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DEVELOPMENT OF GINGER REINFORCED

POLYVINYL ALCOHOL BIOCOMPOSITES


Thesis submitted in partial fulfillment of requirements for the award of the degree of
Master of Technology
In
Polymer Science and Technology

Submitted by

KUDZAI HAMISH RUZVIDZO


M.Tech. IV Semester
Enrollment No: A516103516001
Academic Session: 2016-18

Under the Supervision of

Prof. A.P. Gupta (Supervisor) Dr. Joydeep Dutta (Co-Supervisor)


Head Professor
Centre for Polymer Technology Department of Applied Chemistry

Amity School of Applied Sciences (ASAS)

Amity University Haryana, Gurugram


July 2018
UNDERTAKING

I hereby declare that the matter embodied in this dissertation entitled “Development of ginger

reinforced polyvinyl alcohol biocomposites”, submitted to the Department of Polymer Science

and Technology, Amity School of Applied Sciences, Amity University Gurugram, Haryana, for

the award of the degree of Master of Technology in Polymer Science and Technology is my

original work. I have not plagiarized or submitted the same work for the award of any other degree.

In case this undertaking is found incorrect, I accept that my degree may be unconditionally

withdrawn.

4 July, 2018 (Kudzai Hamish Ruzvidzo)

Manesar, Gurugram Enrollment No. A516103516001

Department of Polymer Science and Technology

Amity University Haryana

Gurugram

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CERTIFICATE

This is to certify that the work contained in this project report entitled “Development of ginger

reinforced polyvinyl alcohol biocomposites”, submitted by Kudzai Hamish Ruzvidzo, has been

carried out under the supervision of Prof. A.P. Gupta and Prof. Joydeep Dutta. The matter

embodied in this dissertation has not been submitted elsewhere for any degree.

Prof. A.P. Gupta Prof. Joydeep Dutta


Supervisor Co –Supervisor
Head Professor
Centre for Polymer Technology Department of Applied Chemistry

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ACKNOWLEDGEMENT

I would like to thank my research supervisors, Prof. A.P Gupta, Head, Department of Polymer
Science and Technology, ASAS and Prof. Joydeep Dutta, Professor, Department of Applied
Chemistry, ASAS, for their kind assistance and dedication throughout the whole tenure of the
dissertation.

My sincere thanks also to the Amity University Haryana, for providing me an opportunity and
access to the laboratory and research facilities.

I must acknowledge as well the lab staff of Department of Chemistry supervised by Mr. Vijay
Kumar who offered unflagging support and wise advice throughout my work in laboratory.

Special mention goes to my parents, Mr. E Ruzvidzo and Mrs. B Ruzvidzo, my special friend
Miss. Rumbidzai Authentic Fungura, my colleagues Mr. Tapiwanashe Shumba and Miss. Pooja
Nehra for their support during the tenure of the dissertation.

Above all, I thank the Almighty God for guiding and protecting me throughout.

Amity University Haryana (Kudzai Hamish Ruzvidzo)


Date: 4 July 2018

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ABSTRACT
Biocomposites of polyvinyl alcohol (PVA) reinforced with different weight percentages of ginger
(Zingiber officinale) and of thickness between 0.30mm to 0.35mm were developed and their
tensile strengths, water absorption capacity, water vapour transmission rate (WVTR),
biodegradation by soil burial tests and thermal analysis by Thermogravimetric analysis (TGA)
were evaluated. The fibres were extracted from ginger using water retting for 14 days. The
biocomposites were fabricated using hand lay-up method and the different weight percentages of
ginger fibres were 1%, 3% and 5%. The fibre orientations in the biocomposites were bidirectional,
unidirectional, diagonal and random. Water absorption analysis showed a high water uptake but
lower than that of pure PVA. Water vapour transmission rate of the PVA/ginger biocomposites
were high though lesser than those of pure PVA samples. For the soil burial test, the rate of
biodegradation increased with an increase in fibre content, with the 5wt% sample having the
highest rate of biodegradation. The thermal analysis showed that the biocomposite had a higher
degradation temperature of 310oC as compared to that of the PVA sample that was 290 oC. The
results of this study showed that the ginger reinforced polyvinyl alcohol biocomposite was
completely biodegradable thus; it can find applications in packaging.

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TABLE OF CONTENTS

S. NO. CONTENTS PAGE NO.

Acknowledgement (iv)
Abstract (v)
1. Introduction 1-6

2. Literature review 7-24


3. Materials and Methods 25-38

3.1 Materials

3.2 Extraction of fibre from ginger


3.3 Biocomposite fabrication
3.4 Testing and characterization methods
3.4.1 Water absorption of biocomposites
3.4.2 WVTR of biocomposites
3.4.3 Soil burial biodegradation of samples
3.4.4 Tensile strength of biocomposites
3.4.5 Thermogravimetric analysis
4. Results and discussion 39-53
4.1. Thickness of biocomposite samples
4.2. Water absorption of biocomposites
4.3. WVTR of biocomposite samples
4.4. Biodegradation of biocomposites
4.5. Tensile curves of biocomposites
4.6. TGA of biocomposite samples
5. Conclusions 54

6. References 55-59

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LIST OF FIGURES
Figure 1.1 Classification od matrix materials of composites
Figure 2.1 Structures of Zingiberene, gingerols and shogaols
Figure 2.2 Structures of farnesene and curcumene
Figure 2.3 Ginger productivity of India in last decade
Figure 2.4 Structures of some biodegradable polymers
Figure 2.5 Polymerization of polyvinyl alcohol
Figure 2.6 Hand lay-up composite fabrication process

Figure 3.1 Image of ginger used in experiments

Figure 3.2 Flowchart of the fibre extraction process


Figure 3.3 Water retting and stripping of fibres from ginger
Figure 3.4 Images of unwashed ginger fibres plus washed and dried ginger fibres
Figure 3.5 Image of the initial stage in fabrication of the biocomposites
Figure 3.6 Arrangement of ginger fibres in PVA solution
Figure 3.7 Images of ginger reinforced PVA biocomposites samples produced
Figure 3.8 Water vapour transmission rate (WVTR) test representation
Figure 3.9 Soil burial biodegradation test site
Figure 4.1 Water absorption results
Figure 4.2 G vs t graph for rectangular biocomposite sample A
Figure 4.3 G vs t graph for rectangular biocomposite sample B
Figure 4.4 Water vapour transmission rate (WVTR) of pure PVA samples
Figure 4.5 Soil burial biodegradation test results
Figure 4.6 Tensile strength for PVA sample
Figure 4.7 Tensile strength for bidirectional oriented biocomposite samples
Figure 4.8 Tensile strength for randomly oriented biocomposite samples
Figure 4.9 Tensile strength for 1wt% biocomposite samples
Figure 4.10 TGA plot of pure PVA sample
Figure 4.11 TGA plot of biocomposite sample

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LIST OF TABLES

Table 1 Classification of plant fibres


Table 2 Summary of research on natural fibre reinforced composites
Table 3 Classification of ginger
Table 4 Production of ginger in India in last decade
Table 5 Summary of research on soil burial biodegradability of some substances
Table 6 Physical and chemical properties of polyvinyl alcohol
Table 7 Summary of biocomposite samples prepared
Table 8 Weather conditions during the soil burial test
Table 9 Thickness of PVA/ginger biocomposite samples
Table 10 Water absorption test results
Table 11 Water vapour transmission rate (WVTR) results for circular sample
Table 12 WVTR experimental data results for rectangular sample A
Table 13 WVTR experimental data results for rectangular sample B
Table 14 WVTR experimental data results for pure PVA samples
Table 15 Soil burial biodegradability test results

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LIST OF ABBREVIATIONS
ASTM American Society for Testing and Materials

CMC Ceramic Matrix Composite

FRP Fibre-Reinforced Polymer

FTIR Fourier Transform Infrared

ISO International Organization for Standardization

MMC Metal Matrix Composite

PLA Polylactic Acid

PMC Polymer Matrix Composite

PVA Polyvinyl Alcohol

PVAc Polyvinyl Acetate

TGA Thermogravimetric Analysis

TS Transverse Section

USDA United States Department of Agriculture

WSP Water Soluble Polymers

WVTR Water Vapour Transmission Rate

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CHAPTER 1: INTRODUCTION
1.1 Overview of composites
Some applications require a mix of different materials with unique and distinct properties to have
the best characteristics. Thus, nowadays it is essential to combine different materials as to produce
a final product with superior and unique properties over the individual materials1. For instance,
polymers are usually resistant to chemicals, lightweight, thermal insulators, electrical insulators,
processable in many ways etc., however their other mechanical properties, like tensile strengths,
are not that great. Plant fibres have great tensile strengths, thus a mix of a polymer with those plant
fibres will produce a product that has superior strength properties in addition to special individual
properties of these materials. Some include increased strength, toughness, stiffness, reduced
weight, increased durability, thermal insulation, resistance to corrosion, creep, fatigue, tear etc.
Compared with other manufactured materials, composites have the important characteristic that
the individual material will remain distinct2. A composite has two phases i.e. a matrix phase and a
dispersion phase3. The matrix phase is continuous material that encloses the composite. The matrix
can be a metal, polymer, ceramic or carbon4. Polymer matrix can be either a thermoset such as
epoxy or a thermoplastic such as polyphenylene sulphide. The matrix is a binder as it holds fibres
together and helps align them in the stress direction, helps transfer the load, protects the reinforcing
material from environmental damages like toxic chemicals, abrasion, oxidative attacks, moisture,
radiation, temperature etc., prevents formation of cracks in fibre and maintains geometry of
reinforcement5. The dispersion phase is responsible for the core of composites6. The connection to
the matrix is by bonding. Reinforcing materials are the solid constituent of the composite that
provide strength and stiffness. Reinforcements can be whiskers, flakes, fibres, particulates, solid
eutectics etc.7 Apart from providing strength in the composite, reinforcing materials can
additionally be used to provide resistance against heat, corrosion, electricity etc. while also
providing rigidity. Composite materials find applications in many sectors of industry like in the
automobile industries, marine applications, electronic circuit boards, aeronautical applications,
safety and security sectors, chemical plants, sporting equipment like tennis racquets, construction,
biomedical, musical instruments, aerospace etc.8
Matrices

Polymer Matrix Ceramic Matrix Metal Matrix


Carbon Matrix
Composites Composites Composites
Composites
(PMC) (CMC) (MMC)

Thermoplastics
or Thermosets

Figure 1.1: Classification of matrix materials of composites

Polymer Matrix Composites (PMC) consist of reinforcing fibres bound together by either a
thermoplastic or a thermoset resin matrix9. These type of composites have low weight, are very
strong, are very stiff, cheap, have good resistance to both corrosion and abrasion and can be easily
made. However, Polymer matrix Composites have low thermal resistances, the coefficients of
thermal expansions are usually high, most are fabricated by lay-up method that is laborious and
slow10. Thus, a need arose for newer and faster automation fabrication methods for Polymer Matrix
Composites. Ceramic Matrix Composites (CMC) consist of a ceramic material being the matrix in
a composite11. A ceramic can be referred as an inorganic non-metallic solid material that has very
strong ionic bonding, is crystalline in nature and possess high moduli, high compressive strength,
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high hardness, inert to most chemicals, their thermal conductivities are usually low etc.
However, ceramics have very low fracture toughness. Thus, Ceramic Matrix composites (CMC)
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are vital to enhance toughness of composite materials. Unlike in Polymer matrix composites
where the aim of reinforcement is for enhancing how strong the composite is, in Ceramic Polymer
Matrix (CMC) the reinforcements used such as carbon, glasses, oxides and non-oxides adds to
how strong composites become. Metal Matrix composites (MMC), a composite material, in which

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the matrix is a metal like aluminum, titanium, magnesium, iron, nickel, cobalt or silver14. MMCs
have the advantages of having low densities, excellent creep, excellent wear resistances, being
strong and able to sustain high temperatures etc.

1.2 Plant fibre reinforced polymers


Fibre reinforced polymers, or FRPs, are composite material that consist of either a thermosetting
resin or thermoplastic and a fibre. A fibre is a natural substance or even a synthetic substance
having an L/D ratio greater than 100, thus it is much longer than wide. Natural fibres are those that
originate from plants, animals or mineral sources. Plant fibres are those of cellulose that are
extracted from the parts of a plant like bast or stem, leaf, seed hair or husk15. Examples include
cotton, flax, sisal, hemp, jute, kenaf, ramie, abaca etc. Plant fibres have use in making paper, ropes
and clothes16.

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Table 1: Classification of plant fibres

Plant Fibre Source Examples


Seed Fibre Seeds of plants  Cotton
 Kapok (from seed pods of kapok tree,
Ceiba pentandra)
Leaf fibre Leaves of plants  Sisal
 Agave
 Abaca
 Cantala
 Henequen
 Phormium
 Caroa
 Istle
 Sansevieria
Bast fibres Inner bark or bast  Flax
surrounding stems  Jute
of plants  Kenaf
 Hemp
 Ramie
 Rattan
 Soya bean fibre

Fruit fibre Fruits of plants  Coir (coconut fibre)


Stalk fibre Stalks of plants  Wheat straws
 Rice straws
 Barley straws
 Tree wood
 Bamboo
 Grass

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1.3 Advantages and disadvantages of composite materials
These composite materials offer many advantages over traditional materials like metals. These
advantages make the utilization of these materials more attractive in this ever growing and
competitive industrial market. Composite materials offer the following advantages i.e. reduced
weight, increased strength, rigidity, resistance to fatigue, resistance to toxic chemical substances
like acids, alkalis etc., resilience, cost saving, increased thermal and electrical insulation, increased
safety due to having low thermal and electrical conductivities. Other advantages include varied
design options or flexibility, high strength-to-weight ratios, corrosion resistance, high-impact
strengths, dimensional stability, radar transparency, durability and water resistance. However,
composite materials also have the following drawback i.e. special equipment are required, hot
curing is usually needed, as compared to wrought metals composites are more brittle. Thus,
composites damage easily. Raw materials have high costs, complex and labour intensive
fabrication process. Hot curing or cold curing involves plenty of time. Fortunately, many of the
above disadvantages can be minimized by proper design and material selection.

1.4 Need and objectives of the Present work


As stated above, composite materials have many useful properties and applications, thus there is
an ever-increasing demand for FRPs. Also due to the non-biodegradability of most synthetic
polymers, there is need to look into alternative biodegradable polymers such as polyvinyl alcohol.
Many researchers have looked into different natural fibres like banana, hemp, jute, flax, ramie,
sisal, coconut husk etc. However, as of present, no researcher has explored use of ginger fibres as
reinforcement for FRPs. Hence, the present work is carried out with the following objectives:

 To develop an effective, environmentally friendly method of extracting fibres from ginger


 To develop ten biocomposite samples of ginger fibre as reinforcement and polyvinyl
alcohol as matrix, with different fibre orientations
 To test the tensile strength of the developed composites and to make a comparative analysis
between each samples
 To analyze the stress-strain behaviour of each sample and to study the strain behaviour of
samples
 To make a comparative analysis of characteristics of the developed samples against
unreinforced polyvinyl alcohol samples

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 Analysis of the prepared composites using TGA
 To determine the water absorption capacity, percentage biodegradability and water vapour
transmission rate (WVTR) of the biocomposite samples and analyze these properties with
respect to packaging applications.
The thesis consists of five chapters. Chapter I, “Introduction”, presents a general overview of
composites, their classifications, applications, advantages, drawbacks, plant fibre reinforced
polymers etc.

Chapter II includes a “Review of Literature” which gives information of the previous work
concerning biocomposites and ginger.

Chapter III is the “Materials and Methods” which gives the detailed experiments and tests adopted
during the research work. This includes the extraction of the fibres from ginger, production of
composite samples and ASTM standards testing methods.

Chapter IV comprises “Results and Discussions” which details results of the present research
work. Tensile strengths results, water absorption results, biodegradability test, water vapour
transmission rate, TGA and FTIR results are discussed in detail.

Chapter V highlights the “Summary and Conclusions”, which concludes the research work and
gives brief summary and major conclusions drawn from the study. The chapter also gives more
ideas on how to extend the research work in future for researchers.

Literature cited in the thesis has been listed in “Bibliography”.

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CHAPTER 2: REVIEW OF LITERATURE
2.1 Natural fibres as reinforcements in composites
Ghazali et al. used harakeke and hemp fibres as reinforcements in biocomposites. They used
chemicals such as NaOH or together with sodium sulphate to extract the fibres. Analysis using
single fibre tensile testing, X-ray diffraction (XRD), scanning electron microscopy (SEM) and
Thermogravimetric analysis (TGA) of the fibres was conducted. Chemical treatment of the fibres
caused thermally stable fibres and higher crystallinity index. Hyper-branched polymers (HBP)
were used to plasticize the fibres which in turn enhanced composite ductility and impact
strengths17.

Garkhail et al. explored the possibility of utilizing vegetable fibres as reinforcements in


composites. Flax fibres were used together with polyhydroxyalkanoates (PHA) matrices. Chemical
modification of the fibre/matrix interface/interphase was explored. They discovered that fibre
modification did not have any influence on the interfacial shear strengths18.

Techapaitoon et al. explored the fracture toughness of natural fibre composites consisting of
digylycidyl ether of bisphenol-A (DGEBA) epoxy matrix and flax fibres in one composite and
plain-woven regenerated cellulose fibres in the other. Two methods were employed to fabricate
the composites i.e. resin infusion under flexible tooling (RIFT) and resin transfer molding (RTM).
Interlaminar fracture energies of 20J/m2 were determined for flax-fibre reinforced biocomposites
developed by RIFT process. For those developed using RTM process, the fracture energy was
963J/m2.19

Asumani et al. developed composites of kenaf fibres as reinforcement and polypropylene as


matrix. They focused on improving mechanical properties of the composite such as fatigue, tensile
strengths, impact strengths etc. They employed a modified compression moulding consisting of a
film-stacking technique in the manufacture of the composites. Alkali treatments and alkali-silane
treatments were employed for fibre treatments so as to improve fibre-matrix interfacial adhesion.
Results showed that alkali treatment improved the mechanical properties of kenaf/PP composites.
However, alkali-silane treatments are ideal as additional silane treatments enhance fibre-matrix
interfacial adhesion20.

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Zhu et al. developed renewable flax composites using mimosa tannin resin and pine-oil derived
supersap epoxy resin. These composites were gauged for their usefulness in modern vehicle
applications. The flax/supersap composites were suitable for exterior structural uses and
flax/tannin composites were applicable for interior non-structural uses21.

Li et al. developed a composite consisting of flax fibre as reinforcement and polyethylene (PE) as
matrix using injection moulding and also investigated effects of material properties and processing
parameters. Treatments were done as to reduce the hydrophilicity of fibres and enhance the fibre-
matrix adhesion. The matrices used were mainly High Density Polyethylene (HDPE) and Linear
Low Density Polyethylene (LLDPE) 22.

Jabbar et al. studied developments of jute-based composites using green epoxy matrix. Composites
were developed using compression molding and hand lay-up methods. The fibres were treated with
alkalis and characterized using FTIR. Mechanical properties were also determined. Creep was
analyzed using three models23.

Wretfors et al. developed a renewable composite of wheat gluten plastic with hemp fibres as
reinforcement. Retting was used for fibre extraction. Effects of fibre on the mechanical strengths
were analyzed24.

Gupta S.K et al. investigated the mechanical behaviours of epoxy-based composites reinforced by
short bamboo fibres. They concluded that mechanical properties were greatly influenced by the
size of the fibres used. Excess fibres caused deterioration of mechanical properties due to lack of
proper bonding of the matrix and the fibre around the interface. Thus, the transfer of load to the
bonding fibres is disrupted25.

Kumar S et al. developed epoxy-based composites reinforced by banana fibres. Their main goal
was to examine the mechanical behaviour of the composites. The composites were developed
using the hand lay-up technique. They concluded that fibre loading and length had high effects on
the mechanical properties like hardness, flexural strength, tensile strength, impact strength etc26.

Nagarajan et al. developed a biocomposite from a pre-blend of (PHBV-PBAT) matrix and


switchgrass through extrusion then injection moulding. They proved that increasing fibre loading
led to deterioration of mechanical strength of the composites. The properties of the composite were

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improved by the utilization of a compatibilizer. They also developed other biocomposites of
(PHBV-PBAT) matrix and various lignocellulosic fibres27.

Table 2: Summary of research on natural fibre reinforced composites

Reference Composite Notable outcomes


Ghazali et al.17 Harakeke and hemp Chemical treatment of the fibres caused thermally
fibres reinforced stable fibres and higher crystallinity index.
biocomposites
Garkhail et al.18 Flax fibres and Fibre modification did not have any influence on
polyhydroxyalkanoates interfacial shear strengths
(PHA) matrices
Techapaitoon et al.19 Digylycidyl ether of Interlaminar fracture energies of 20J/m2 for
bisphenol-A (DGEBA) biocomposites developed by RIFT process. For those
epoxy matrix and flax developed using RTM process, the fracture energy was
fibres 963J/m2
Asumani et al.20 Kenaf fibres reinforced Alkali treatment improved the mechanical properties of
polypropylene kenaf/PP composites.
composite
Zhu et al.21 Renewable flax The flax/supersap were applicable for exterior
composites using structural uses and flax/tannin composites suitable for
mimosa tannin resin interior non-structural applications.
and pine-oil derived
supersap epoxy resin.
Li et al.22 Flax fibre reinforced Treatments were done as to minimize hydrophilicity of
polyethylene (PE) fibres and enhance the fibre-matrix adhesion.
composite
Jabbar et al.23 Jute-based composites Creep was analyzed using three models
using green epoxy
matrix
Wretfors et al.24 Renewable composite The hemp fibres were extracted by retting
of wheat gluten plastic

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reinforced with hemp
fibres
Gupta S.K et al.25 Epoxy-based Excess fibres caused deterioration of mechanical
composites reinforced properties due to lack of proper bonding of the matrix
with short bamboo and the fibre around the interface. Thus, the transfer of
fibres load to the bonding fibres is disrupted
Kumar S et al.26 Epoxy-based Fibre loading and length had high effects on the
composites reinforced mechanical properties like hardness, flexural strength,
with banana fibre tensile strength, impact strength etc.
Nagarajan et al.27 (PHBV-PBAT) matrix Increase of fibre loading led to deterioration of
and switchgrass mechanical strength of the composites. They also
developed other biocomposites of (PHBV-PBAT)
matrix and various lignocellulosic fibres

2.1.1 Zingiber officinale


Ginger, also known as Zingiber officinale, is a rhizome that belongs to the Zingiberaceae plant
family28. Ginger is a well-known spice as well as finding many important medicinal uses. Ginger
is found in many areas such as India, China, Jamaica, Nigeria, Thailand, Australia, Peru, Nepal,
Indonesia, Bangladesh and Korea Republic. Ginger has an aromatic odour as well as a pungent
taste29. Fresh ginger, dried ginger or preserved ginger are the forms ginger is usually found in30.
Ginger is said to come from the word stringa-vera, a Sanskrit term meaning, “horn-like body”.31

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Table 3: Classification of ginger

Kingdom: Plantae

Subkingdom: Tracheobionata

Common name: Ginger, Ginger root, Zingiberic rhizoma

Botanical name: Zingiber officinale

Family name: Zingiberaceae

Class: Liopsida

Clade: Angiosperms

Clade: Monocots

Genus: Zingiber

Order: Zingiberales

2.1.2 Chemical constituents of Ginger


Ginger has more than 400 discrete chemical compounds32. Ginger’s chemical composition
comprises of 33

 10% fats,
 1-4% essential oils
 5% fibers,
 60% starch,
 6% inorganic material,
 10% proteins,
 10% residual moisture,

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Sahdeo Prasad and Amit K. Tyagi et al. (2015) reported the major compounds of ginger rhizomes
as 50–70% carbohydrates, 3–8% lipid, phenolic compounds and terpenes. Terpenes include
zingiberene, β-bisabolene, α-farnesene, β-sesquiphellandrene, and α-curcumene, and phenolics
include gingerol, shogaol and paradols. Zingiberene, C15H24, which makes the bulk of ginger oil,
is a monocyclic sesquiterpene. Zingiberene gives ginger the flavoring and makes up about 30% of
the oils. Gingerols contribute about 23–25% while shogaol contributes about 18–25%. These two,
shogaol and gingerols, contribute a greater quantity compared to others. Other constituents present
include raw fibre, minerals, amino acids, ash, vitamins such as nicotinic acid and vitamin A,
protein and phytosterols.

Figure 2.1: Zingiberene, gingerols and shogaols structures (Source:


Essential Medicines and Health Products Information Portal)

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Constituents of ginger depend on where it originates as well as the physical state of the rhizome34.
Gingerols are responsible for pungency of fresh ginger. Two important groups of chemicals in
ginger are34:

(i) Volatile oils:

Volatile oils give aroma as well as taste of ginger. Sesquiterpene hydrocarbons like zingeberene,
curcumene and farnesene, as well as bisabolene and b-sesquiphellandrene, are the volatile oil
constituents of ginger. Zingeberene is about 35%, curcumene about 18% and farnesene about 10%
34
.

Figure 2.2: Structures of Farnesene and curcumene (Source: ChemSpider)

(ii) Nonvolatile pungent compounds:

Gingerols, especially [6]-gingerol, which is the major one, are the most active constituent in fresh
ginger. Other gingerols include [8]-gingerol and [10]-gingerol. Nonvolatile pungent substances
comprises of [6]-gingerol, [8]-gingerol, [10]-gingerol, shogaols, zingerone and paradols35. As the
[6]-gingerol, [8]-gingerol and [10]-gingerol are thermally unstable, they form [6]-, [8]- and [10]
under high temperatures35. Gingerols dehydrate to form shogaols, and paradols are formed by
adding hydrogen to shogaol35. Generally, gingerols are similar to paradols35.

(iii) Other constituents:

Other constituents found in ginger include carbohydrates, minerals, fats, minerals, waxes etc.
Zingibain or commonly named ginger protease is also found in ginger36. In addition, ginger has
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about 3 to 8% lipids like oleic, capric, linoleic, palmitic, triglycerides etc. as well as about 50 to
70% carbohydrates present as starch37. Volatile oils contribute about 1-2% of ginger as well as 5
to 8% resinous matter. The oils consists of more than 50 constituents and exude the aroma of
ginger38. These volatile oils of ginger comprise of the sesiquiterpenes like β besabolene and
zingiberene, monoterpenes like β-phelandrene, cineol, borneol, citral as well as zingiberol39.

2.1.3 Ginger production in India


During the last ten years, India has surpassed China to become the largest producer of ginger in
the world. Approximately 1.8million tonnes of ginger is produced in the world every year, with
India and China producing nearly 50% of total output40. Ginger is produced mostly is the following
states of India including Assam, Gujarat, Karnataka, Arunachal Pradesh, Meghalaya, Sikkim,
Orrisa, Mizoram, West Bengal, Uttarakhand and Kerala41. Many varieties of ginger are produced
in India including Varada, Rejhata, Mahima, Suruchi, Suprabha, Maran, Nadia, Himanchal,
Karakkal, Pink ginger, Ellakallan, Sabarimala, Mananthody and Bhaise. From 2008 to 2017 India
has produced the following quantities of ginger:

Table 4: Production of ginger in India in the past decade

Year Area ( hectares) Production (Tonnes) Productivity (Tonnes/ha)

2008-09 108640 380100 3.50


2009-10 107540 385330 3.58
2010-11 149100 702000 4.71
2011-12 155000 756000 4.88
2012-13 134430 669350 4.98
2013-14 138200 683160 4.94
2014-15 153100 795820 5.20
2015-16 156910 1 025 110 6.53
2016-17 164850 (Est) 1 081 430 (Est) 6.56
Sources: National Horticulture Board and Spices Board India, Min of Commerce and Industry

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Ginger productivity of India in last decade

7 6.53 6.56

6
5.2
4.88 4.98 4.94
4.71
5

4 3.5 3.58

0
2008-09 2009-10 2010-11 2011-12 2012-13 2013-14 2014-15 2015-16 2016-17

Productivity (Tonnes/ha)

Figure 2.3: Ginger Productivity of India in last decade

2.1.4 Uses and benefits of ginger


Ginger has many uses i.e. culinary use as a major spice in cooking, manufacture of confectionaries
(candies and sweets), manufacture of soft drinks and alcoholic beverages. Ginger serves as
flavoring agent in baking products like ginger bread, cakes and biscuits. Ginger serves as fragrance
for soaps and cosmetics. Ginger finds applications in medicine for uses as anti-inflammatory,
antifungal, anti-vomiting, analgesic, anti-ulcer, treatment of cold induced diseases such as asthma,
cough, rheumatism etc. Ginger also lowers cholesterol levels, is used for gastrointestinal relief and
serves as an immune booster.

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2.2 Biodegradable polymers
Polymers have extensive applications in packaging, textiles, automotive industries, construction,
medicine, electronics, plumbing, adhesives, aerospace, furniture, sporting equipment, music,
agriculture etc. Unfortunately, synthetic polymers are non-biodegradable thus; they tend to create
environmental pollution issues as they remain in landfills or oceans for long periods. This tends to
affect both humans and wildlife. A polymer is a macromolecule made up of joining many repeated
subunits called monomers42. Biodegradation is the putrefaction of substances by action of bacteria,
algae, fungi etc. ASTM as well as ISO have defined degradable plastics as “Those that undergo a
significant change in chemical structure under specific environmental conditions” 43
.
Biodegradation of polymers occurs either in oxygen (aerobic) or without (anaerobic). As reported
by Subramanian Senthilkannan Muthu in Assessing the Environmental Impact of Textiles and the
Clothing Supply Chain, the basic equations for the two processes can be simplified as:

Aerobic biodegradation of polymers

Polymer + Oxygen → Carbon dioxide + Water + Biomass + Residue(s)

Anaerobic biodegradation of polymers

Polymer → Carbon dioxide + methane + Water + Biomass + Residue(s)

Thus as shown, biodegradable polymers break down after use and produces gases such as carbon
dioxide, methane, nitrogen etc., biomass, water and inorganic salts.

Kucharczyk et al. dealt with latest advances in synthesis, modification and degradation of
biodegradable polyesters. Systems based on lactic acid – polylactides were mainly centred on. The
polyesters would have medical applications. Degradation studies of the polylactides produced
were also done under various conditions44.

Gleadall et al. explored bioresorbable polymer degradation and improvement of models to


understand the mechanisms involved in the degradation process. They focused also on the changes
that occur in Young’s modulus of degrading polymers by developing a finite element method. The
study led to an Effective Cavity Theory that predicts change in Young modulus of degrading
polymers45.

16
Soleimani et al. developed new polymeric nanomaterials that would have biomedical uses. They
focused on the design, synthesis and evaluation of new biodegradable polymers and nanoscale
assemblies for drug delivery. Firstly they developed many poly(ester amides) composed of α-
amino acids, diols, and diacids. Then a poly(ester amide) - poly(ethylene oxide) conjugate was
developed and made into micelles as to achieve controlled release of PTX via hydrolysis of ester
linkages46.

Aydin et al. developed biodegradable polymer intended for bone plate applications. Biodegradable
fibres of Poly(L-lactide) and Poly(3-hydroxybutyrate-co-3-hydroxyvalerate) with hydroxyapatite
(HAP) nanoparticles were produced using extrusion method plus spinning to provide
reinforcements of polymeric bone plates47.

Moura et al. developed biodegradable copolymers of EVA and PLA using transesterification
reactions. They synthesized a maximum of 25% of the copolymer. ISO 14851 (1991) was used for
biodegradation tests. The results showed that the procedure allowed for development of
biodegradable copolymers with identical properties to those of conventional polymers48.

Vaskova et al. developed biodegradable packaging materials consisting of polycaprolactone,


polyhydroxybutyrate and starch. The mixtures were prepared using a twin-screw extruder. SEM
micrographs were used to describe the morphology of the blends49.

Díaz et al. developed and studied properties together with uses of biodegradable polymers
developed from diols and dicarboxylic acids. The uses of these biodegradable polymers include
hydrogels, soft tissue engineering, drug delivery systems and liquid crystals. They considered
usage of aromatic units and α-amino acids as the stiffness of molecular chains as well as
intermolecular interaction could be easily changed. They showed that poly(ester amide)s from
naturally occurring amino acids offered huge potential in biomedical uses as biodegradable
materials50.

17
Figure 2.4: Structures of some biodegradable polymers (Source: Gross R.A,
Kalra B, Biodegradable Polymers for the Environment)
2.2.1 Polyvinyl alcohol
Polyvinyl alcohol (PVA), [CH2CH(OH)]n, is a colourless, water-soluble, biodegradable synthetic
resin which surprisingly when compared with most vinyl polymers, is not made via polymerization
of the corresponding monomer51. Instead, PVA involves firstly polymerization of vinyl acetate
monomers by free radicals to form polyvinyl acetate (PVAc), which is then dissolved in an alcohol
such as methanol with a catalyst like sodium hydroxide52. Then a partial hydrolysis or complete
hydrolysis will remove the acetate group (CH3COO) from the polyvinyl acetate but does not
disrupt its long chain structure, thus PVA is a hydrophilic linear polymer. The synthesis of PVA
is summarized as shown below:

18
Figure 2.5: Polymerization of polyvinyl alcohol
Polyvinyl alcohol has chemical formula (C2H3OR)n where R = H or COCH3. The physical
description of polyvinyl alcohol can be described as being odourless, tasteless, translucent white
to cream-coloured granules or powders53. 4% aqueous solutions of polyvinyl alcohol have a pH
from 5 to 8 and it is also strongly hydrophilic53. The boiling point of polyvinyl alcohol is
approximately 644 degree Fahrenheit at 760 mm Hg54. The melting point of polyvinyl alcohol is
between 212 degrees Celsius to 267 degrees Celsius55. Polyvinyl alcohol is highly soluble in water
but solubility of polyvinyl alcohol in water increases with a decrease in molecular weight56.
Polyvinyl alcohol is insoluble in animal oils, vegetable oils, acetone, aromatic hydrocarbons,
chlorinated hydrocarbons, esters, and ether but slightly soluble in ethanol57. The density of
polyvinyl alcohol is between 1.19-1.31 g/cm³.58 When polyvinyl alcohol is heated to
decomposition, acrid smoke is emitted with irritating fumes also59. The viscosity of polyvinyl
alcohol ranges from above 4.8 to 5.8 mPa.s for a 4 % solution at 20 °C60. Polyvinyl alcohol is
unique in that it is made by alcoholysis or saponification or hydrolysis of polyvinyl acetate. The
acetate groups from the polyvinyl acetate are replaced with hydroxyl groups61.

19
2.2.2 Polyvinyl alcohol as a matrix in biocomposites
Jyoti et al. developed a biocomposite of polyvinyl alcohol and date palm leaf fibre (PVA/DPL) by
melt mixing fabrication method using various proportions of the fibres. The fibres were treated
with certain chemicals as to improve the dispersion and better compatibility of them with the PVA
matrix. The acrylic acid treated DPL fibres produced better qualities compared with other methods.
Properties were analyzed like morphology, tensile strength; Young’s modulus, elongation at break,
impact strength, flexural strength etc. and the results were compared to those of virgin PVA
matrix62.

Ching et al. developed and characterized a PVA/oil palm empty fruit bunch fibre composite by
casting evaporation technique. There was intimate contact between the empty fruit bunch fibre and
the polyvinyl alcohol. They showed that addition of 1 wt% of empty fruit bunch fibre led to an
increase in the tensile strength and modulus od the PVA/empty fruit bunch composite. Stiffness of
the PVA that was reinforced with 3 wt% of empty fibre bunch increased by 300% compared to the
neat polyvinyl alcohol63.

Tian et al. developed polyvinyl alcohol/modified silicon carbide (SiC) composites. The modified
silicon carbide was used as a filler because of its relatively good abrasive nature thus; it would be
able to improve the wear resistance of PVA. The composites were fabricated using a melt process
and then subjected to tensile tests. The suitability of the composites for tribological uses was being
analyzed. The interactions between the matrix and the filler were enhanced by the utilization of
coupling agents. The surface modified SiC particles were also well dispersed within the polyvinyl
alcohol which enhanced their compatibility with the matrix64.

Pron et al. developed a polyvinyl alcohol – polypyrrole conducting composite by the exposing the
solid polyvinyl alcohol films containing FeCl3 or K3Fe(CN)6 to the vapours of the pyrrole. They
showed that the distribution of the oxidant within the polyvinyl alcohol matrix is crucial for the
morphology and electrical properties of the developed composites65.

Ahmed et al. developed polyvinyl alcohol – iodine composites by addition of different weight
percentages i.e. 2,4 and 6% of the iodine to the polyvinyl alcohol matrix. The main use of the
developed composites were to treatment of wounds infected with diseases especially diabetes.
Injured mice were used to apply the solutions and films as to evaluate the healing action. They
showed that the drug was antibacterially active and healed the wounds well66.

20
Singha et al. developed biocomposite films of starch and polyvinyl alcohol. The reinforcement
was in the form of delignified Grewia optiva fibre as well as methyl methacrylate (MMA) grafted
fibres. Citric acid was the plasticizer and the cross-linker was glutaraldehyde. Tests were done for
their mechanical properties, biodegradability and antibacterial properties. Results from SEM
revealed great adhesion between starch and polyvinyl alcohol blend matrix and fibres. Results also
revealed the biocomposite films were suitable for food packaging applications67.

Polyvinyl alcohol has a variety of uses i.e. as a release agent, as a binder and thickener, to make
Vinylon, as a textile-sizing agent, for paper coatings, in packaging as water-soluble films, is useful
in PET bottles as a CO2 barrier. Polyvinyl alcohol is also used as PVA fibre that is utilized as
concrete reinforcement, as polyvinyl nitrate raw material, as surface-active agent, as protective
chemical-resistant gloves, as protective colloid in suspension polymerization. When polyvinyl
alcohol is doped with iodine, it polarizes light and polyvinyl alcohol finds application in medical
procedures.

21
Table 5: Summary of research on the soil burial biodegradability of some substances

Reference Substance Biodegradation Main results


test
Shafik et al.68 PVA /Corn Starch Soil burial All buried films lost weight loss, with
(CS) blend films degradation of loss of weight increasing with burial
2×2cm2 samples time. The weight loss decreased as the
at depth of 10cm. PVA content increased.
Harith et al.69 PVA/Corn Starch Soil burial 10%PVA/90%CS sample had greatest
Blend Films degradation of loss of weight and pure PVA had the least
2×2cm2 samples weight loss over time. This was due to
at depth of 10cm presence of corn starch in film which is
more biodegradable
Korbag et al.70 PVA/lignin blend Soil burial test PVA/lignin blend with the less content of
films
PVA in the mixture had the greatest
values of weight loss.
Yaacob et al.71 PLA/paddy straw Soil burial testing PLA/PSP biocomposites had faster
powder for 6 months degradation as compared to pure PLA
biocomposite because lignocellulosic material is easily
attacked by microorganisms. Voids left
presence of moisture also allowed
colonization by microorganisms
Anuar et al.72 PLA-Kenaf Fibre Soil burial test at Increasing the Kenaf fibre content led to
Biocomposite temperatures of an increase in biodegradation of the
26ºC. biocomposite. Highest weight loss was
for PLA-20KF suggesting that Kenaf
fibres favoured biodegradability factors
and promoted faster degradation of the
PLA biocomposite.

22
2.3 Hand Lay-Up Composite Fabrication Method
Composites are made in three processes i.e. open molding, closed molding and cast polymer
molding.73 Open molding is a simple, low cost process which the resins, and fibre reinforcements
are exposed to air. Thus, the composites cure or harden. Hand lay-up, filament winding, casting
and spray-up are all open molding techniques.74 Hand lay-up is the easiest and popular open
molding composite manufacturing process. It also requires less amount of equipment compared
with other techniques.

Figure 2.6: Hand lay-up composite fabrication process (Source: Fundamentals


of Modern Manufacturing: Materials Processes, And Systems, 2Nd Ed)

23
Mikell P. Groover et al (2002) reported that hand lay-up composite manufacturing process can be
best explained in the steps shown in Figure 6. In step (1), the mold is treated with mold releasing
substance to avoid the sticking of polymer to the surface. In step (2) a thin gel coat is then put onto
the outside covering of molding. In step (3), when partial setting of the gel coat has occurred,
quantities of both resin and the fibre are then applied. Rollers thoroughly wet the reinforcement
and eliminate air. In step (4), the part is cured. Curing time is dependent on which polymer is
utilized. For example, epoxy based systems at room temperature cure in about 24 to 48 hours. In
step (5) the part which has now completely hardened is ejected. The hand lay-up composite
manufacturing method is usually utilized for thermosets like epoxy. It is the simplest of all
composite fabrication methods. It offers cheaper tooling and many part sizes. Hand lay-up
composite fabrication method is used in areas like making of aircraft components, boat hulls, large
container tanks, swimming pools, stage props, some automotive parts etc.75. The materials used as
matrix in this method include epoxy, unsaturated polyester, polyvinyl esters phenolic resin etc.
and the reinforcements are glass fibre, carbon fibre, aramid fibre and natural plant fibres like ginger
fibres.

2.4 Water retting process of plant fibre extraction


Retting is an important method of fibre extraction from plants. The main idea behind this concept
of fibre extraction is to employ moisture and bacteria. These then rot or dissolve cellular tissues
nearby and gummy substances that surround the fibre bundles.76 Bast fibres are from the inner
bark of a plant. The rotting is orchestrated by enzyme action of microbes naturally present in retting
water. This then makes it easier to separate the fibres from the stem. Retting methods include water
retting, dew retting, tank retting, chemical retting, enzyme retting and microbial retting. Water
retting produces best quality of fibres. It involves immersing the stalks of fibre plants in slowly
running cold or warm water for four days to fifteen days. This is preferable, as it will not carry
away the bacteria. The active organism is usually Clostridium felsineum and disintegrates the
pectin into organic acids, hydrogen, carbon dioxide and alcohols. 77

24
CHAPTER 3: MATERIALS AND METHODS
3.1 Materials
Reagents of pure quality were extensively used for the experiments. Polyvinyl alcohol (Mol. Wt.
85,000 to 1,24,000) was purchased at the Central Drug House (CHD), Vardaan House, Daryaganj,
New Delhi, India. Distilled water was also used throughout for all experiments. Table 6
summarizes the properties of the polyvinyl alcohol.

Table 6: Physical and chemical properties of polyvinyl alcohol (PVA)

Appearance White crystalline powder/flakes/granules


Molecular weight 85,000 to 1,24,000
Solubility 4% solution in cold water is clear and
colourless
Viscosity of 4% aqueous solution at 20oC 23 – 38 cP
Ash Max 0.75%
Degree of hydrolysis 86.0 – 89.0%

The ginger was purchased from the local market at Amity University Haryana.

Figure 3.1: Ginger used in experiments

25
3.2 Extraction of fibre from ginger

Storage of
Washing Peeling of ginger in
of ginger ginger freezer for 3
days

Water
Washing and Stripping of retting of
drying of ginger ginger for
ginger fibres fibres 14 days

Figure 3.2: Flowchart of the fibre extraction process


The ginger, purchased from the local market at Amity University Haryana, was firstly peeled. The
peeled ginger was then put in a freezer for three days. The frozen peeled ginger was immersed into
a container filled with cold water and stored for 14 days to ret. Caution was taken to store the
container far from households as an unpleasant smell was produced during the retting process. The
container was kept in an underground waterway for two weeks with an average high temperature
of 37oC and an average low temperature of 22oC, average relative humidity of 33% and an average
pressure of 1008 mbar78. Retting time is also very crucial, as under-retting leads to great difficulty
in stripping of the fibres whilst over-retting will produce very weak fibres. After retting process,
the fibres were then easily stripped from the ginger by hand.

26
Figure 3.3 - Water retting and stripping of fibres from ginger

27
Figure 3.4: Unwashed ginger fibres (left) plus washed and
dried ginger fibres (right)
3.3 Biocomposite fabrication
3.3.1 Preparation of polyvinyl alcohol solution
10% polyvinyl alcohol solution was prepared. 10grams of polyvinyl alcohol powder was slowly
added to 100mL of deionized water in a volumetric flask. After full dispersion of the powder, the
mixture was then heated until the polymer became solubilized. After heating, the polyvinyl alcohol
solution was left to cool.

3.3.2 Preparation of biocomposite samples


Hand lay-up method was utilized in the development of the biocomposites. Polystyrene sheets
were cut to form a 20𝑐𝑚 × 10𝑐𝑚 × 2𝑐𝑚 rectangular prism with the top open. 50mL of the 10%
polyvinyl alcohol solution was then poured in the polystyrene rectangular prism.

28
Figure 3.5: Initial stage in fabrication of biocomposites

Ginger fibres were then arranged into the polyvinyl alcohol solution.

Figure 3.6: Arrangement of ginger fibres into polyvinyl alcohol solution

29
Three different fibre content weight percentage classes of biocomposite samples were prepared.
The first class consisted of 1 wt% ginger fibre, the second 3 wt% ginger fibre and the third 5 wt%
ginger fibre.

Table 7: Summary of biocomposite samples prepared

Fibre Amount Amount of Amount of Orientations


content of distilled ginger
(wt. % of Polyvinyl water fibre
matrix) alcohol
1% 5 grams 50ml 0.05 grams  Unidirectional continuous fibres
 Random arrangement
 Diagonal continuous fibres
 Bidirectional continuous fibres
3% 5 grams 50mL 0.15 grams  Random arrangement
 Bidirectional continuous fibres
5% 5 grams 50mL 0.25 grams  Random arrangement
 Bidirectional continuous fibres
After arranging the fibres in the polyvinyl alcohol solution, the setup was left for 12 hours at room
temperature. 50mL of polyvinyl alcohol solution was then added. The biocomposite was left for 2
days at room temperature.

30
Some of the ginger reinforced polyvinyl alcohol biocomposite samples developed are shown in
the images below:

31
32
33
Figure 3.7: Images of ginger reinforced polyvinyl alcohol
biocomposite samples produced

34
3.4 Testing and characterization methods
3.4.1 Water absorption test
A modified ASTM D570 procedure was employed for the water absorption test. In this test three
dried rectangular ginger reinforced polyvinyl alcohol biocomposites of length 28mm and width
25mm were first weighed. Samples were then emerged into water in a freezer for 24 hours. A
freezer was employed in this procedure because the ginger reinforced polyvinyl alcohol
biocomposite is greatly soluble in water, thus decreasing the temperature would reduce the rate of
solubility.79 After 24 hours samples were ejected, dried with a cloth and immediately weighed.
The water absorption is percentage change (gain) or increase in weight 80.

Wet weight − Dry weight


% Water Absorption in 24 hours = × 100
Dry weight

Where wet weight refers to the weight of the biocomposite samples after being emerged in water
for 24 hours, and dry weight refers to the initial weight of the biocomposite samples.

3.4.2 Water vapour transmission rate (WVTR) test


As the ginger reinforced polyvinyl alcohol biocomposites is meant for packaging uses, it is vital
to determine the extent of its moisture transmission capacity. This is important as in packaging;
some dry materials may be damaged if moisture penetrates it. ASTM – E96 procedure D is used
for WVTR tests. The units of WVTR are gm−2 day −1 . The lower the value of WVTR means the
better the packaging material is to protect against moisture transmission.

To determine the WVTR of biocomposite samples, two modified ASTM – E96 procedure D wet
cup methods were used.

Method 1

Three circular biocomposite samples were put on top of beakers containing distilled water. The
open mouth of the beaker was then sealed but making sure that 37mm diameter of the biocomposite
sample would remain exposed such that it would become the test area.

35
Figure 3.8: Water vapour transmission rate (WVTR) test representation
The initial weight was measured and then the setup was put in an incubator at 500C for 24 hours.
Afterwards the final weight was measured.

WVTR is then determined using the formula:

Initial weight − Final weight


WVTR =
1 day × Test area of circular biocomposite specimen

Method 2
Rectangular specimen were used, the first had dimensions of 36𝑚𝑚 × 28𝑚𝑚 and the other
35𝑚𝑚 × 22𝑚𝑚. These samples were put on top of beakers containing distilled water, making
sure to leave about 1.8cm space between the distilled water and test area of specimen. The open
mouth of the beaker was then sealed but making sure that the dimensions of the rectangular
specimen used would remain exposed such that it would become the test area. A temperature of
600C and a testing time of 6 hours was used. The setup was periodically weighed at one-hour
intervals for 6 hours. The weight change, G, was measured every hour. A graph of weight
change, G, vs time t was then plotted. From the graph, the linear portion’s slope is the one useful
in WVTR calculations.

36
Slope of G vs t graph linear portion divided by the test specimen area determines the value of the
WVTR.

G
(t)
WVTR =
A

slope of G vs t graph
=
Test area of specimen

3.4.3 Soil burial biodegradation test

Figure 3.9: Soil burial biodegradation test site


The developed ginger reinforced polyvinyl alcohol biocomposites will have applications in
packaging, thus they should be able to biodegrade after use as to reduce the harmful pollution
effects on the environment. Test biocomposite samples were first weighed. The biocomposites
were then buried in soil for 15 days. They were periodically weighed after every 5 days. The
weight loss was then determined.

initial weight before burial−final weight after burial


% weight loss = × 100
initial weight before burial

37
The meteorology data for the period from 13 June 2018 to 29 June 2018 when the test was done
at Amity University Gurgaon, Haryana, India were:

Table 8: Weather conditions during the soil burial test

Temperature Humidity Pressure


High 45oC (22 Jun, 14:30) 100% (27 Jun, 23:30) 1003 mbar (27 Jun, 23:30)
Low 26oC (19 Jun, 05:00) 14% (22 Jun, 17:30) 993 mbar (25 Jun, 17:00)
Average 340C 51% 1000 mbar
* These data were taken from CustomWeather, © 2018

3.4.4. Tensile testing of biocomposites


Tensile testing was performed on the ginger reinforced polyvinyl biocomposites using a universal
testing machine according to ASTM D638. Samples measuring 70mm in length and 10mm in
width were used for testing. The samples were mounted between the grips of the testing machine.
The gauge length was 60mm and were pulled at crosshead speed of 30mm/min.

3.4.5 Thermogravimetric analysis of biocomposites


Thermogravimetric analyses of the ginger reinforced polyvinyl alcohol biocomposites was
performed using a Thermogravimetric analyzer (PerkinElmer Pyris-6). They measure the changes
in the mass of a sample as a function of the temperature. The experiments were carried out under
nitrogen atmosphere by heating the biocomposite samples in an aluminum crucible at 10 oC/min
from 40oC to 800oC.

38
CHAPTER 4: RESULTS AND DISCUSSION
4.1 Thickness of samples
The thickness of the pure PVA samples were higher than that of the biocomposite samples. The
thickness of six PVA/ginger biocomposite samples were measured and the results are shown in
Table 9

Table 9: Thickness of PVA/ginger biocomposite samples

Sample Thickness (mm)


A 0.30
B 0.33
C 0.32
D 0.35
E 0.33
F 0.33

The thickness of the biocomposite samples were between 0.30mm to 0.35mm


4.2 Water absorption test analysis
The results for the three ginger reinforced polyvinyl alcohol biocomposite samples used in this
experiment were as follows:

Table 10: Water absorption test results

Sample Initial dry weight Wet weight (grams) % Water


(grams) Absorption
A 0.586 2.007 242
B 0.560 1.943 247
C 0.558 1.929 246

39
% water absportion % Water absorption of biocomposite samples in 24 hours

242 247 246

Sample A Sample B Sample C

Figure 4.1: Water absorption results


The average value of these three samples was then taken as the percentage water absorption. The
percentage water absorption of biocomposite samples was 245%. This value of 245% water
absorption of the ginger reinforced polyvinyl alcohol biocomposites is quite high. This may be
because of hydroxyl groups (-OH) in the polyvinyl alcohol structure which aid in the absorbance
of the high quantities of water. The water absorption of pure PVA samples was 289%, hence
increasing the fibre content decreased the water absorption of the biocomposites. The percentage
water absorption was comparable with other water absorption values of other polyvinyl alcohol
composites in literature, for example, Tan et al. studied the water absorption values of kenaf fibre
– polyvinyl alcohol composite and found out values of 273% and 251% for 2 and 10wt% of
polyvinyl alcohol respectively81.

40
4.3 Water vapour transmission rate (WVTR) test analysis
The results of the WVTR test performed on the ginger reinforced polyvinyl alcohol biocomposites
are:

Method 1 results
Table 11: WVTR results for circular sample

Sample Diameter Initial weight Final weight WVTR (gm-2day-1)


(mm) (grams) (grams)
A 37 102.525 102.203 299.5
B 37 103.721 103.397 301.3
C 37 101.577 101.256 298.5

Method 2 results analysis


For rectangular sample A:
Table 12: WVTR experimental data results for rectangular sample A

Time from beginning of Measured weight (grams) Weight change


experiment (hours) (t) (grams), G
0 136.228 0
1 136.196 0.032
2 136.129 0.067
3 136.038 0.091
4 135.925 0.113
5 135.801 0.124
6 135.663 0.138

41
G vs t graph for biocomposite sample
0.16

0.14

0.12
Weight change,(G), grams

0.1

0.08

0.06

0.04

0.02

0
0 1 2 3 4 5 6 7
Time (t), hours

Figure 4.2: G vs t graph for rectangular biocomposite sample A


The WVTR of rectangular sample A was 297.6 gm−2 day −1
For rectangular sample B:
Table 13: WVTR experimental data results for rectangular sample B

Time from beginning of Measured weight (grams) Weight change

experiment (hours) (t) (grams), G

0 137.584 0
1 137.533 0.051
2 137.448 0.085
3 137.349 0.099
4 137.237 0.112
5 137.118 0.119
6 136.991 0.127

42
G vs t graph for biocomposite sample
0.14

0.12
Weight change,(G), grams

0.1

0.08

0.06

0.04

0.02

0
0 1 2 3 4 5 6 7
Time (t), hours

Figure 4.3: G vs t graph for rectangular biocomposite sample B


The WVTR of rectangular sample B was 290.9 gm−2 day −1
Averaging the five results, the WVTR of the ginger reinforced polyvinyl alcohol biocomposites
was 297.6 gm−2 day −1 .
WVTR for pure polyvinyl alcohol (PVA) sample:
Table 14: WVTR experimental results of pure PVA samples

Sample Specimen Time of testing Initial Final weight WVTR


diameter (mm) (hours) weight (grams) (gm-2day-1)
(grams)
A 27 24 102.276 102.027 434.9
B 27 24 101.970 101.703 466.3
C 27 24 102.171 101.908 459.3

43
WVTR of pure PVA samples

466.3 459.3
434.9
WVTR (gm-2day-1)

Sample A Sample B Sample C

Figure 4.4: WVTR of pure PVA samples

Averaging the three values, the WVTR of PVA sample was 453.5 gm−2 day −1 .
WVTR is one of the critical parameters for assessing packaging materials. Lower values of WVTR
show that the material has good resistance to water vapor transmission. The results showed that
pure polyvinyl alcohol sample had a greater WVTR value as compared to that of the ginger
reinforced polyvinyl alcohol solution. Polyvinyl alcohol is hydrophilic and as such due to hydroxyl
group, it can readily interact with water molecules thus consequently increasing the WVTR as
compared to other less hydrophilic substances. In ginger reinforced polyvinyl alcohol
biocomposite samples, the WVTR decreases because as the percentage composition of ginger
increases the hydrophilicity in turn decreases. It is impossible to compare WVTR values with
literature as they were not done under the same conditions. However, Suki et al. determined
WVTR values of 8.6g/m2h, 9.2g/m2h, 9.7g/m2h, 10.3g/m2h for PVA/BFF blends of 90/10, 80/20,
70/30, 60/40 respectively82.

44
4.4 Biodegradability test results
The results for the biodegradability tests were

Table 15: Soil burial biodegradability test results

Sample Initial Weight loss Weight loss Weight loss %


weight after 5 days after 10 after 15 biodegradability
(grams) (grams) days days
(grams) (grams)
5 wt.% 0.369 0.129 0.251 0.362 98.1%
bidirectional
3 wt.% 0.388 0.113 0.221 0.349 89.9%
bidirectional
1 wt.% 0.350 0.098 0.199 0.294 84%
bidirectional

Soil burial biodegradation test


100

90

80

70
% weight loss

60

50

40

30

20

10

0
5 days 10 days 15 days
Time (days)

5 wt% bidirectional 3 wt% bidirectional 1 wt% bidirectional

Figure 4.5: Soil burial biodegradability test results

45
From the results, the rate of biodegradability of the ginger reinforced polyvinyl alcohol
biocomposites increased with an increase in fibre content or with a decrease in ratios of PVA.
Also, in the soil sorption of water by the biocomposites would promote the entry of
microorganisms which would enhance the biodegradability process. From literature, the weight
loss of pure PVA is lesser that those of biocomposite samples since the fibres would aid in the
absorption of water which would speed up the biodegradation. From the results, the 5wt.%
bidirectional ginger reinforced polyvinyl alcohol biocomposite samples showed highest
biodegradation rate, whilst the 1wt.% bidirectional ginger reinforced polyvinyl alcohol
biocomposite samples showed the least biodegradation rates. Comparing with pure PVA, from
literature, Ooi et al. 2011, reasoned that pure PVA will have lesser biodegradation rates compared
to PVA biocomposites because the C-C backbone linkage of the PVA. Guohua et al. 2006 reported
that pure PVA samples exhibit greater resistance to soil burial biodegradation. During the period
the samples were buried, there was rainfall in Haryana, thus the excess water may have permeated
into the ginger reinforced biocomposite specimens. Table 5 in review of Literature section also
has a summary of research results on the soil burial biodegradability of some other composite
materials constituting PVA.

46
4.5 Tensile strength of biocomposites
The results from the tensile testing are shown

4.5

3.5

3
Standard force [MPa]

2.5

1.5

0.5

0
-5 0 5 10 15 20 25
Elongation [%]

Figure 4.6: Tensile curve for PVA

1wt% bidirectional sample


7

6
Standard force [MPa]

0
-10 0 10 20 30 40 50 60 70 80
Elongation [%]

47
5wt% bidirectional sample
10

7
Standard force [MPa]

0
-10 0 10 20 30 40 50 60 70 80
Elongation [%]

3wt% bidirectional sample


9
8
7
Standard force [MPa]

6
5
4
3
2
1
0
-5 0 5 10 15 20 25 30 35 40
Elongation [%]

Figure 4.7: Tensile curves for bidirectional oriented samples

48
5wt% random sample
14

12

10
Standard force [MPa]

0
-10 0 10 20 30 40 50 60 70 80
Elongation [%]

Figure 4.8: Tensile curves for randomly oriented samples

1wt% diagonal sample


12

10
Standard force [MPa]

0
-20 0 20 40 60 80 100
Elongation [%]

49
1wt% unidirectional sample
12

10
Standard force [MPa]

0
-10 0 10 20 30 40 50 60 70 80
Elongation [%]

1wt% bidirectional sample


7

5
Standard force [MPa]

0
-10 0 10 20 30 40 50 60 70 80
Elongation [%]

50
1wt% random sample
7

5
Standard force [MPa]

0
-10 0 10 20 30 40 50 60
Elongation [%]

Figure 4.9: Tensile curves for 1wt% biocomposite samples


The tensile test gives results for load versus elongation curve, which is then converted into a stress
versus strain curve. The load-elongation curve will have the same shape as the engineering stress-
strain curve .From Figure 4.9 it was shown that the 1wt% unidirectional orientation had the greatest
tensile strength compared to 1wt% diagonal orientation, 1wt% random orientation and 1wt%
bidirectional orientation. This is in agreement with Almeida et al. who opinioned that a composite
reinforced with fibres aligned in one direction have high modulus and strength in the fibre direction
and poor mechanical characteristics in the transverse direction. The 1wt% randomly oriented
sample had the least tensile strength properties. From Figure 4.8 it was shown that the tensile
strength of the bidirectional oriented samples increased from the 1wt% sample to the 5wt% sample.
This is due to the fact an increase in ginger fibre content causes an increase in the strength of the
biocomposite. This trend was also the same for the 1wt%, 3wt% and %wt% of the randomly
oriented samples from Figure 4.7.

51
4.6 Thermogravimetric analysis (TGA)

TGA plot for pure PVA


100 1
90 0.5

Derivative Weight % (%/min)


80 0
70 -0.5
Weight % (%)

60 -1
50 -1.5
40 -2
30 -2.5
20 -3
10 -3.5
0 -4
0 100 200 300 400 500 600 700 800
Temperature (degrees celcius)

Weight % Derivative Weight %

Figure 4.10: TGA plot of PVA sample

TGA plot for biocomposite sample


100 2
90
1

Derivative Weight % (%/min)


80
70 0
Weight % (%)

60
-1
50
-2
40
30 -3
20
-4
10
0 -5
0 100 200 300 400 500 600 700 800
Temperature (degrees celcius)

Weight % Derivative Weight %

Figure 4.11: TGA plot of biocomposite sample

52
Figure 4.10 shows the weight percentage vs sample temperature of the PVA sample. Figure 4.11
shows the weight percentage vs sample temperature of the ginger reinforced polyvinyl alcohol
biocomposite. The TGA curves of both pure PVA samples and PVA/ginger showed three weight
loss stages. For the pure PVA sample, the initial weight loss occurred at temperature region of 40
to 110°C due to the evaporation or loss of moisture from the polymer matrix. The loss in weight
was about 5.88wt% in this stage. The major loss of weight occurred in the 150 to 380°C. This is
because of the degradation of the side chain i.e. O-H groups of the PVA. The loss of weight in
stage was about 55wt%. The third stage ranged from temperatures above 400°C and corresponded
to the cleavage or breakdown of the C–C backbone of the polyvinyl alcohol. The weight loss in
this stage was around 30%. The degradation temperature of the PVA sample was 290oC.

The PVA/ginger biocomposites also exhibited three major stages of weight losses. The initial
weight loss occurred in the region from region 40 to 110°C and was due to the loss of moisture in
the biocomposites. The weight loss was about 4.16wtpercentage. The greatest weight loss occurred
from temperatures of 160 to 400oC and this was due to the structural degradation of the PVA
matrix in the biocomposites. The weight loss at this stage was about 52wt%. The third stage was
for temperatures above 400oC and it corresponds to the cleavage or breakdown of the backbone of
PVA as well as the degradation of fibre. The degradation temperature of the PVA/ginger
biocomposite sample was 310oC.

The degradation temperature of the PVA/ginger biocomposite sample was higher than that of PVA
sample because an increase for fibre enhances interaction between fibre and matrix, which in turn
improves the thermal resistance.

53
CHAPTER 5: CONCLUSIONS
In the study of the development of PVA/ginger biocomposites, ginger fibres were successfully
extracted using the water retting method. The extracted ginger fibres showed good tensile strength,
with the tensile increasing with increasing fibre content up to the 5wt% biocomposite samples.
The PVA/ginger composites were successfully developed using the hand lay-up method and had
different fibre weight percentage. The fibre and matrix had good compatibility and all are
hydrophilic in nature. The results of the water absorption test showed that the PVA/ginger
biocomposites had high water absorption capabilities due to the hydrophilic nature of both the
polyvinyl alcohol polymer and the natural fibres. However, an increase in the ginger fibre content
caused a decrease in the water absorption. The water vapour transmission rates also showed the
high tendency of the biocomposites for moisture transmission. However, the WVTR was lesser as
compared to that of pure PVA samples showing that incorporation of fibres reduces the moisture
transmission. Soil biodegradation tests also showed that the PVA/ginger biocomposites had a great
biodegradation rate as compared to pure PVA and an increase in fibre content corresponded to an
increase in the biodegradability of the biocomposites. This is great as the biocomposites would
have applications in packaging and as such, the high rates of biodegradation are vital as to reduce
environmental pollution as caused by most non-biodegradable synthetic polymers. The thermal
analysis of the biocomposites by TGA showed that the degradation temperature of the PVA/ginger
biocomposite was higher than that of pure PVA because the presence of the fibres enhanced
interactions between fibre and matrix that in turn improved the thermal resistance of the
biocomposite. Considering the above properties of the biocomposite samples developed, they can
find applications in packaging.

54
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