ARTICLE IN PRESS

Physica B 405 (2010) 20212027

Contents lists available at ScienceDirect

Physica B
journal homepage: www.elsevier.com/locate/physb

Chitosan ller effects on the experimental characterization, spectroscopic

investigation and thermal studies of PVA/PVP blend lms
E.M. Abdelrazek a, I.S. Elashmawi b, S. Labeeb a,
a
Physics Department, Faculty of Science, Mansoura University, Mansoura 35516, Egypt
b
Spectroscopy Department, Physics Division, National Research Centre, Giza, Egypt

a r t i c l e in fo abstract

Article history: Structural, optical, thermal and morphological studies were performed for pure PVA/PVP (50/50) blend
Received 11 October 2009 and PVA/PVP blend lled with different concentrations of chitosan upto 40 wt% using casting method.
Received in revised form The prepared lms were investigated by different techniques. All techniques demonstrate the
16 December 2009
complexation between chitosan and the polymers blend. There were some changes in the IR absorption
Accepted 17 January 2010
bands position and its intensities. UVvis analysis revealed intensity of the shoulder around
273280 nm increase with increasing chitosan content. Differential scanning calorimetry (DSC) showed
Keywords: thermal stability of the product samples and that has improved after lling chitosan increases. Scanning
Polymer blend electron microscope (SEM) images of different concentrations of lms revealed that large crystals
Chitosan
characteristic of chitosan were also frequently present, when chitosan content increase upto 20 wt%,
PVA/PVP blend
rough surfaces and crystalline structures are the dominant features. The X-ray diffraction (XRD) showed
FT-IR
X-ray that the incorporation of chitosan into the polymeric matrix causes decreasing in the crystallinity
SEM degree of the samples and this indicates the complexation between the ller and the polymers
DSC blend. Thermogravimetric analysis (TGA) is used to study the samples in the temperature range of
30500 1C. Figures show typical TGA thermograms of weight loss as a function of temperature for the
present system.
& 2010 Elsevier B.V. All rights reserved.

1. Introduction usually have larger diameters in several microns compared with

Chitosan, the deacetylated derivative of chitin, is one of the
abundant, renewable, nontoxic and biodegradable carbohydrate
polymers and available largely in the exoskeletons of shellsh and
insects. Chitosan has been widely applied as a functional
biopolymer in food and pharmaceutics. Chitosan is known to
have various biological activities including immunoenhancing
effects, antitumoral, antifungal and antimicrobial activities [13].
The unique characteristics of chitosan nanoparticles could provide
a higher afnity for negatively charged biological membranes and
site-specic targeting in vivo [4].
Chitosan, a copolymer of glucosamine and N-acetyglucosa-
mine units linked by 14 glucosidic bonds, is a cationic
polysaccharide obtained by alkaline deacetylation of chitin.
Because of its biodegradability, nontoxicity, biocompatibility,
and antifungal activity, chitosan and its derivatives have been
widely used in the elds of medicine, cosmetics, agriculture,
biochemical separation systems, tissue engineering and so on
[58]. Chitosan bers, traditionally produced by wet spinning,
 Corresponding author. Tel.: + 20 108734123; fax: + 20 502246781.
E-mail address: Soskaya@live.com (S. Labeeb).
the electrospun bers. Blending is an efcacious way to modify
spinning behaviors of chitosan.
Polymers have increasingly become attractive because of a
large number of applications, including photonics, biotechnology
and optoelectronics. The blending of different polymers or
inorganic particles with polymers represents a strategic route to
improve the performance of a material, allow realization of novel
composite systems that enhance the performance of the parent
polymer. This tailoring of the macroscopic properties by the
process of polymer blending is the result of modifying the
composite structure at the microscopic scale [9]. Generally,
solution blending of different polymers is one of the methods
used to get new material with a variety of properties. These
properties mainly depend on the characteristics of the parent
homo polymers and the blend composition [10]. Hence, the study
of these systems is receiving increasing attention, since an
adequate mixture of the polymers can be used to optimize the
performance of polymer-based systems, in a cheaper and quicker
way compared with synthesizing new polymers. In this case,
whether the behavior of the blend is intermediate between the
properties of the components or is considerably different it will be
determined by the miscibility and phase behavior of the blend.
Miscibility, at the molecular, level is possible only when the

0921-4526/$ - see front matter & 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.physb.2010.01.095
 ARTICLE IN PRESS
2022 E.M. Abdelrazek et al. / Physica B 405 (2010) 20212027
different polymers are capable of establishing specic interactions
between their chains, causing negative enthalpy and Gibbs free
energy of mixing. Poly (vinyl pyrrolidone) (PVP) is a vinyl polymer
possessing planar and highly polar side groups due to the peptide
bond in the lactam ring [11]. It is an amorphous polymer and
possesses high Tg because of the presence of the rigid pyrrolidone
group, which is strong on drawing the group and is known to form
various complexes with other polymers. On the other hand poly
(vinyl alcohol) (PVA) is a semicrystalline polymer, studied
extensively because of its many interesting physical properties,
which arise from the presence of OH groups and the hydrogen
bond formation. When these two polymers are mixed, the
interactions between PVA and PVP are expected to occur through
interchain hydrogen bonding between the carbonyl group of PVP
and the hydroxyl group of PVA. Hence, these hydrogel blends are
stable within the physiological environment because of physical
crosslinks consisting of intermolecular hydrogen bonds and
intermolecular hydrogen bonds within PVA [12].
2. Experimental work
2.1. Materials used and preparation method
Polyvinyl alcohol (PVA) from Merck, in Germany, and had
molecular weight 14 000 and polyvinyl pyrrolidone (PVP) from
Aldrich chemical co. Ltd (Gillingham, England) were used as
received. Equal quantity of PVA/PVP blend (50/50) by weight was
added to doubly distilled water with stirring the solution at 50 1C
to complete dissolution. Required quantity (0.0, 5, 10, 20, 30 and
40 wt%) of chitosan from Fluka, in USA, has high molecular weight
was also dissolved in doubly distilled water with hydrochloric
acid, HCl, with ratio (94:6) of doubly distilled water and HCl,
respectively. The solution was poured onto cleaned Petri dishes
and dried in oven at 70 1C for 4 days to ensure removal of the
solvent traces. After drying, the lms were peeled from Petri
dishes and kept in vacuum desiccators until use. The thickness of
the obtained lms was in the range of E20 mm (for FT-IR and UV
vis measurements) to E150 mm (for other measurements).
2.2. Measurements
X-ray diffraction scans were obtained using DIANO corpora-
tion-USA equipped using Cu-Ka radiation (l = 1.540 A, the tube
operated at 30 kV, the Braggs angle (2y) in the range of 5601.
FT-IR absorption spectra were carried out using the single beam
Fourier transform-infrared spectrometer (FT-IR-430, JASCO,
Japan). FT-IR spectra of the samples were obtained in the spectral
range of 4004000 cm  1. Ultra violetvisible (UVvis) absorption
spectra were measured in the wavelength region of 200700 nm
using spectrophotometer (V-570 UVvis, JASCO, Japan). Scanning
electron micrograph of the studied samples was performed
using SEM (JEOL-JSM 6100). The SEM specimens were prepared
by evaporating gold onto the lm surface after drying under
vacuum. Surface of the samples were coated with a thin layer
of gold (3.5 nm) by the vacuum evaporation technique to
minimize sample charging effects due to the electron beam. The
differential scanning calorimetery of the prepared lms was
carried out using an equipment type (Shimadzu DSC50) from
room temperature to 400 1C with a heating rate of 10 1C/min.
Shimadzu TGA-50 H was used for the thermogravimetric analysis
of the samples. A small amount of the sample was taken for the
analysis and the samples were heated from room temperature to
520 1C at a rate of 10 1C min  1 in nitrogen atmosphere on
platinum cell.
3. Results and discussion
3.1. Fourier transform infrared analysis (FT-IR)
Infrared spectroscopy has been used to identify interactions in
polymers blend. FT-IR spectroscopy is very sensitive to the
formation of hydrogen bonds [13].
Fig. 1(ac) shows FT-IR absorption spectra of pure PVA, pure
PVP and PVA/PVP (50/50) blend without and with different
concentrations of 5, 10, 20, 30 and 40 wt% from chitosan recorded
at room temperature in the region 4004000 cm  1. FT-IR
absorption bands, positions and its assignments of all prepared
composite lms are listed in Table 1 [1416].
From Fig. 1(a), for pure PVA, the bands at about 3455 and
1630 cm  1 are assigned to OH stretching and bending vibration
of hydroxyl group, respectively [16]. The band corresponding to
methylene group (CH2) asymmetric stretching vibration occurs at
about 2933 cm  1. The band at about 1096 cm  1 corresponds to
CO stretching of acetyl groups present on the PVA backbone
[14,15]. The vibrational band at about 1647 cm  1 corresponds to
CQC stretching of PVA and PVP [17].
Fig. 1(b) for pure PVP shows a small absorption band at about
1539 cm  1 that is assigned to the characteristic vibration of CQN
(pyridine ring) [17]. The absorption band at about 962 cm  1 due
to the out-of-plane rings CH bending [18].
Fig. 1(c) shows the FT-IR spectrum of pure PVA/PVP blend
without and with different fractions of chitosan. The main
characteristic bands of pure chitosan are listed in Table 2. From
the table shown, it is remarkable to nd that the bands are
assigned to saccharide structure at 1166, 1077, 1018 cm  1 and
strong amino characteristic bands a round 3430, 1660 and
1290 cm  1 are assigned to OH stretching, amide I and amide II
bands, respectively [19].
For the spectra of the weight fractions 5, 10, 20, 30 and 40 wt%
of chitosan they indicate a clear increasing in the intensity of the
band around 3380 cm  1 was attributed to a hydroxyl group (OH)
stretching vibration of PVA with a secondary amide (NH) of
chitosan. The band at around 1077 cm  1 indicates the presence of
a hydroxyl group (OH) with polymeric association and a
secondary amide (NH). Also appeared band at 1450 cm  1 for
the weight fraction Z20% of chitosan that has been assigned to
CQN pyridine ring. This conrms the complexation between the
pure blend and chitosan [19]. The small absorption band around
912 cm  1 was found to be characteristic of the syndiotactic
structure of the prepared lms. Nagura et al. [20] reported that
the syndiotacticity of the PVA samples causes dense molecular
packing in the crystal and also stronger intermolecular hydrogen
bonds, which, in return, are responsible for the disappearance of
the molecular motion. This band appeared in the spectra of
pure PVA and the lled lms, but it disappeared in the spectrum
of the pure blend and this may be attributed to the addition of
PVP to PVA.
These results manifested the conclusion of the specic interaction
in PVA/PVP blend matrixes and the chitosan as ller [21].
3.2. Optical absorption analysis
The optical absorption (UV/VIS) spectrophotometric scans in
the wavelength range of 200700 nm of pure PVA/PVP blend and
the blend lled with chitosan samples are shown in Fig. 2. The
observed spectra are characterized by a main absorption edge
around 240 nm for all curves that slightly shifted towards shorter
wavelengths with increasing chitosan content. The shift of the
absorption edge in the lled lms reects the variation in the
energy band gap, which arises due to the variation in crystallinity
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E.M. Abdelrazek et al. / Physica B 405 (2010) 20212027 2023

1.4
Pure PVA Pure PVP
0.7
1.2

0.6
1.0
0.5
Absorbance

Absorbance
0.8
0.4
0.6
0.3

0.4
0.2

0.2
0.1

0.0 0.0
4000 3500 3000 2500 2000 1500 1000 500 4000 3500 3000 2500 2000 1500 1000 500
Wavenumber (cm-1) Wavenumber (cm-1)

% Chitosan

40
Absorbance (a. u.)

30

20

10

5
0

4000 3500 3000 2500 2000 1500 1000 500

Wavenumber (cm-1)

Fig. 1. (a) FT-IR spectrum of pure PVA; (b) FT-IR spectrum of pure PVP; and (c) FT-IR spectra of PVA/PVP blend without and with different concentrations of (5, 10, 20, 30
and 40 wt%) from chitosan.

Table 1
Assignments of the FT-IR characterization bands of the pure PVA, pure PVP and pure PVA/PVP blend.

Pure PVA Pure PVP Pure blend

Wavenumber Assignment Wavenumber Assignment Wavenumber Assignment

(cm  1) (cm  1) (cm  1)

3455 OH stretching 3455 OH stretching 3380 OH stretching of alcohols and phenols

2933 CH2 2924 CH2 asymmetric stretching 1647 CQC stretching
2910 CH2 asymmetric 2892 CH2 symmetric stretching 1630 OH bending
stretching
1647 CQC stretching 1664 CQC stretching 1450 OH bending
1760 CQO stretching 1461 CH2 bending 1441 CQC (pyridine ring)
1565 OH and CH bending 962 CH out of plan rings bending 962 Out-of-plane rings CH bending
1430 OH and CH bending
1326 CH2 out of plane bending
1240 CH2 bending
1144 CH wagging
1096 COC stretching
925 CO symmetric stretching
850 CH2 rocking
803 CQC stretching
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2024 E.M. Abdelrazek et al. / Physica B 405 (2010) 20212027

Table 2
Assignments of the FT-IR characterization bands of the pure chitosan and (PVA/PVP +chitosan).

Pure chitosan PVA/PVP+ chitosan

Wavenumber (cm  1) Assignment Wavenumber (cm  1) Assignment

3480 C6OH stretching Around 3380 OH stretching

2950 NH stretching of secondary amide Around 3322 NH stretching of secondary amide
1660 Amide I band of chitosan Around 2953 Pyridine ring
1558 Amide II band of chitosan, overlapping with NH3 band (1500 cm  1) 16531648 CQC stretching
1166 Strong amino group 15581550 NH bending
1077 Around 1450 CQN pyridine ring
1018 Around 1332 CQC pyridine ring
10831090 CO stretching
849843 CQC stretching

contrast to traditional crystalline samples. Moreover, it is possible

to improve further the modied optical PVA photopolymer by the
[(100-X) PVA/PVP+ (X) chitosan]% applications of an external electric eld [24].

3.3. Scanning electron microscope (SEM)

Chitosan has a aky nature and it is poor water soluble

molecule, and so we add HCl to complete dissolution. Scanning
electron images of different concentrations of lms were
obtained. Fig. 3 illustrates the lms of PVA/PVP blend with
different concentrations 0.0, 5, 20 and 40 wt% of chitosan, Fig. 3a
X (wt%) shows smooth areas which could be visualized of polymer blends
Absorbance (a. U.)

PVA/PVP and this indicates the homogeneity between the

polymer blends. Chitosan was incorporated into the lms and it
0
appeared as smooth and rough areas which could be visualized
5 when chitosan content increase (Fig. 3b).
Large crystals characteristic of chitosan were also frequently
present, when chitosan content increases upto 20 wt%, rough
10 surfaces and crystalline structures are the dominant features in
Fig. 3c, also this scanning shows a highly polycrystalline structure,
20 these structural properties of the dried chitosan matrices may be
responsible for offering a larger surface area, and therefore, a
better matrix solvent interaction and this allows faster solvent
30 uptake.
The morphology of SEM (picture d) agree well with that in
(picture c), where the difference in Fig. 3d when chitosan content
increase (420 wt%), the dissociation process occurred. The most
obvious result is that it possessed a scaly structure.

40
3.4. Differential scanning calorimetery (DSC)

200 300 400 500
Wavelength (cm -1)
Fig. 2. UVvis spectra of pure PVA/PVP blend and the PVA/PVP blend with
different concentrations of chitosan.
within the polymer matrix [22]. The band at 218 nm in the UV
spectra is assigned to n-p*. Another absorption shoulder is
observed at about 273280 nm [23] and it may be attributed to
p-p* which comes from unsaturated bonds mainly CQO. The
increase in this shoulder with increasing chitosan content may be
attributed to the interaction between chitosan and the polymers
blend, and hence complexation. The intensity of this shoulder
increases with increasing chitosan content, and this indicates that
chitosan can be used as an optical sensor which is applied in
optical elds. And also, PVA photopolymer can be used as
materials operating for light spectra in the visible region in
600 700 An important factor in the development of new materials
based on polymeric blends, is miscibility between the polymers in
the mixture, because the degree of miscibility is directly related to
nal properties of polymeric blend. There are many studies
related to the miscibility of PVA and PVP we studied the
miscibility of PVA/PVP blend by DSC.
Fig. 4 shows the DSC thermograms for the thermal behavior of
PVA/PVP blend lms lled with mass fraction of (X)chitosan,
where X= 5, 10, 20, 30 and 40 wt% at the temperature range from
30 to 400 1C.
From the thermograms, a heat ow is observed from 30 to
40 1C, this is attributed to liberation of the small amount of
moisture that is always present in the conventional polymer
unless it is carefully vacuum dried. Pure PVA/PVP blend curve
shows a small endothermic transition (at about 50 1C) attributed
to glass transition temperature (Tg) of the relaxation process
resulting from micro-Brownian motion of the main chain back-
bone. The presence of a single glass transition temperature has
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E.M. Abdelrazek et al. / Physica B 405 (2010) 20212027 2025

Fig. 3. Morphology of pure PVA/PVP blend and PVA/PVP blend doped with chitosan: (a) Pur PVA/PVP blend; (b) 5% of chitosan; (c) 20% of chitosan; and (d) 40% of chitosan.

(x) Chitosan 120

40 [(100-X)PVA/PVP+(X)chitosan]%
30 100
Endo.

20
80 X (wt%)
Weight loss(%)

10
5
60

40 30
20
10
40
20
5

0
50 100 150 200 250 300 350 400 0 100 200 300 400 500
Temperature (C) Temperture (oC)

Fig. 4. DSC thermograms of pure PVA/PVP blend and PVA/PVP blend lled with Fig. 5. TGA thermograms of PVA/PVP blend with different fractions of chitosan
different concentrations of chitosan. ller.

been widely accepted as a demonstration of the miscibility of
polymer blends [25]. From DSC studies, single glass transition
temperatures are observed for each blend sample (Fig. 5), which
indicates that the PVA and PVP were miscible in the range of
composition tested in this study. Also, the glass transition
temperature (Tg) has also decreased this indicates that the ller
acts as a plasticizer for the polymers blend. An endothermic peak
is observed at about 170 1C indicating the PVA/PVP blend melting
temperature. However, the area under the peak in the range of
170190 1C was also found to be increasing accordingly, this peak
indicated increasing in enthalpy of melting because of increase in
the amount of chitosan crystals. The values of Tw, Tg and Tm are
listed in Table 3. From the gure and the table, PVA/PVP blend
lms with different levels of ller. These values and peaks show a
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2026 E.M. Abdelrazek et al. / Physica B 405 (2010) 20212027

Table 3
The values of Tw, Tg, Tm and Ea of pure PVA/PVP blend lled with different
concentrations of chitosan. [(100-X)PVA/PVP+(X)chitosan]%

W (wt%) Tw Tg Tm E

5 40 52 170 1.049

Intensity (a.u)
10 40 51.8 175 1.055
20 45 51.5 180 1.085 X (wt%)
30 45 50.3 189.5 1.114
40 40 50 190 1.162

0
5
small shift of melting temperature towards higher temperatures 10
as the chitosan content increases. This indicates increasing the
thermal stability of the lms up to X= 30% and for X430% we
noticed that the value of Tm remain constant. 0 10 20 30 40 50 60 70
2 (degree)

3.5. Thermogravimetric analysis (TGA)

[(100-X)PVA/PVP+(X)chitosan]%
TGA is considered as the most important method for studying
thermal stability of polymers. Moreover, the kinetics of the
accompanied decomposition reaction has been reviewed. The
sample weight decreases slowly as the reaction begins, then Intensity (a.u)
decreases rapidly over a comparatively narrow temperature range X (wt%)
and nally levels off as the reactants are used up. The shape of the
curve depends primarily upon the kinetics parameters involved,
20
i.e. order of reaction (n) and activation energy (E). The values of
these parameters are important in estimation of thermal stability.
TGA is used in studying the samples in the temperature range of
30500 1C. Fig. 5 shows typical TGA thermograms of weight loss
as a function of temperature for the present system. It is evident 40
that initial weight loss for the other samples starts around 50 1C
the lled lms, which may be due to the loss of interapped water 0 10 20 30 40 50 60 70
molecules. The second weight loss occurs at 170190 1C, which 2 (degree)
attributed to melting temperature (Tm). In general, the major
weight losses are observed in the range 340500 1C which may Fig. 6. (a, b): X-ray diffraction scans of PVA/PVP blend with different mass
fractions of chitosan.
correspond to the structural decomposition of the polymer.
Determination of the activation energy: The activation energy (E) for
the main thermal decomposition for TGA measurments of the present
samples, which depends on the residual mass, can be calculated 3.6. X-ray diffraction (XRD)
(in general) using integral equation of Coats and Redfern [26]:
    Fig. 6(a, b) show the XRD scans of pure PVA/PVP (50/50)
log1a R 2RT E blend and PVA/PVP blend lled with various mass fractions
log 2
log 1  1
T DE E 2:304RT of chitosan ller. The observed diffractograms exhibit an
where T is the absolute temperature, E is the activation energy in amorphous feature which is characterized by two halos
J/mol, R is the universal gas constant (8.3136 J/mol K), n is the order of centered at about 2y =12.81 and 20.11 characteristic of the (1 0 1)
reaction, and a is the fractional weight loss at that particular and (0 2 0) planes of semicrystalline (crystalline and amorphous)
temperature is calculated as nature of PVA/PVP blend lms, respectively [27]. The present
X-ray scans revealed no signicant change in the position of two
wi wt halos and after complexation with ller, the intensity of the blend
a 2
wi wf diffraction peaks is further decreased. This is because the
interactions between the blend and ller which leads to a
where wi is the initial weight, wt is the weight at given temperature
decrease in the intermolecular interaction between the blend
and wf is the nal weight of the sample. For n=1, Eq. (1) reduces to
chains and as well as the crystalline degree [14]. From Fig. 6(b)
   
log1a R 2RT E the XRD diffractograms a crystalline peak is observed at 2y =8.641
log log 1 0:434 3
T2 DE E RT for PVA/PVP blend lms lled with chitosan at X= 40%. Li et al.
[28] and Liu et al. [29] reported that two typical peaks at 2y = 10.31
By ploting  loglog1a=T 2  against 1000=T for each sample, we and 19.41 were observed for pure PVP. The XRD diffractograms in
obtain straight lines. Then, the apparent activation energies are Fig. 6(b) shows a small sharp peak at about 2y =19.71 and clear
calculated from the slopes of these lines using the expression: sharp peak at 32.81 resulting from the crystalline phase with the
E 2:303R  slope 4 polymeric matrix, due to increasing of chitosan content. These
scattering angles which may be associated with the reections
Values of the apparent activation energy (E) of the samples are listed (2 0 0) and (1 1 2), respectively [30]. The intensity of sharp peak
in Table 3. From this table, it clears that values of the activation (2y = 32.81) decreased with chitosan content, increases and
energy are changed due to the increasing chitosan content. enhances complexation between the polymers blend and
 ARTICLE IN PRESS
E.M. Abdelrazek et al. / Physica B 405 (2010) 20212027 2027

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