibers showed the highest stress at maximum load, Young’s
modulus and hardness. The increase in the stress at maximum
load, Young’s modulus and hardness were found to be approxi-
mately 27.5%, 320% and 31.0%, respectively.
3.5. Water absorption
The result of percentage water absorption of different TPCS/
LDPE composites after water immersion carried out at the temper-
ature of 30–32 °C is presented in Fig. 6. It was found that all TPCS/
LDPE composites showed the rise in the percentage water absorp-
tion when the water immersion time increased. This was mainly
due to the hydrophilic components in the composites, i.e. the TPCS,
the carrageenan and the cotton fibers. However, no significant dif-
ference in the percentage water absorption among different com-
posites could be noticed. The percentage water absorption of all
TPCS/LDPE composites determined after 30 days of the testing
was found to be approximately 7%.
3.6. Biodegradation by soil burial test
Biodegradation test was conducted using soil burial test. Differ-
ent TPCS/LDPE composites were buried under soil surface for 0, 6
and 12 weeks; then, the tensile test was carried out. It was found
from Fig. 7 that, for the non-modified TPCS/LDPE composite, the
increase duration of the biodegradation test caused a decrease of
the stress at maximum load (Fig. 7(a)) and Young’s modulus
(Fig. 7(b)) because the TPCS component was degraded by the
microorganisms existed in soil. This was also because the compos-
ite absorbed water from the soil; as a result, the occurrence of fun-
gus in various parts of the composite was detected.
Moreover, the addition of the carrageenan and/or the cotton
fibers into the TPCS/LDPE composites caused a significant drop of
the stress at maximum load and Young’s modulus, compared with
the non-modified TPCS/LDPE composite. This was because of the
biodegradable parts of the TPCS, the carrageenan and the cotton
fibers. The results suggested that the incorporation of the carra-
geenan and/or the cotton fibers into the non-modified TPCS/LDPE
composite could accelerate the biodegradation of the non-modified
 J. Prachayawarakorn, W. Pomdage / Materials and Design 61 (2014) 264–269
Fig. 7. Mechanical properties of different composites modified by carrageenan and/
or cotton fibers after soil burial test for 12 weeks (a) stress at maximum load, (b)
Young’s modulus and (c) strain at maximum load.
composite. On the contrary, the strain at maximum load was, oppo-
sitely, increased as shown in Fig. 7(c) since the composites became
softer. It should be mentioned that the stress at maximum load and
the Young’s modulus of the carrageenan-modified TPCS/LDPE com-
posite, after 12 weeks of the soil burial test, were lower than those
of the cotton fiber-modified TPCS/LDPE composite. The results sug-
gest that the carrageenan shows more efficiency for the accelera-
tion of the biodegradation process than the cotton fibers.
4. Conclusions
The biodegradable TPCS/LDPE composites, processed by injec-
tion molding machine, were modified using the carrageenan and/
or the cotton fibers. IR peak shift of the O–H stretching region
269
was observed in all of the modified TPCS/LDPE composites. Degree
of crystallinity of all the composites was approximately 35%. The
significant improvement of mechanical properties of the compos-
ites was obtained by the addition of the carrageenan and/or the
cotton fibers. The highest mechanical properties was found for
the TPCS/LDPE composites modified by both the carrageenan and
the cotton fibers. The increase of the stress at maximum load
and Young’s modulus was approximately 27.5% and 320%, respec-
tively. The percentage water absorption of all the modified com-
posites was approximately the same as the non-modified
composite. Besides, all of the modified composites were easier to
degrade, compared with the non-modified composite.
Acknowledgement
The authors express their sincere appreciation to KMITL
Research Fund for supporting the study financially.
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