FABRICATION AND CHARACTERIZATION OF COMPOSITE...

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FABRICATION AND CHARACTERIZATION OF COMPOSITE BIODEGRADABLE FILMS FROM CHITOSAN AND CORN SILK MOHD FAIZAN JAMALUDDIN A thesis submitted in fulfillment of the requirements for the award of the degree of Bachelor of Chemical Engineering Faculty of Chemical & Natural Resources Engineering Universiti Malaysia Pahang MAY 2009

Transcript of FABRICATION AND CHARACTERIZATION OF COMPOSITE...

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FABRICATION AND CHARACTERIZATION OF COMPOSITE BIODEGRADABLE FILMS FROM CHITOSAN AND CORN SILK

MOHD FAIZAN JAMALUDDIN

A thesis submitted in fulfillment of the requirements for the award of the degree of

Bachelor of Chemical Engineering

Faculty of Chemical & Natural Resources Engineering Universiti Malaysia Pahang

MAY 2009

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“I declare that this thesis entitled Fabrication and Characterization of Composite

Biodegradable Film from Chitosan and Corn Silk is the result of my own research

except as cited in the references. The thesis has not been accepted for any degree and

is not concurrently submitted in candidature of any other degree”

Signature : …………………………………

Name of author : MOHD FAIZAN BIN JAMALUDDIN

Date : …………………………………

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ABSTRACT

Composite biodegradable film made from chitosan has been most potential

type of packaging especially in food packaging. Corn silk and starch, were used to

enhance the physical and chemical properties of the composite biodegradable film.

Corn silk is good to increase physical properties because it consist of zein a corn

protein. It also contain some of chemical compound that is good to fight the

mycotoxins. The film preparation process consist of hydrolyzation of corn silk fibers

which was done at a temperature range of 80°C before to be mixed with chitosan

based solution. The solution was then casted and characterized in terms of

morphology changes and physical and chemical properties. Based on the study, the

fibers from corn silk do gives an extra physical properties for the chitosan-base

composite film. The melting point has change to a more better value in order to

sustain more heat during packaging before it gradually melts compared to chitosan

alone. After the fiber being added with starch, the composite film able to give higher

melting point Futhermore,the mechanical and thermal strength increase but only by

small value. This is due to the effect of miscibility of solution before casting it to be

a film. Results obtain from FTIR, TGA, DSC and AFM proved that by using corn

silk as an additive, the composite film is experimentally enhanced in terms of

physical properties. From the study, it can be concluded that the fibers from corn silk

fiber has a great potential for being fiber to support the matrix base composite film

but there must be further research on how to mix the fiber well with the starch.

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ABSTRAK

Bio komposit filem yang mempunyai asas matriks dari bahan chitosan

merupakan bahan untuk membungkus. Chitosan, bahan yang berjaya menarik

perhatian ramai saintis dan pengkaji dengan kelebihan yang ada di mana chitosan

merupakan bahan yang mempunyai sifat sifat fizikal yang sangat bagus untuk

dijadikan filem serta anti-fungi yang ada dalam sifatnya yang membolehkan ia bebas

dari bakteria yang berbahaya.Walaubagaimanapun, terdapat masalah di mana masih

tiada bahan yang sangat sesuai dijadikan sebagai agen penambah tetapi bahan

organik merupakan bahan yang paling sesuai kerana mempunyai fiber organik untuk

mengukuhkan filem walaupun terdapat sebahagian sintetik fiber. Bulu jagung dan

kanji merupakan bahan yang dalam kajian mampu menambah baikkan ciri ciri fizikal

dan kimia di dalam komposit filem tersebut. Bulu jagung mempunyai ciri ciri yang

baik dari segi fizikal di mana terdapat bahan zein protein yang merupakan protein

jagung. Ia juga mempunyai bahan kimia yang baik untuk melawan bakteria ataupun

mikotoksin Proses filem ini bermula dengan proses hidrolisis fiber bulu jagung yang

di jalankan sekitar 80oC sebelum dicampurkan dengan asas campuran cecair

chitosan. Cecair itu kemudian dituang di atas gelas kaca dan dibiarkan kering selama

satu hari. Dan dikaji dari segi permukaannya, ciri-ciri fizikal dan kimianya .Daripada

kajian yang dijalankan, fiber bulu jagung berjaya memberi kesan yang lebih baik

kepada ciri ciri fizikal komposit filem chitosan kerana ia mengubah takat lebur yang

lebih baik daripada takat lebur biasa asas chitosan sahaja. Selepas ia di tambah pula

dengan kanji, komposit memberi keputusan yang lebih baik tetapi dengan hanya

sedikit perubahan. Ia disebabkan oleh kesan kebolehan bercampur. Keputusan yang

diberikan oleh FTIR, TGA, DSC dan AFM membuktikan bulu jagung dan kanji

mampu menambah baik ciri ciri fizikal .Daripada kajian yang dijalankan, bulu

jagung dan kanji mampu menjadi fiber untuk menyokong struktur asas matrik dalam

komposit biofilem tetapi masih memerlukan kajian untuk meningkatkan kebolehan

bercampur antara bahan tersebut

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TABLE OF CONTENTS

CHAPTER TITLE PAGE

DECLARATION i

ACKNOWLEDGEMENT ii

ABSTRACT iii

ABSTRAK iv

TABLE OF CONTENTS v

LIST OF FIGURE viii

LIST OF TABLES xi

LIST OF ABBREVATIONS xii

LIST OF APPENDICES xiii

1 INTRODUCTION 1

1.1 Background of Study 1

1.2 Problem Statment 3

1.3 Significance of Study 3

1.4 Objective 5

1.5 Scope of Study 5

2 LITERATURE REVIEW 6

2.1 Biopolymer 6

2.2 Biodegradable Film 7

2.3 Biocomposite Films 8

2.4 Polysaccharides 9

2.5 Chitosan 10

2.6 Starch 12

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2.7 Corn Silk 16

2.8 Related Research of biocomposite 16

2.9 Polyethylene glycol impact in composite 17

biofilm

2.10 Biological Properties 18

2.11 Biodegradable Film Preparation 19

2.12 Characterization of Biodegradable 21

films

2.12.1 Atomic Force Microscope 21

(AFM)

2.12.2 Fourier Transform Infra 23

Red (FTIR)

2.12.3 Differential Scanning 26

Calorimeter (DSC)

2.12.4 Thermo Gravitation 27

Analysis (TGA)

2.12.5 Scanning Electron 29

Microscope (SEM)

3 METHODOLOGY 31

3.0 Materials and Equipment 31

3.1 Methodology for Fabrication 32

3.1.1 Isolation of Fiber 32

3.1.2 Film Preparation 33

3.2 Film Characterization 33

3.2.1 Atomic Force Microscope (AFM) 34

3.2.2 Fourier Transform Infrared (FTIR) 34

3.2.3 Thermo Gravimetric Analysis 34

(TGA)

3.2.4 Differential Scanning Calorimeter 35

(DSC)

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4 RESULTS AND DISCUSSIONS 36

4.0 Result and Discussion 36

4.1 Atomic Force Microscopy (AFM) 36

4.1.1 Topographic analysis for three 37

film samples

4.1.2 Surface Roughness 40

4.2 Fourier Transform Infrared (FTIR) 41

4.2.1 Infra Red spectrum of sample J 41

4.2.2 Infra Red spectrum of sample K 45

4.2.3 Infra Red spectrum of sample L 48

4.3 Thermal Gravimetric Analysis (TGA) 52

4.3.1 Thermogravimetric traces for the 52

sample J

4.3.2 Thermogravimetric traces for the 53

sample K

4.3.3 Thermogravimetric traces for the 57

sample L

4.4 Differential Scanning Calorimeter 60 4.4.1 DSC curve of sample J 60 4.4.2 DSC curve of sample K 63 4.4.3 DSC curve of sample L 65 5 CONCLUSION AND RECOMMENDATIONS 68

4.1 Conclusion 68

4.2 Recommendation 69

LIST OF REFERENCES 71

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LIST OF FIGURES

NO TITLE PAGE

2.1 Schematic presentation of bio-based polymers based on their 7

origin and method of production

2.2 Some important monosaccharides 10

2.3 Structural formula of chitin 11

2.4 Comparing the chemical structures of cellulose,chitin 11

and chitosan

2.5 Shows a chemical formula of chitosan in Haworth´s projection 12

2.6 A structural formula of amylase 13

2.7 A structural formula of amylopectin 13

2.8 A layout of an AFM operation 21

2.9 Atomic Force Microscope Machine 22

2.10 The outline of the FTIR process 23

2.11 Basic structure of polymers 24

2.12 Fourier Transform Infra Red 25

2.13 Differential Scanning Calorimeter 26

2.14 Thermo Gravitation Analysis 27

2.15 The plan for SEM structure 28

3.1 Films produced from 4g corn silk fiber and 2 g chitosan 31

3.2 Films produced from 6g corn silk and 2g chitosan 32

3.3 Films produced from mixed of 2g Starch , 2g Chitosan 32

and 1g Corn Fiber

3.4 Corn Silk at top of Corn used to act as fiber to strengthen the films 33

3.5 Product after Corn silk being dried a while after cut off 34

from corn plant

3.6 Corn Silk in Beaker before the isolation of fiber process started 34

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3.7 Corn Silk is soaked in chemical treatment of isolation 35

of fiber process

3.8 The final product after isolation of fiber process ran 35

3.9 Chitosan used in from R&M Chemicals or Sigma Aldrich 36

3.10 Polyethylene Glycol (PEG) 400 used as plasticizer additive 37

3.11 Acetic Acid used to be add into solution of films 37

3.12 Acetic Acid mix with Chitosan and pre heat 38

to let the chitosan and acid mix.

3.13 Gelatinization of Starch before mix with acetid acid 38

and chitosan mixture

3.14 Mixture of fiber, chitosan and starch being stir with 39

300 rpm for 3-5 hours

3.15 A mixture of Corn silk fiber, chitosan and starch being 39

degassed for 12 hours to 24 hours.

3.16 A mixture of chitosan ,starch and fiber corn silk being 40

cast on glass plate and to be leave alone for one to two days.

3.17 A casted film being peeled after one day 40

3.18 Fourier Transform Infra Red 42

3.19 Plate from the FTIR being drop with chemical 42

provided before start the experiment

3.20 Plate from FTIR being put back before the put the films on it 43

3.21 Films being put to plate at FTIR before being distinguish 43

3.22 The films absorbance spectrum will be interpret in 44

software on computer screen

3.23 Differential Scanning Calorimeter 45

3.24 Small amount of films being used 45

3.25 The plate and the amount of films used in plate being determine 45

3.26 The films put into the base plate. 46

3.27 The top plate put onto the films and base plate 47

3.28 The plate with films contain in it being put into puncher 48

being punch

3.29 The plate with films being weight again 48

3.30 The plate with films being put into place provided in DSC 48

3.31 Process start automatically by setting in the software 49

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provided, the DSC

4.1 Sample J in 2D projection 51

4.2 Sample J in 3D projection 51

4.3 Sample K in 2D projection 52

4.4 Sample K in 3D projection 52

4.5 Sample L in 2D projection 53

4.6 Sample L in 3D projection. 53

4.7 Infrared spectrum of sample J 57

4.8 Chitosan 58

4.9 Cellulose 58

4.10 Infrared spectrum of sample K 60

4.11 Amylose 62

4.12 Infrared spectrum of sample L 64

4.13 Decomposition trend of Sample J 67

4.14 Decomposition trend of sample K 69

4.15 Decomposition trend of sample L 72

4.16 DSC curve for sample J 75

4.17 DSC curve for sample K 77

4.18 DSC curve for sample L 80

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LIST OF TABLES

NO TITLE PAGE

3.1 The amount of substances for preparing the solution 31

4.1 The surface roughness of the three film samples that 54

were analyzed

4.2 Some characteristic infrared absorption peaks 55

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LIST OF ABBREVIATIONS

v/v - volume / volume Mt - Metric Tonne um - ultra meter g - Gram OH- - Hydroxide functional group NH- - Amide functional group PVA - Polyvinyl Alcohol CGM - Corn Gluten Meal AFM - Atomic Force Microscope FTIR - Fourier Transform Infrared TGA - Thermo Gravimetric Analysis DSC - Differential Scanning Calorimeter SEM - Scanning Electron Miscroscopy

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LIST OF APPENDICES

APPENDIX TITLE PAGE A Results 74 B Film after Fabrication Process 83 C Isolation of Fiber 85 D Fabrications of Film 88 E Characterization of Film using FTIR 93 F Characterization of Film using Differential 95

Scanning Calorimeter

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CHAPTER 1

INTRODUCTION

1.1 Background of Study

It is normally when the consumer products purchased in our everyday lives

have either come with or been dispensed in packaging films or wrappers where its

distinct role in contributing enormously to the food packaging industry alone is

ascertained by the fact that these films are utilized to fulfill at least one of the least

functions such as to provide product protection from physical damage, contamination

and deterioration.

Other trends and demands that significantly influence food safety are

documentation and traceability, legislation, and consumer demand for safer,

healthier, more convenient,better tasting, lower cost and environmentally friendly

products.

Particularly, the food packaging films help to further the extend food’s shelf-

life properties by colossally ward off oxidative and microbial spoilage. By that idea,

its fair to sum up that the purpose of food packaging is to preserve the quality and

safety of the food contained from the time of manufacture until the time it is used by

the consumer (Cutter, 2006; Marsh and Bugusu, 2007).

Starkly notable to the food packaging industry are the emphasis and pressure

being tossed upon effective food packaging technology. The use of protective films

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or coatings and suitable packaging by the food industry has nevertheless switched

mainstream and become an ongoing topic of monumental interest because of their

packaging potentiality attributed to the ability in increasing the shelf life of many

food products (Sorrentino et al., 2007).

Furthermore, food packaging technologies putting antimicrobial packaging

films at the forefront play a pivotal role since many food products are, most of the

time, subjected to microbial attacks and contamination (Appendini and Hotchkiss,

2002) by undesirable microbes such as fungi, yeast and bacteria during the courses of

production, packaging and distribution. Thus, it is essentially important to note that

many novel packaging technologies are continually being developed to prolong the

shelf-life and improve the safety or sensory properties of fresh foods.

By means of the correct selection of materials and packaging technologies, it

is tantamount to the possibilities of being able to keep the product quality and

freshness during the time required for its commercialization and most importantly,

consumption (Stewart et al., 2002).

In the mean time, the researches still keep going to find a new material to

replace the non- biodegradeable material. Packaging technologies such as modified

atmosphere packaging and antimicrobial active packaging based on volatile

(essential oils and alcohols) or non-volatile components (chitosan and nisin) have

been developed as a result of these demands (Betty- Cory , 2006)

Even though most of the packaging films used today to preserve foods are of

synthetic origin, it is worth to say that in recent years, bio-based materials such as

carbohydrates and proteins have, gradually if not extensively, been tested and

experimented to develop biodegradable films which had been proven to have more

and more versatile properties (Perez-Mateos et al., 2007). This has undoubtedly set

off and given rise to the diverse utilization of packaging films made of bio-based

materials.

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1.2 Problem Statement

Since the last 20 years, petrochemical polymers, commonly called “plastics,”

have been booming and are by far the most widely used polymers for packaging

because of their high performance and low cost (Callegarin et al., 1997). Until as

recent as today, the largest part of all materials used in the packaging industries is

produced from fossil fuels and practically non-biodegradable (Sorrentino et al.,

2007).

For this, the packaging materials for foodstuff, like any other short-term

storage packaging material, represent a serious global environmental problem

(Kirwan and Strawbridge, 2003). Normally these packaging stuff littered on the

main road and being washed away by the rain through the drainage system and end

up in the river.

A big effort to extend the shelf life and enhance food quality while reducing

packaging waste has encouraged the exploration of new bio-based packaging

materials, such as edible and biodegradable films from renewable resources

(Tharanathan, 2003).

The goal of food packaging is to contain food in a cost-effective way that

satisfies industry requirements and consumer desires, maintains food safety, and

minimizes environmental impact (Marsh and Bugusu, 2007).

1.3 Significance of Study

Vast of interest in the search for biologically compound from natural sources

has taken part in development of biodegradable compound in recent years. Some of

the research able to contribute toward the formulation based on natural products is

inarguably their low or absent toxicity, their complete biodegradability, the

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availability from renewable sources, and in most cases and situations, the undoubted

leverage displayed by their low-cost if compared with those compounds obtained by

total chemical synthesis (Tringali, 2001)

Chitosan is a linear β-1,4-D-glucosamine is a biocompatible, non toxic

compound mainly obtained by deacetylation of chitin, a natural structural component

present for instance in crustaceans.

Chitosan inherent biocide properties which is excellent in against wide range

of microorganisms such as filamentous fungi, yeast and bacteria (Coma, Deshcamps,

& Martial- Gros, 2003; Moller, Grelier, Pardon, & Coma, 2004). This biopolymer

also presents interesting properties by excellent film forming capacity and gas and

aroma barrier properties at dry conditions, which makes it a suitable material for

designing food packaging structure (Caner, 2005).

Unfortunately, the hygroscopic properties of the bio-packaging containing

polysaccharides are responsible for their weak moisture barrier and thus have little or

no influence on the dehydration/rehydration phenomena of the foodstuffs, a property

crucial for maintaining organoleptic and microbiological food qualities (F. Se´bastien

et al, 2006).

Therefore, the biopolymer need to associate with the polysaccharide with a

more moisture- resistant polymer, while maintaining the overall biodegradability of

the product. The association with polylactic acid being considered in the form of

(blending) films (F. Se´bastien et al, 2006).

In 1996, the outbreak of food-borne illness by Escherichia coli O157:H7 in

Japan was intensely influenced to strengthen the inspection of the imported meats in

Korea, and also to make every efforts to seek promptly out an infected person who

suffering from diarrhea. The chemical components of corn silk, which has been used

as a diuretic in Chinese medicine, were analyzed and the antibacterial activity against

Escherichia coli O157:H7 (H. J. Chung et al, 2003)

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Throughout the years, many research have been done to improve the

performance of biodegradable film in the food packaging area. From all the points

above, an attempt is done to investigate the effect of different chitosan concentration

in a composite biodegradable film.

1.4 Objectives

The objectives of this study are: a) To fabricate composite of chitosan and corn silk.

b) To characterize composite of chitosan and corn silk.

1.5 Scope of study

The scope of this study are:

a) The fabrication of biodegradable film using chitosan and corn silk.

b) The characterization of biodegradable film using Atomic Force Microscope

(AFM) , Fourier Transform Infrared (FTIR) Spectroscopy, Differential

Scanning Calorimetry (DSC) and Thermogravimetric Analysis (TGA).

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CHAPTER 2

LITERATURE REVIEW

2.1 Biopolymers

Bio-based polymers may be divided into three main categories based on their

origin and production. It depend on the sources of biopolymer. Some of biopolymer

being extracted or removed from biomas. Examples are polysaccharides such as

starch and cellulose and proteins like casein and gluten. The extraction process

involved is the process to isolate the biopolymer from certain structure such as from

corn silk, husk, empty fruit bunch, wheat straw, or fat from meat and protein from

bone. Hydrolysis is one of the extraction process involved by remove water and

certain chemical compound in the sources. (Tharanathan, 2003)

Secondly is the polymer produced by classical chemical synthesis using

renewable bio based monomer The polymer is the chain of monomer. So , the bio-

based monomer will bind to one another to form biopolymer. The good example of it

is polylactic acid, a bio-polyester polymerized from lactic acid monomers. The

monomers themselves may be produced via fermentation of carbohydrate feedstock.

(Petersen et al., 1999)

Finally, the polymer produced by microorganisms or genetically modified by

bacteria such as polyhydroxylalkonoates. The developments with bacterial cellulose

however are in progress because of this polymer is still in research. (Petersen et al.,

1999)

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The most common bio-based polymers, materials and packaging are

presented in the following (Petersen et al., 1999)

Figure 2.1: Schematic presentation of bio-based polymers based on their origin and

method of production. Source: Adapted from Petersen et al., 1999.

2.2 Biodegradable films Biodegradable film is the biopolymer films. It is environmentally friendly and

could be degraded by microorganisms without further assistance. The films may

contain of polysaccharides, proteins, lipids and etc. The films easy to degrade due to

it’s the polymer that built in it is made of organic materials. The biodegradable may

consist of one or two organic materials. If the films consist of two organic materials

that can be easily biodegrade, it called as biocomposite degradable films.

(Tharanathan, 2003)

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The barrier properties of the biodegradable films are important parameters

when considering a suitable barrier in foods and food packaging. Protein and

polysaccharide films are generally good barriers against oxygen at low and

intermediate relative humidity (RH) and, while having relatively good mechanical

properties, most of them have poor moisture barrier properties (Lai and Padua.,

1998).

Films based on biopolymers are generally sensitive to the relative humidity of

the air since they are normally hygroscopic and have limited mechanical resistance

compared with synthetic films. Nevertheless protein-based films display high

deformability. A possible solution to improve the mechanical characteristics of

protein-based films could be the mixing of these biopolymers with synthetic

polymers (Tharanathan, 2003)

2.3 Biocomposite Films Composites are engineered materials made from two or more constituents

with significantly different physical or chemical properties from their components,

which remain separate and distinct within the finished structure. There are two types

of constituent materials, which are known as matrix and reinforcement components.

The matrix in the material surrounds and supports the reinforcement component by

maintaining their relative positions. (Tharanathan, 2003)

Most of the literature published on composites deals with synthetic polymers.

The sources are plant cell walls or some types of living organisms if it is not in

conflict with ethical principles. Polysaccharides are environmentally friendly and

could be degraded by microorganisms without further assistance. It is believed that

their use could be profitable especially when they are by-products of other processes.

As there are other natural polymers or related carbohydrate groups like proteins,

lignin or cyclodextrins, which are used as constituents of polysaccharide-containing

composites, their environmental impact is also covered. (Tharanathan, 2003)

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There were many research been run such as by combining the

polysaccharides from rice starch and chitosan or by combining the protein from

whey protein and zein corn protein. Films based on biopolymers are generally

sensitive to the relative humidity of the air since they are normally hygroscopic and

have limited mechanical resistance compared with synthetic films. Nevertheless

protein-based films display high deformability. A possible solution to improve the

mechanical characteristics of protein-based films could be the mixing of these

biopolymers with synthetic polymers (Tharanathan, 2003),

2.4 Polysaccharides

Carbohydrates (Polysaccharides) are naturally occurring compounds of

carbon, hydrogen and oxygen. Many carbohydrates have the empirical formula

CH2O. One distinct example is the molecular formula for glucose which is C6H12O.

All carbohydrates vary dramatically in their properties such as the case of sucrose,

also known as table sugar, and cotton that are both carbohydrates but displaying

distinguishable characteristics. The monosaccharide, often called simple sugars, are

the simplest carbohydrate units as they cannot be further hydrolyzed to smaller

carbohydrate molecules (Fessenden et al., 1998).

The monomer of polysaccharides which monosaccharide has many structure

or isomer. D-glucose, D-fructose, D-galactose, D-ribose and 2-deoxy-D-ribose is five

from many isomer of monosaccharide.

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Figure 2.2: Some important monosaccharides (Fessenden et al., 1998).

Monosaccharides also known to be able to bond together to form dimers,

trimers, etc. and ultimately, polymers. Polysaccharides that are composed of two to

eight units of monosaccharide are referred to as oligosaccharides (Greek oligo-, “a

few”). If more than eight units of monosaccharide result from the hydrolysis process,

the carbohydrate is a polysaccharide. Common examples of carbohydrates are starch

found in rice, flour and corn-starch, cellulose, a fibrous constituent of plants and the

principal component of cotton and chitin which can be found mostly in arthropods

like crabs and insects (Fessenden et al., 1998).

2.5 Chitosan

The principal structural polysaccharide of the arthropods like crabs, shrimps

and insects is chitin. It occurs as an important constituent of the exoskeleton of

many organisms, particularly crustaceans, insects and molluscs and in the walls of

most fungi and some algae (Poirier and Charlet, 2002).

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It has been estimated that 109 tons of chitin are biosynthesized each year.

Chitin is a linear polysaccharide consisting of β-linked N-acetyl-D-glucosamine.

Upon hydrolysis, chitin yields 2-amino-2-deoxy-D-glucose in which the acetyl group

is lost in the hydrolysis step. In nature, chitins are bonded to non-polysaccharide

materials such as proteins and lipids (Fessenden et al., 1998).

Figure 2.3: Structural formula of chitin. Source: Fessenden et al., 1998

Chitin is chemically identical to cellulose, except that the secondary hydroxyl

group on the alpha carbon atom of the cellulose molecule is substituted with

acetoamide groups (Figure 4).

Figure 2.4: Comparing the chemical structures of cellulose, chitin and chitosan. Source: Fessenden et al., 1998

Also, according to research, chitin, a homopolymer of b-(1 → 4)-linked N-

acetyl-D-glucosamine, is one of the most abundant, easily obtained, and renewable

natural polymers, second only to cellulose (Tolaimate et al., 2000). A sharp

nomenclature with respect to the degree of N-deacetylation has not been defined

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between chitin and chitosan. In general, chitin with a degree of deacetylation of

above 70% is considered as chitosan.

Figure 2.5: A chemical formula of chitosan in Haworth´s projection

Chitosan is produced by thermochemical alkaline deacetylation of chitin. It

is a biopolymer with unique properties favorable for a broad variety of industrial and

biomedical applications. Chitosan is characterized by its degree of N-acetylation

(DA) and this degree influences not only its physicochemical characteristics but also

its biodegradability and immunological activity. (Tolaimate et al., 2000).

It is worth noting that chitosan derived from b-chitin shows higher reactivity

than that derived from a-chitin in N-phthaloylation (Tolaimate et al., 2000).

Chitosan possesses repeating units of 1,4 linked 2-deoxy-2-aminoglucose.

The amino group NH2 can be protonated to NH3+ and readily form electrostatic

interactions with anionic groups in an acid environment. This property has been

applied on edible films (Xu et al., 2005).

2.6 Starch

Starch is the second most abundant polysaccharide. It is also worth noted that

it can be found as a reserve polysaccharide present in the endosperm of the grain of

corn (Zea mays L.), banana pulp (Musa paradisiaca), yucca (Manihot esculenta) and

among others (Romero-Bastida et al., 2005).

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Most importantly, starch is the main source of carbohydrate in the human diet

and contributes as a valuable ingredient to the food industry where it is being widely

used as a thickener, gelling agent, bulking agent and water retention agent. In most

cases, natural starch is partially crystalline in its native granule form (Iida et al.,

2008).

Starch can be separated into two principal fractions based upon solubility

when triturated, meaning literally pulverized, with hot water. About 20% of starch is

amylose which is soluble and the remaining 80% is amylopectin which is widely

insoluble (Fessenden et al., 1998).

Figure 2.6: A structural formula of amylose (Fessenden et al., 1998)

Figure 2.7: A structural formula of amylopectin (Fessenden et al., 1998

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The amylose fraction is essentially linear, whereas amylopectin is highly

branched. The two starch components have different properties and are not suitable

for the same applications (Stawski, 2008; Paes et al., 2008) and amylose is the

constituent responsible for the film-forming capacity of starches (Romero et al.,

2005).

The amount of both starch components has been influential on many various

properties of these materials such as swelling capacity, water solubility, water-

binding capacity (Sandhu et al., 2005), barrier and mechanical properties of starch

films (Rindlav et al., 1998) and microscopic properties.

There are 250 or more glucose units per amylose molecule and the exact

number depends upon the species of animal or plant. In the measurement of chain

length, it is complicated by the fact that natural amylose degrades into smaller chains

upon separation and purification. Amylose molecules form helices or coils around I2

molecules. (Fessenden et al., 1998).

Many starch-based ingredients that have been developed are principally used

to take up water and to produce viscous fluids and/or gels to impart the desired

textural quality to food products. In addition, water immobilization in foods prevents

growth of micro-organisms, thereby contributing to a longer shelf life (Ritota et al.,

2008). Gelatinization is the process where change the linear amylase to become

enriched with amylopectin.

Very often, the functional properties of starch are acquired by gelatinization,

which comprises of heating a suspension of granules above a characteristic

temperature, causing the starch granule to swell irreversibly (Marques et al., 2006).

During the swelling, the linear amylose molecules diffuse out of the swollen granules

and are preferentially solubilized. The final state can be viewed as a continuous

phase of amylose in which more or less overlapped swollen granules, enriched with

amylopectin, are suspended.

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All of the current understandings of gelatinization are based on heating starch

granules by using conduction heating modes. Under these conditions, gelatinization

is understood as the cumulative irreversible changes that occur to a starch granule in

the presence of moisture and heat (Palav and Seetharaman, 2006). These changes

again as discussed above, include granule swelling due to absorption of moisture in

the amorphous regions of the granule, leaching of small molecular weight polymers

including amylose, loss of the crystalline order and the consequent loss of

birefringence, leaching of larger molecular weight polymers from the granule

including fragments of amylopectin and, finally, starch solubilization (Sakonidou et

al., 2003).

On heating starch in excess water conditions, the granules are also found to

swell in which the starch polymers are partially solubilized and leached from the

granules, and finally the starch granules disintegrate (Bilbao et al., 2008). Starch

gives two distinct endotherms during gelatinization at low water contents. According

to (Donovan et al., 2004) that these endotherms were due to phase transitions, which

were governed by the degree to which ordered regions within granules were

hydrated. The high temperature transition is due to melting of crystallites without

adequate moisture.

When excess water is present, the high temperature transition disappears.

Further reports by Donovan suggest that, at high water contents, the amorphous

regions of the granules imbibed water and swelled, resulting in stripping or

separation of starch chains from portions of these crystallites. When all crystals are

stripped at high moisture levels, there would not be any crystallites remaining to be

melted at high temperature (Ratnayake and Jackson, 2007)

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2.7 Corn Silk

Corn is one of the most widely planted crops in the world. It is estimated that

the total yield of corn in 2001 was 6.1 × 108 Mt. Only in China, the yield of corn may

have reached 1.2 × 108 Mt.(Chao et. al, 2003).

Cornsilk has detoxifying, relaxing and diuretic activity. Cornsilk is used to

treat infections of the urinary and genital system, such as cystitis, prostatitis and

urethritis. Cornsilk helps to reduce frequent urination caused by irritation of the

bladder and is used to treat bed wetting problems. In China, cornsilk is traditionally

used to treat oedema and jaundice. Studies indicate that cornsilk can reduces blood

clotting time and reduce high blood pressure.(Chung et al, 2003)

There was much kind of protein and minerals in corn silk. The research is still

going on, but it is believe that corn silk maybe also contain corn protein which is

zein. Zein normally produced commercially from corn gluten meal (CGM). CGM is

a co-product material that is obtained during starch production. It is low priced and is

used mainly as animal feed (Ghanbarzadeh, Oromiehi and Musavi., 2006). Zein

forms films with high tensile strength and low water vapor permeabilities compared

to other protein-based films. It also has a desirable heat seal property. Furthermore,

corn zein can be used as a binder to fatty acids as both are alcohol soluble. Zein is

insoluble in water. The insolubility of zein in water is due to the low content of polar

amino acids and a high content of nonpolar amino acids 2.8 Related Research Biocomposite Films

Numerous investigations have been reported on the studies of films made

from chitosan (Park et al., 2002, and Wiles et al., 2000) and chitosan blends with

natural polymers (Lazaridou and Biliaderis, 2002 and Xu et al., 2005)

Chitosan provides unique functional, nutritional, and biomedical properties,

and its present and potential uses range from dietary fiber to a functional ingredient

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and processing aid. Some of the well known applications of chitosan include its use

for prevention of water pollution, medicine against hypertension, antimicrobial and

hypocholesterolemic activity, flavor encapsulation, seed coating, film-forming, and

controlled release of food ingredients and drugs (Struszczyk and Pospieszny, 1997).

Rice starch and its major components, amylose and amylopectin, are

biopolymers, which are attractive raw materials for use as barriers in packaging

materials. They have been used to produce biodegradable films to partially or

entirely replace plastic polymers because of its low cost and renewability, as well as

possessing good mechanical properties (Xu, Kim, Hanna, and Nag, 2005). However,

wide application of starch film is limited by its mechanical properties and efficient

barrier against low polarity compounds (Azeredo et al., 2000 and Kester and

Fennema, 1986). This constraint has led to the development of the improved

properties of rice-based films by modifying its starch properties and/or incorporating

other materials. (Films based on biopolymers are generally sensitive to the relative

humidity of the air since they are normally hygroscopic and have limited mechanical

resistance compared with synthetic films.

Nevertheless protein-based films display high deformability. A possible

solution to improve the mechanical characteristics of protein-based films could be

the mixing of these biopolymers with synthetic polymers (Tharanathan, 2003), such

as poly(vinyl alcohol) (PVA), which is also hydrophilic and biodegradable. Some

studies on the development and characterization of films based on PVA and protein

blends have been published, such as PVA/wheat (Dicharry et al., 2006),

PVA/collagen hydrolysate (Alexy et al., 2003), and PVA/gelatin (Bergo et al., 2006)

have demonstrated the presumed biodegradability of these blended films.

2.9 Polyethylene glycol impact in composite biofilms

The composite biofilms of chitosan-polylactic acid incorporated with

Polyethylene glycol will make the product more flexible and ‘easy to recover’

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materials. The chitosan-polylactic acid films will have variable thickness depend on

their blending mixture and the concentration of polyethylene glycol. The higher the

polyethylene glycol, the easier the films of chitosan were removed from

polypropylene support and more flexible there were (F. Se’bastian et al., 2006).

The higher concentration of polyethylene glycol in the composite films, the

more higher the water vapor transmission rate will be, it is due to progressive film

plasticization which is associated with modification of the hydrophilic character of

polylactic acid film. The polyethylene glycol, thus decrease the material cohesion by

creating intermolecular spaces and increasing water molecule diffusion coefficient or

the easier separation of polyethylene glycol with the amorphous phase of polylactic

acid which significantly explain the result (Renouf-Glauser et al., 2005).

The content of polyethylene glycol will also reduce the rigidity and the

brittleness of materials, thus improving their mechanical properties and their

recovery. It is due to hydrolytic reactions by water absortion(Renoulf-Glauser et al.,

2005).

2.10 Biological Properties

Mycotoxins can be characterized as secondary metabolites of various

toxigenic fungi. Mycotoxins occur in a range of human and animal disease (Coker,

1997). Exposure to mycotoxins can produce both acute and chronic toxicities

ranging from death to deleterious effects upon.

The development of active materials based on antifungal coatings and films

could be one solution to limiting the growth of these phytopathogens. Chitosan used

as polymeric matrix to produce films from renewable resources which exhibit

potential antifungal properties on mycotoxinogen strains because of its good film

forming properties and its recognized antimicrobial activity (Coma et al., 2002)

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The used of chitosan as antifungal activities being prove by coating delayed

Alternaria sp, Penicilliium sp and Cladosporium sp growth. This behavior is similar

to the action of synthetic preservatives such as calcium propionate and potassium

sorbate (Agullo et al., 2003).

The polycationic property allows chitosan to interact with negatively charged

substance, thereby exhibiting antimicrobial activity on molds. Thus, it show that the

limitation of the development of mycotoxinogen fungi (Agullo et al., 2003).

Three mechanisms have been proposed for chitosan’s antifungal properties.

The biopolymer appears work both by iinterfering directly with fungal growth and

also on plants, by activating many defense rensponses. The chelating properties of

chitosan make it an antifungal agent. Moreover, a strong inhibiton of Aspergillus

niger spore germination on a solid medium supplemented with chitosan and observe

that chitosan produced spore aggregation and morphological anomalies. In previous

study, the analysis through epifluorescence show that chitosan may acts on nucleic

acids (Sebti et al., 2005).

2.11 Biodegradable Film Preparation

A composite film formulation can be tailored made to suit to the needs of a

specific commodity or farm produce. For example, oranges having a thick peel are

prone to anaerobic conditions, which lead to an early senescence and spoilage if the

composite film is rich in lipids. Phase separation encountered during the preparation

of composites is overcome by using emulsifying agents. Use of plasticizers such as

glycerin, enthylene glycol, sorbitol, etc. in the film formulations or composites is

advantageous to impart pliability and flexibility, which improves handling (Garcia et

al., 2000). Use of plasticizers reduces the brittleness of the film by interfering with

the hydrogen bonding between the lipid and hydrocolloid molecules.

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The use of wax coating of fruits by dipping is one of the age-old methods that

were in vogue in the early 12th century (Krochta et al., 1994). This was practiced in

China, essentially to retard water transpiration losses in lemon and oranges. Later fat

coating of food products, specifically called ‘‘larding’’ was in vogue in England.

Sausage casing used very commonly nowadays is nothing but a material derived

from a protein source (gelatin). Usually a film thickness of ~2.5 mm is employed,

and coating is done by several methods. Films are reformed thin membranous

structures, which are used after being formed separately, whereas in coatings the thin

film is formed directly on the commodity.

The coating can also be done by a foam application method. Emulsions are

usually applied by this method. In here extensive tumbling action is necessary to

break the foam for uniform distribution of the coating solution, over the commodity

surface. Coating by spraying is the conventional method generally used in most of

the cases. Due to high pressure (60–80 psi) less coating solution is required to give a

better coverage. Programmable spray systems are available for automation during

such operations.

Biodegradable packaging films are generally prepared by wet casting of the

aqueous solution on a suitable base material and later drying. Choice of the base

material is important to obtain films, which can be easily removed without any

tearing and wrinkling. Infrared drying chambers are advantageous in that they hasten

the drying process (Tharanathan, Srinivasa, and Ramesh, 2002). Optimum moisture

content (~5–8%) is desirable in the dried film for its easy peel off from one edge of

the base material.

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2.12 Characterization of Biodegradable Film

There are several methods for characterize the biodegradable films which are

using Atomic Force Microscopy (AFM), Fourier Transform Infrared (FTIR),

Differential Scanning Calorimeter (DSC), Thermo Gravitation Analyzer (TGA) and

last but not least Scanning electron microscope (SEM).

2.12.1 Atomic Force Microscopy (AFM)

The atomic force microscope (AFM) is one of the most powerful tools for

determining the surface topography of native biomolecules at subnanometer

resolution. Unlike X-ray crystallography and electron microscopy (EM), the AFM

allows biomolecules to be imaged not only under physiological conditions, but also

while biological processes are at work. Because of the high signal-to-noise (S/N)

ratio, the detailed topological information is not restricted to crystalline specimens.

Hence single biomolecules without inherent symmetry can be directly monitored in

their native environment.

The AFM can also provide insight into the binding properties of biological

systems. In order to determine the specific interaction between two kinds of

molecules in an AFM, one kind is bound to the tip of a cantilever and the other kind

covers the surface of the sample support. The adhesion force upon separation is then

a measure of the binding strength. This method allowed the intermolecular forces

between individual ligand-receptor pairs, complementary DNA strands, cell adhesion

proteoglycans, and the specific antigen-antibody interaction to be determined.

The AFM works in the same way as our fingers which touch and probe the

environment when we cannot see it. By using a finger to "visualize" an object, our

brain is able to deduce its topography while touching it. The resolution we can get by

this method is determined by the radius of the fingertip. To achieve atomic scale

resolution, a sharp stylus (radius ~1-2 nm) attached to a cantilever is used in the

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AFM to scan an object point by point and contouring it while a constant small force

is applied to the stylus. With the AFM the role of the brain is taken over by a

computer, while scanning the stylus is accomplished by a

simple technique provides a

understand how the system of biological systems might function.

Atomic Force Microscopy (AFM) is

surface of biodegradable film (Bining

smaller than 100 A is scanning across a surface with a constant force. London

der Walls interactions will occur between the atoms

these forces are detected. This will result in a line scan or profile of the surfaces

(Mulder, 1996). It has emerged as the technique of choice for conducting single

molecule force spectroscopy, owing largely to the limite

applied by competing methodologies such as the use of optical tweezers or magnetic

beads (Strick et al., 2003). The level of information obtained from AFM images,

however, depends critically on the size, shape, and terminal f

probe tips used for imaging and whether the sample consists of isolated molecules or

packed molecular arrays (Engel

Figure

AFM to scan an object point by point and contouring it while a constant small force

is applied to the stylus. With the AFM the role of the brain is taken over by a

r, while scanning the stylus is accomplished by a piezoelectric tube

provides a peep into the microscopic world, and it enables us to

understand how the system of biological systems might function.

Atomic Force Microscopy (AFM) is rather new method to characterize the

surface of biodegradable film (Bining et al., 1986). A sharp tip with a diameter

smaller than 100 A is scanning across a surface with a constant force. London

der Walls interactions will occur between the atoms in the tip and the surface and

these forces are detected. This will result in a line scan or profile of the surfaces

(Mulder, 1996). It has emerged as the technique of choice for conducting single

molecule force spectroscopy, owing largely to the limited range of forces that can be

applied by competing methodologies such as the use of optical tweezers or magnetic

2003). The level of information obtained from AFM images,

however, depends critically on the size, shape, and terminal functionality of the

probe tips used for imaging and whether the sample consists of isolated molecules or

packed molecular arrays (Engel et al., 1997)

Figure 2.8: A layout of an AFM operation

22

AFM to scan an object point by point and contouring it while a constant small force

is applied to the stylus. With the AFM the role of the brain is taken over by a

piezoelectric tube. This

, and it enables us to

rather new method to characterize the

1986). A sharp tip with a diameter

smaller than 100 A is scanning across a surface with a constant force. London –van

in the tip and the surface and

these forces are detected. This will result in a line scan or profile of the surfaces

(Mulder, 1996). It has emerged as the technique of choice for conducting single

d range of forces that can be

applied by competing methodologies such as the use of optical tweezers or magnetic

2003). The level of information obtained from AFM images,

unctionality of the

probe tips used for imaging and whether the sample consists of isolated molecules or

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Figure 2.9: Atomic Force Microscope Machine 2.12.2 Fourier Transform Infrared (FTIR)

Fourier Transform Infrared Spectroscopy (FTIR) is most useful for

identifying chemicals that are either organic or inorganic. It can be utilized to

quantitate some components of an unknown mixture. It can be applied to the analysis

of solids, liquids, and gasses. The term Fourier Transform Infrared Spectroscopy

(FTIR) refers to a fairly recent development in the manner in which the data is

collected and converted from an interference pattern to a spectrum. Today's FTIR

instruments are computerized which makes them faster and more sensitive than the

older dispersive instruments. (Kim et al., 2004).

FTIR can be used to identify chemicals from spills, paints, polymers,

coatings, drugs, and contaminants. FTIR is perhaps the most powerful tool for

identifying types of chemical bonds (functional groups). The wavelength of light

absorbed is characteristic of the chemical bond as can be seen in this annotated

spectrum. (Kim et al., 2004).

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Figure

By interpreting the infrared absorption spectrum, the chemical bonds in a

molecule can be determined. FTIR spectra of pure

unique that they are like a molecular "fingerprint". While organic compounds have

very rich, detailed spectra, inorganic compounds are usually much simpler. For most

common materials, the spectrum of an unknown can be identified

library of known compounds. WCAS has several infrared spectral libraries including

on-line computer libraries. To identify less common materials, IR will need to be

combined with nuclear magnetic resonance, mass spectrometry, emission

spectroscopy, X-ray diffraction, and/or other techniques.

Because the strength of the absorption is proportional to the concentration,

FTIR can be used for some quantitative analyses. Usually these are rather simple

types of tests in the concentration range of a few ppm up to the percent level. For

example, EPA test methods 418.1 and 413.2 measure the C

petroleum or total hydrocarbons. The amount of silica trapped on an industrial

hygiene filter is determined by FTIR using NIOSH method 7602.

The Fourier-transform infra

that can detect much higher absorbances than the UV

long-winded explanation of why, which might also help you understand the lecture

portion of the class. The FTIR acquires an ab

Figure 2.10: The outline of the FTIR process

By interpreting the infrared absorption spectrum, the chemical bonds in a

molecule can be determined. FTIR spectra of pure compounds are generally so

unique that they are like a molecular "fingerprint". While organic compounds have

very rich, detailed spectra, inorganic compounds are usually much simpler. For most

common materials, the spectrum of an unknown can be identified by comparison to a

library of known compounds. WCAS has several infrared spectral libraries including

line computer libraries. To identify less common materials, IR will need to be

combined with nuclear magnetic resonance, mass spectrometry, emission

ray diffraction, and/or other techniques. (Skoog et al., 2003)

Because the strength of the absorption is proportional to the concentration,

FTIR can be used for some quantitative analyses. Usually these are rather simple

types of tests in the concentration range of a few ppm up to the percent level. For

est methods 418.1 and 413.2 measure the C-H absorption for either

petroleum or total hydrocarbons. The amount of silica trapped on an industrial

hygiene filter is determined by FTIR using NIOSH method 7602.(Skoog et al

transform infrared spectrometer gives an absorbance spectrum

that can detect much higher absorbances than the UV-visible spectrometer. Here is a

winded explanation of why, which might also help you understand the lecture

portion of the class. The FTIR acquires an absorbance spectrum without using a

24

By interpreting the infrared absorption spectrum, the chemical bonds in a

compounds are generally so

unique that they are like a molecular "fingerprint". While organic compounds have

very rich, detailed spectra, inorganic compounds are usually much simpler. For most

by comparison to a

library of known compounds. WCAS has several infrared spectral libraries including

line computer libraries. To identify less common materials, IR will need to be

combined with nuclear magnetic resonance, mass spectrometry, emission

., 2003)

Because the strength of the absorption is proportional to the concentration,

FTIR can be used for some quantitative analyses. Usually these are rather simple

types of tests in the concentration range of a few ppm up to the percent level. For

H absorption for either

petroleum or total hydrocarbons. The amount of silica trapped on an industrial

Skoog et al., 2003)

red spectrometer gives an absorbance spectrum

visible spectrometer. Here is a

winded explanation of why, which might also help you understand the lecture

sorbance spectrum without using a