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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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
ii
“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 : …………………………………
iii
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.
iv
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
v
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
vi
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)
vii
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
viii
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
ix
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
x
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
xi
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
xii
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
xiii
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
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
2
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