SYNTHESIS AND CHARACTERIZATION OF NANOCHITOSAN- …

www.wjpr.net Vol 7, Issue 8, 2018. 533

Sudha et al. World Journal of Pharmaceutical Research

SYNTHESIS AND CHARACTERIZATION OF NANOCHITOSAN-

POLYVINYL ALCOHOL-CARBOXYMETHYL STARCH TERNARY

BLENDS OF VARIOUS COMPOSITIONS WITH GLUTARALDEHYDE

AS CROSSLINKING AGENT

K. Rajeshwari1, T. Gomathi

2 and P. N. Sudha

2*

1Department of Chemistry, Adhi College of Engineering, Kanchipuram.

*2PG and Research Department of Chemistry, D.K.M College for Women, Vellore,

Tamil Nadu, India.

ABSTRACT

The interest in biopolymers and its derivatives has increased in recent

years due to its following properties such as biodegradability,

biorenewability, biocompatibility, physiological inertness and

hydrophilicity. The primary purpose of this study is to provide

complete global level value of its one of the derivative chitosan in

nanoform as nanochitosan mainly remediating tannery effluents. The

nanochitosan has larger surface area as compared to chitosan. The

present study explores the synthesis of nanochitosan/polyvinyl alcohol/

carboxymethylstarch a ternary blends of various ratio (1:1:1), (1:2:1),

(1:1:2) and (2:1:1) with glutaraldehyde as a crosslinking agent. The

prepared blends were characterized using sophisticated analytical tools

such as Fourier transform infrared spectroscopy (FTIR), X-ray diffraction studies (XRD),

Thermal analysis (TGA and DSC) and Scanning electron microscopic images (SEM)which

confirms the formation of blends and its thermal stability.

KEYWORDS: Nanochitosan, polyvinyl alcohol, carboxymethyl starch, ternary blends,

Characterization.

1. INTRODUCTION

The nanochitosan has more advantages than chitosan such as higher surface area, chemical

and mechanical stability. It is a natural material with excellent physiochemical properties

World Journal of Pharmaceutical Research SJIF Impact Factor 8.074

Volume 7, Issue 8, 533-549. Conference Article ISSN 2277– 7105

*Corresponding Author

Dr. P. N. Sudha

P.G. and Research

Department of Chemistry,

D.K.M College for

Women, Vellore,

TamilNadu, India.

Article Received on

05 March 2018,

Revised on 25 March 2018,

Accepted on 15 April 2018

DOI: 10.20959/wjpr20188-11171



environment friendly material, possesses bio activity and does not harm humans it also has

high catalytic activity, anti bacterial and shrink –proofing properties, material having

excellent physicochemical properties, this makes it a good applicant in drug and gene

delivery, and also in removal of heavy metal.[1]

The polyvinyl alcohol is nontoxic, good

barrier for oxygen, aroma, oil and solvents, which is prepared by partial or complete

hydrolysis of poly (vinyl acetate), Polyvinyl Alcohol is a synthetic resin with hydrophilic

properties, it increases the persistence of the tear film and therefore used as a lubricant, forms

a soluble plastic film upon drying.[2,3]

The carboxymethyl starch is a natural starch derivative,

which is a linear and branched starch polymer. The starch becomes more resistant to thermal

degradation and bacterial attack because of it. Carboxymethylstarch is a derivative of starch.

It has stability against freezing, excessive heat, and acids. Carboxymethyl starch is a

renewable, nontoxic, and biodegradable polysaccharides with numerous applications such as

removal of cations like calcium, iron, from dispersed phase.CMS has been extensively

applied as wall paper adhesive, as textile printing thickener and also has applications in the

pharmaceutical industry, cationic starch is used as wet end sizing agent in paper

manufacturing.[4,5]

The main aim of the present study was just to synthesize the

nanochitosan/polyvinyl alcohol/ carboxymethylstarch blends of various ratios. The prepared

blends were characterized and then the results were investigated.

2. MATERIALS AND METHODS

2.1 MATERIALS

Chitosan was gifted by India sea foods, Cochin, Kerala for our study. Carboxymethyl starch

and Polyvinylalochol were of Sigma Aldrich, India, and Sodium tripolyphosphate were

obtained from Central Drug House Pvt. Ltd. All other chemical used were of analytical grade.

Millipore water was prepared in the laboratory by double distillation of deionised water in

quartz distillation plant.

2.2 METHODS

2.2. A. Preparation of Nanochitosan by Ionotropic gelation

The nanochitosan was prepared by ionotropic gelation method using sodium

tripolyphosphate. Ionotropic gelation is based on the ability of polyelectrolyte to cross link in

the presence of counter ions to form hydrogels the faster ionic reactions between chitosan and

TPP, non toxic nature of these components and easy process, we adopted the gel ionization

technique for the synthesis of nanochitosan particles.[6]

http://en.wikipedia.org/wiki/Derivative_%28chemistry%29

http://en.wikipedia.org/wiki/Wallpaper_adhesive

http://en.wikipedia.org/wiki/Textile_printing

http://en.wikipedia.org/wiki/Sizing

http://en.wikipedia.org/wiki/Paper_machine

http://en.wikipedia.org/wiki/Paper_machine



2.2. B. Preparation of Nanochitosan (NCS) - Polyvinyl alcohol (PVA) and

Carboxymethyl starch (CMS) a ternary blend (Ratio - 1:1:1, 1:2:1, 1:1:2, 2:1:1)

The ternary blend of nanochitosan - polyvinyl alcohol and carboxymethylstarch with

glutraldehyde of above ratios were prepared. About 1 g of nanochitosan in dispersed form in

distilled water was weighed and taken along with, 1 gm of polyvinyl alcohol which was

dissolved in minimum quantity of distilled water separately and was dissolved with 1 gm

weight of Carboxymethyl Starch dissolved in minimum amount of distilled water in a beaker

separately. The above solutions were then thoroughly mixed under magnetic stirring with 7ml

of glutraldehyde as a crosslinking agent and thereafter filtered, washed thrice with double

distilled water. These biopolymeric ternary blends were stored at room temperature in double

distilled water for few hours and then dried by pouring in a Petri dish and for 24 hrs of 1:1:1

ratio, in similar manner other ratios were also prepared of different proportions.[6,7,8]

3. Characterization of Polymer blends

FTIR study was carried by using Perkiln- Elmer spectrophotometer. The prepared

nanochitosan-polyvinyl alcohol & carboxymethylstarch ternary blends were studied by FTIR

in the wavelength range between 400cm-1

and 4000cm-1. X–ray diffraction (XRD) patterns of

nanochitosan-polyvinyl alcohol & carboxymethylstarch ternary blend composites were

investigated using X-ray powder diffractometer (XRD – SHIMADZU XD – D1) using a Ni –

filtered Cu K X–ray radiation source. The comparative intensities were recorded within the

range of 100

– 900 (2 ) at a scanning rate of 50min

-1. Thermogravimetric analysis was studied

to quantify the thermal weight loss of the nanochitosan-polyvinyl alcohol &

carboxymethylstarch ternary blend on a SDT Q600 V8.0 build 95 instrument at a heating rate

of 100C per minute in nitrogen atmosphere. The weight losses at different stages were

analysed. The differential scanning calorimeter (DSC) was used to observe the thermal

property of the nanochitosan-polyvinyl alcohol & carboxymethylstarch ternary blend

composites. The measurements were performed with NETZSCH DSC 200 PC in a pan Al,

pierced lid in the N2 atmosphere at a heating rate of 100 K /min. The results were recorded

and analysed. The surface morphology and cross sectional morphology of the nanochitosan-

polyvinyl alcohol & carboxymethylstarch ternary blend composites were observed with

scanning electron microscopy to confirm the compatibility of the mixtures of nanochitosan-

polyvinyl alcohol & carboxymethylstarch ternary blend. For the examination, the samples

were cut into pieces of various sizes and wiped with a thin gold – palladium layer by a sputter



coater unit (VG – microtech, UCK field, UK) and the cross section topography was analysed

with a Cambridge stereoscan 440 scanning electron microscope (SEM, Leica, Cambridge.).

4. RESULTS AND DISCUSSION

4.1 FT-IR spectroscopy

FTIR spectroscopy provides information on the blend and composite composition and also

polymer - polymer interactions. The following section describes the FT-IR spectral details of

nanochitosan (Figure 1), and NCS/PVA/CMS composites of various composition is described

in the (Figure 1 a,b,c,d) weight ratio in the presence of the cross linking agent glutaraldehyde.

Fig: 1. The FT- IR spectrum of nanochitosan.

The spectra shows major peak at 3386.92cm-1

corresponds to –OH stretching of axial OH

group, -NH stretching. The peak obtained at 2908.57cm-1

corresponds to the aliphatic –CH

asymmetric stretching. Certain peaks observed at 1635.20cm-1

, 897 cm-1

corresponds to –NH

bending and C-C stretching. P=O Stretching 1219.00 cm-1

, P-O stretching 1058.87 cm-1

are

the additional peak seen in nanochitosan which was not present in chitosan. C-O- C stretch

1163.38 cm-1

also observed.[6,7,8]



H:\1\MEAS\.8 RG11 Instrument type and / or accessory 09/01/2013

3324.1

8

2936.5

9

2363.2

02332.5

4

2193.7

52119.2

9

1715.8

3

1637.5

71593.4

2

1414.9

3

1369.9

3

1251.4

3

1081.1

8

1016.3

9

846.8

6

500100015002000250030003500

Wavenumber cm-1

60

70

80

90

10

0

Tra

nsm

itta

nce

[%

]

Page 1/1

Fig.1.a. FTIR Spectra of NCS/PVA/CMS (1:1:1) with GLU.

Fig.1.b. FTIR Spectra of NCS/PVA/CMS [1:2:1] with GLU.

Fig. 1. c. FTIR Spectra of NCS/PVA/CMS [1:1:2] with GLU.



Fig. 1. d. FTIR Spectra of NCS/PVA/CMS [2:1:1] with GLU.

Thus the shift in the peak confirms the perfect formation of blend.

Table: 1. FTIR Spectral details of Nanochitosan, Polyvinyl alcohol, Carboxymethyl

starch ternary blend of various compositions.

The FTIR spectrum of Nanochitosan, Polyvinyl alcohol, Carboxymethylstarch (1:1:1) with

GLU ternary blend compared to other ratio. The broad band at 3324.18cm-1

upon blending is

due to the intermolecular hydrogen bonding N-H and O-H stretching vibration. On

comparing with pure nanochitosan the above mentioned peak has been shifted to lower wave

number during blending. The absorption bands present at 1715.83 cm-1

and 1637.57cm-1

is

assigned to the C=O and C=N stretching vibrations.

Responsible group

Wave number cm-1

(1:1:1) with

GLU

(1:2:1) with

GLU

(1:1:2) with

GLU

(2:1:1) with

GLU

N-H stretching and O-H

stretching 3324.18 3332.85 3334.86 3332.86

C-H asymmetric modes 2936.59 2939.18 2939.53 2938.40

C=O stretching 1715.83 1717.76 1716.07 1716.78

Carbonyl stretching (amide

I) and C=N stretching 1637.57 1648.57 1643.88 1641.18

-CH2 scissoring 1414.93 1427.35 1431.39 1416.02

O-H bending 1369.93 1371.78 1370.60 1326.88

P=O stretching 1251.43 1250.90 1253.04 1252.56

C-O-C stretching of

polysaccharide structure.

1081.18,

1016.39

1086.62,

1020.48

1098.57,

1017.82

1081.86,

1017.94

CH2 rocking 846.86 837.23 848.85 845.64



4.2. XRD STUDIES

Fig: 2. XRD pattern of the nanochitosan.

Fig: 2. a. XRD pattern of NCS/PVA/CMS (1:1:1) with GLU.

Fig: 2. b. XRD pattern of NCS/PVA/CMS (1:2:1) with GLU.



Fig: 2. c. XRD pattern of NCS/PVA/CMS (1:1:2) with GLU.

Fig: 2. d. XRD pattern of NCS/PVA/CMS (2:1:1) with GLU.

Table – 2: XRD details of Nanochitosan and NC/PVA/CMS blends.

Samples 2 θ Values Xc%

Nanochitosan 27º - 16.2

NC/PVA/CMS (1:1:1)+ GLU 19° - 19.8

NC/PVA/CMS (1:2:1) + GLU 19° - 21.3

NC/PVA/CMS (1:1:2) + GLU 20° 30° 27.10

NC/PVA/CMS (2:1:1) + GLU 20° - 28.72

From the XRD pattern of NC/PVA/CMS ternary blends with GLU a broad distorted

humplike diffraction peak at around 2θ = 190 was obtained for all the ratios, thus indicating

amorphous morphology of the blend.

From the degree of cystallinity values as given in the Table - 2 it was concluded that when

the concentration of PVA increases the morphology of blend changes to semi crystalline form

whereas increase in concentration of NC and CMS makes the blend more amorphous.



4.3 Thermogravimetric Analysis

Thermogravimetric analysis (TGA) is a thermal analysis techniques used to characterize a

wide variety of materials it gives a relation between losses in weight of material with

temperature. Thermal details of ternary blends of NC/PVA/CMS of various ratios in presence

and of glutaraldehyde are discussed below.[8]

Fig.3. Thermogram of Nanochitosan.

Residue:0.2570%(0.008216mg)

12.79%(0.4088mg)

79.11°C

111.12°C

98.27°C

154.88°C

35.09%(1.122mg)

319.09°C

376.74°C

353.63°C

26.41%(0.8442mg)

432.36°C

472.91°C

446.37°C

0.0

0.1

0.2

0.3

0.4

0.5

Der

iv. W

eigh

t (%

/°C

)

5

25

45

65

85

105

Wei

ght (

%)

0 100 200 300 400 500 600 700 800

Temperature (°C)

Sample: Sudha RG6 feb 21 2013Size: 3.1970 mg DSC-TGA

File: C:...\2013\Sudha RG6 feb 21 2013.001Operator: TARun Date: 2013-02-21 12:18Instrument: SDT Q600 V8.0 Build 95

Universal V4.1D TA Instruments

Fig: 3. a. Thermogram of NCS/PVA/CMS (1:1:1) with GLU.

10.25%(0.3070mg)

67.27°C

121.23°C

97.07°C

66.51%(1.993mg)

299.82°C

377.44°C

337.97°C

22.67%(0.6792mg)

443.21°C

474.28°C

435.53°C

456.01°C

Residue:0.1296%(0.003884mg)

0.0

0.2

0.4

0.6

0.8

Der

iv. W

eigh

t (%

/°C

)

5

15

25

35

45

55

65

75

85

95

105

115

Wei

ght (

%)

0 100 200 300 400 500 600 700 800

Temperature (°C)

Sample: Sudha RG 3 feb 19 2013Size: 2.9960 mg DSC-TGA

File: C:...\2013\Sudha RG 3 feb 19 2013.001Operator: TARun Date: 2013-02-19 15:18Instrument: SDT Q600 V8.0 Build 95


Fig: 3. b. Thermogram of NCS/PVA/CMS (1:2:1) with GLU.



10.87%(0.2761mg)

84.44°C

123.83°C

99.48°C

46.48°C

16.77%(0.4261mg)

237.39°C

292.15°C

282.56°C

52.65%(1.338mg)

400.38°C

457.68°C

437.94°C

Residue:6.046%(0.1536mg)

0.0

0.2

0.4

0.6

0.8

Deriv. W

eig

ht (%

/°C

)

10

20

30

40

50

60

70

80

90

100

110

120

Weig

ht (%

)

0 100 200 300 400 500 600 700 800

Temperature (°C)

Sample: Sudha AIS 1 May14 2013Size: 2.5410 mg DSC-TGA

File: C:...\2013\Sudha AIS 1 May14 2013.001Operator: TARun Date: 2013-05-14 14:38Instrument: SDT Q600 V8.0 Build 95


Fig: 3. c. Thermogram of NCS/PVA/CMS (1:1:2) with GLU.

Residue:0.1936%(0.003484mg)

18.38%(0.3308mg)

76.36°C

126.08°C

99.48°C

31.28%(0.5631mg)

275.73°C

306.22°C

298.22°C

351.22°C

447.58°C

0.0

0.2

0.4

0.6

0.8

Deriv. W

eig

ht (%

/°C

)

-15

5

25

45

65

85

105

Weig

ht (%

)

0 100 200 300 400 500 600 700 800

Temperature (°C)

Sample: Sudha BD3 Jan 4 2013Size: 1.8000 mg DSC-TGA

File: E:\2010\Sudha BD3 Jan 4 2013.001Operator: TARun Date: 2013-01-04 09:13Instrument: SDT Q600 V8.0 Build 95


Fig: 3. d. Thermogram of NCS/PVA/CMS (2:1:1) with GLU.

Table 3: TGA Thermal details of Nanochitosan and Nanochitosan, Polyvinyl alcohol,

Carboxymethyl starch ternary blends with GLU.

Percentage

Decomposition

%

Decomposition Temperature º C

(1:1:1) with

GLU

(1:2:1) with

GLU

(1:1:2) with

GLU

(2:1:1) with

GLU

10 110 140 110 100

20 160 270 180 140

30 180 320 270 270

40 250 340 350 290

50 350 350 390 300

60 370 360 430 310

70 400 377.44 450 360

80 430 443.21 457.68 370

90 460 468 - 447.58



Fig. 3.e TGA Thermal details of NCS/PVA/CMS ternary blends with GLU.

The thermal detail also shows two significant weight losses, one weight loss at 50-100°C is

due to the moisture vaporization, the other at 300-400°C is due to the maximum thermal

degradation between PVA and CMS and above 450 °C due to the thermal degradation of

crosslinkages in nanochitosan. The sample of various ratio compared was found that they

disintegrate at high temperature and residues were observed even at 700°C. The highest

weight loss occurs at a temperature range 266.46 – 477.17°C.

4.4 Differential Scanning Calorimetry (DSC)

The differential scanning calorimeter (DSC) is a basic tool in thermal study. It can be used in

many industries from Pharmaceuticals and polymers, to nanomaterials and food products.[9,10]

The DSC thermal data of nanochitosan, ternary blends of NC: PVA: CMS of various ratios in

presence glutaraldehyde were discussed below:

Fig: 4. DSC curves of the nanochitosan.



150.52°C

142.41°C40.31J/g

200.30°C

191.14°C2.279J/g

288.50°C

256.36°C86.05J/g

-3.0

-2.5

-2.0

-1.5

-1.0

-0.5

0.0

He

at

Flo

w (

W/g

)

0 50 100 150 200 250 300 350 400

Temperature (°C)

Sample: sudha sm1 June 122013Size: 1.9000 mgMethod: Ramp

DSCFile: C:...\2012\sudha sm1 June 122013.001Operator: TARun Date: 2013-06-12 09:49Instrument: DSC Q10 V9.0 Build 275

Exo Up Universal V4.1D TA Instruments

Fig: 4.a. DSC curves of NCS/PVA/CMS (1:1:1) with GLU.

241.82°C

215.41°C70.50J/g168.79°C

158.69°C2.594J/g

71.23°C

46.26°C114.0J/g

-4

-3

-2

-1

0

He

at

Flo

w (

W/g

)

0 50 100 150 200 250 300 350 400

Temperature (°C)

Sample: Sudha GG2 Aug 19 2013Size: 1.1000 mgMethod: Ramp

DSCFile: E:\2010\Sudha GG2 Aug 19 2013.001Operator: TARun Date: 2013-08-20 10:43Instrument: DSC Q10 V9.0 Build 275


Fig: 4.b. DSC curves of NCS/PVA/CMS (1:2:1) with GLU.

213.13°C

202.85°C5.497J/g

277.15°C

259.50°C90.38J/g

81.42°C

77.24°C3.888J/g

-6

-4

-2

0

Heat F

low

(W

/g)

0 50 100 150 200 250 300 350 400

Temperature (°C)

Sample: Sudha GG1 Aug 19 2013Size: 1.0000 mgMethod: Ramp

DSCFile: E:\2010\Sudha GG1 Aug 19 2013.001Operator: TARun Date: 2013-08-20 09:19Instrument: DSC Q10 V9.0 Build 275


Fig: 4.c. DSC curves of NCS/PVA/CMS (1:1:2) with GLU.



Fig: 4.d. DSC curves of NCS/PVA/CMS (2:1:1) with GLU.

Table – 4: DSC Thermogram of the NC/PVA/CMS blends of various ratios prepared in

the presence of glutaraldehyde.

Sample Tg °C Tc °C Tm°C

Nanochitosan 142.5 68 217.57 >300

NC/PVA/CMS 1:1:1 + Glu 175 150.52 200.30 256.36

NC/PVA/CMS 1:2:1 + Glu 215 71.23 158.69 241.82

NC/PVA/CMS 1:1:2 + Glu 240 81.42 213.13 277.15

NC/PVA/CMS 2:1:1 + Glu 285 45.11 265.11 336.11

For the blends in presence of crosslinking agent glutaraldehyde the Tg value of

NC/PVA/CMS (1:1:1,1:2:1, 1;1:2, 2:1:1) was found to be 175°C, 215°C, 240°C, and 285 °C

respectively which was greater than nanochitosan. Also the single Tg value expressing

polymer- polymer miscibility.

4.5. SEM ANALYSIS

The scanning electron microscope (SEM) uses a focused beam of high-energy electrons to

generate a variety of signals at the surface of solid specimens. The signals that derive from

electron-sample interactions reveal information about the sample including external

morphology (texture), chemical composition, and crystalline or amorphous form and

orientation of materials making up the sample.[11,12]

http://serc.carleton.edu/research_education/geochemsheets/electroninteractions.html



Fig: 3. SEM image of Nanochitosan.

Fig: 3. a. SEM image of NCS: PVA: CMS (1:1:1) with GLU.

Fig: 3.b.SEM image of NCS: PVA: CMS (1:2:1) with GLU.

Fig: 3.c. SEM image of NCS:PVA:CMS(1:1:2) with GLU.



Fig: 3.d. SEM image of NCS: PVA: CMS (2:1:1) with GLU.

Thus suggesting that the blend has high coarse and porous area. When samples with

crosslinking agent glutaraldehyde (Figure: 3.a, b, c, d.) compared with the nanochitosan.

The surface smoothens on addition of crosslinking agent as shown in the figure.

The observed results indicate that a very good interfacial adhesion between the ternary blend.

The prepared ternary blend of ratio 1:1:1 ratio was found to be highly suitable for the

adsorption process and this may be due to the rough surface nature of blends.

CONCLUSION

The present study was mainly aimed to synthesize and the characterization was carried out

for the prepared blends to confirm its formation and suitability for adsorption. The result of

FTIR confirms the nanochitosan were effectively bound with polyvinyl alcohol and

carboxymethylstarch. TGA and DSC show the thermal stability and compatibility of the

blends. The FTIR results exhibits the formation of the ternary blend prepared in the presence

of glutaraldehyde by studying its various functional group. The, appearance and

disappearance of peaks and the shift in peak position during formation of blend was very well

revealed in the FTIR results. The convalent interaction such as imine formation and the non-

covalent interactions were seen in the ternary blends in the presence of glutaraldehyde.

Further analysis such as XRD results confirm these interactions which were supported by the

change in crystallinity value after blending. The amorphous nature of the blends increases

comparatively. Especially to NC/PVA/CMS (1:1:1) ternary blend prepared in the presence of

glutaraldehyde and it can be further applied for the removal of heavy metal studies due to its

increased amorphous nature. This type of work could encourage the synthesis of new

polymers, where some functionality is required, for specific purposes.



4.6. Proposed mechanism for the synthesis of nanochitosan ternary blend

(NC/PVA/CMS) with glutaraldehyde.

.

.

HO

P

O

P

O

P

HO

O

O

O

O

O

O

NANOCHITOSAN

O

OO

CH2OH

NH3+

OH

n

O

O

CH2OH

NH3+

OH

.

O

O O

CH2OH

NH2

OHO

O

CH2OH

NH3+

OH

n

* *

OH OH

POLYVINYL ALCOHOL

n

.

.

HOP

OP

OP

OH

OOO

OOO

O

O

O

CH2OH

+H3N

OH

n

O

O

CH2OH

+H3N

OH

.

O

O

O

HOH2C

N

HO

O

O

HOH2C

NH3+

HO

n

*

*

OH

OHn

*

* OH

OHn

*

*

OH

OH

n

*

*HO

HO

n

NC/PVA/CMS + GLU - TERNARY BLEND

O

O

O

O

O

OO

OH

OH

OH

OH

O

OH

OH

OH

OH

O

ONa

n

O

O

O

O

O

O

O

HO

HO

OH

HO

O OH

HO

OHHO

OO

n

*

*HO

HOn

CARBOXYMETHYL STARCH

O O

GLUTRALDEHYDE

O

O

OO

O

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