MAPUA INSTITUTE OF TECHNOLOGY AT LAGUNA

Academic Year 2020 - 2021

Synthesis of Polymeric Films from the Potato Peel Starch with Eggshell Powder as
Mechanical Property Enhancer

Trisha A. BARCIA
Kyle Terrenze L. JAVIER
Crishen F. VINZON

Thesis Adviser: Engr. Jesuniño R. Aquino

A Thesis Proposal Submitted

In Partial Fulfilment of the Requirements for the Degree of

Bachelor of Science in Chemical Engineering

 COPYRIGHT

“The advisor and the authors authorize consultation and partial reproduction of

this thesis paper for personal use. Any other reproduction is subject to copyright

projection. When used as a reference, citations must be clearly mentioned.”

Malayan Colleges Laguna, 2020

The Adviser:

Engr. Jesuniño R. Aquino

The Authors:

Trisha A. Barcia
Kyle Terrenze L. Javier
Crishen F. Vinzon

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 BIOGRAPHICAL SKETCH

JUAN REYES DELA CRUZ was born on July 11, 1999 in Calamba City. He

finished his Secondary Education at Malayan High School of science and is an achiever

from Grades 4 to 6. At the moment, he is an incoming 5th year Chemical Engineering

student at Malayan Colleges Laguna. Also, he is an active member of Association of

Chemical Engineering Students at Malayan Colleges Laguna (ACES-MCL) and

Philippine Institute of Chemical Engineers Junior Chapter Luzon (PIChE-JCL).

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 ACKNOWLEDGEMENTS

The group wants to acknowledge the presence of Engr. ----, the adviser, for the

advises and guidance on what to do and what not to do in experiments and paper works.

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ABSTRACT

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 TABLE OF CONTENTS

Copyright i

Biographical Sketch ii

Acknowledgement iii

Abstract iv

Table of Contents v

Introduction

Background of the Study 2

Statement of the Problem 4

Rationale 4

Objectives 5

Theoretical Framework 5

Assumptions, Limitations, and Delimitations 6

Definition of Terms 6

Review of Related Literature 8

Methodology 19

Results and Discussion 78

Summary and Conclusion 59

Recommendations 60

Literature Cited 75

Appendix 80

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 INTRODUCTION

Background of the Study

As the world need plastics for our daily purposes, about 359 million metric tons

of plastics were produced worldwide in 2018, of which 62 million metric tons were

produced in Europe alone. While in the Philippines, Filipinos use more than 163 million

plastic sachet packets, 48 million shopping bags and 45 million thin film bags daily.

These numbers were revealed in a new report released by environmental organization

Global Alliance for Incinerator Alternatives (GAIA) on March 2019. Polymer film is

selected as the best packaging materials due to its versatility, low cost, and permeability.

However, these synthetic materials are unable to be degraded by present natural

microorganisms upon their disposal to the environment. As a result, these non-

biodegradable plastics remain in the environment for a long time and cause an increase in

solid waste production.

Bioplastics are biodegradable plastics which are made from biomass. In early age,

the first plastics were made by using plant through the internal chemical synthesis. One

of the first synthetic plastics was made from cellulose which is a substance come from

plants and trees. Plastics are the most widely used polymer in daily life, since plastic

offers a lot of benefits, in a variety of shapes, for example, film, panels, sheets, or can be

flexible for any applications which requires packaging. Starch, which is a natural

renewable polysaccharide, is considered to be a promising raw material for the

production of bioplastics. To produce bioplastic from starch, glycerol should be added in

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the heating process. The elasticity characteristic of bioplastic can be fabricated by adding

glycerol as plasticizer. Hence, the flexibility of the plastic is provided.

Calcium carbonate (calcite) is the main component in eggshells and is the major

inorganic substance found in an egg and it makes up about 94% of chemical composition

of eggshell. CaCO3 is a common filler for commodity polymers such as low-density

polyethylene (LDPE), high-density polyethylene (HDPE), polypropylene (PP) polyvinyl

chloride (PVC), and polyethylene terephthalate (PET). Eggshells have a greater surface

volume than commercially available CaCO3, resulting in better dispersion in a polymer

matrix. Incorporation of eggshell powder also reduces water absorption and increases the

thermal stability of thermoplastic starch.

Several authors (Shi et al., 2007; Wang et al., 2007a, 2009) have reported that

citric acid could form ester bond with starch. The esterification could take place between

the carboxyl groups on citric acid and the hydroxyl groups on starch. Even if no ester

bond was formed between citric acid and starch, it has been reported that citric acid could

form strong hydrogen bond interactions with starch, stronger than glycerol. The

combination of acetic acid and glycerol produces cellulose acetate which is a chemical

that increases the comprehensive strength of the bioplastic. The addition of eggshell

powder will be able to increase the tensile strength of the bioplastic which will endure

more load or force and it will reduce water absorption. Potato is ranked among one of the

chief crops producing worldwide. As per the statistics of the Food and Agriculture

Organization (FAO), the annual production of potato was over 300 million tons in 2016.

Potato peels consists high sources of starch, which is about 25%. Therefore, potato peels

can be suggested as a suitable source for the manufacturing of bioplastics

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Statement of the Problem

This research will determine if potato peel starch with eggshell powder as a

mechanical property enhancer is effective as polymeric film.

a) Does potato peel starch become an effective alternative component in making

polymeric films?

b) Does polymeric film become more effective when combined with eggshell

powder?

c) What must be the scale of added eggshell powder to obtain the highest durability?

d) What is the significant effect of our study to the environment?

Rationale

The findings of this study benefit major stakeholders of plastic industry,

government agencies that focus in the environment, and community in general.

 Government

Because of the high demand of plastic industry, the result of this study could be a

significant element of the government’s intervention.

 Community

The study will benefit the people because it is environmental friendly.

Biodegradable plastic have many advantages over standard plastic with a lesser impact

to the environment is one of the greatest advantage. This study would also benefit

researchers as a reference for future studies that might be parallel to the study.

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Objectives

The objective of this study is to show that bioplastic film from combination of

starch, eggshell and a thermoset polymer has a potential to become an alternative

resource in plastic making industries, to reduce the utilization of harmful plastics such as

HDPE (High-Density Polyethylene) and PET (Polyethylene) films. To prove that plastic

can be made by using natural base, such as potato starch and eggshell to make a product

that would be safe to the environment.

Conceptual framework

Input Thruput Output

Potato peels Synthesis of Polymeric

starch and polymeric film Films from
eggshell the synthesis
powder of potato peel
starch with
eggshell
powder as
mechanical
enhancer

Figure 1: This shows the conceptual framework

Potato peels starch and eggshell powder were the experimental unit of the study.

The starch underwent the process of polymerization using glycerol and citric acid in

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order to create polymeric film. The polymeric film from the starch based will add

eggshell powder as mechanical enhancer.

Assumptions, Limitations, and Delimitations

This study focused the effectiveness of potato peel starch with eggshell powder as

a mechanical enhancer in making polymeric film. This study is only limited in testing the

durability capability of polymeric film. The set up are: tensile strength, percent

elongation and modulus of elasticity and Fourier-transform infrared.

Definition of Terms

Bioplastics- biodegradable plastics which are made from bio-mass. Based on the

definition, biodegradable plastic is capable to break down or decomposed through

actions by bacteria or others living organisms.

Starch- a white, granular, organic chemical that is produced by all green plants. Starch is

a soft, white, tasteless powder that is insoluble in cold water, alcohol, or other solvents.

Starch is a polysaccharide comprising glucose monomers joined in α 1,4 linkages. The

simplest form of starch is the linear polymer amylose; amylopectin is the branched

form.

Polymeric Film-Polymers that are stretched into a less than 1 mm-thick film by the use

of solution casting.

Polymerization-any process in which small molecules known as monomers combine

chemically to produce a very large chainlike or network molecule.

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Esterification-induces a hydrophobic polymer, mainly the reaction between alcohols and

carboxylic acids to make esters.

Citric acid-belongs to the class of organic compounds known as tricarboxylic acids and

derivatives. These are carboxylic acids containing exactly three carboxyl groups. Citric

acid exists as a solid, soluble (in water), and a weakly acidic compound (based on its

pKa).

Glycerol-also known as glycerin or glycyl alcohol, belongs to the class of organic

compounds known as sugar alcohols. These are hydrogenated forms of carbohydrate in

which the carbonyl group (aldehyde or ketone, reducing sugar) has been reduced to a

primary or secondary hydroxyl group. Glycerol exists as a liquid, very soluble (in

water), and a very weakly acidic compound (based on its pKa).

Thermoset-a material, especially a synthetic plastic or resin, that hardens permanently

after one application of heat and pressure.

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 REVIEW OF RELATED LITERATURE

We illustrate a novel way of enhancing thermoplastic films from feathers by

alkaline hydrolysis and crosslinking with citric acid. Unlike prior process in which toxic

chemicals is involved, complex and costly method to develop films. In this study,

hydrolyzation of feather was done using different concentration of alkali, once the feather

is already hydrolyzed, compression was used, molded into films using glycerol as

plasticizer and crosslinked with citric acid to develop water stability. Alkali hydrolyzed

feathers could be compression shaped into films with tensile strength of 5.9 MPa and

elongation of 31.7% but had weak wet strength. After feather films was crosslinked with

citric acid, values are obtained in such that tensile strength had 1.9 MPa and elongation of

24.6% after being in 90% humidity at 21 °C for 24 hours. Alkaline hydrolysis and citric

acid crosslinking give an opportunity to improve inexpensive and biodegradable

thermoplastics from the inexpensive, renewable and sustainable poultry feathers (Ready,

Chen, & Yang, 2013).

This analysis introduces scientific findings regarding the recycling of bioplastics,

their blends and thermoplastic biocomposites, with special focus on mechanical recycling

of bio-based materials. The study does not incorporate bio-based commodity plastics

such as bio-derived polyolefins that are alike to their petroleum-based counterparts and

that can also be recycled. Recycling of biopolymers and their blends has been measured

using both mechanical and chemical techniques, whereas in biocomposites, the focus has

been on mechanical recycling on these later years. This investigation goes through the

discovery on the recyclability of various materials, the advantages and disadvantages of

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applied methods, as well as the possible approach and opportunities for future

improvements (Sorouidi, & Jakubowicz, 2013). There are still many blends that have not

been scrutinized for their recyclability. Details on commercially available blends which

includes bioplastics outlined in the appendix because of the essence of their possible

effects on the typical plastic recycling streams.

Pectin, an authentic and renewable polysaccharide (used in the food industry as

stabilizer, thickening and encapsulating agent), is considered a polymer with an

exceptional capacity for future improvement. However, because of the weak mechanical

and barrier properties of neat pectin-based films, the approach in food packaging is

extremely limited. In this research, we discuss, for the first time, the rewarding creation,

by thermo-compression molding, of pectin films with natural deep eutectic solvent

(NADES - ChCl:Gly (1:2)) or its individual components (glycerol (Gly) and choline

chloride (ChCl)), as plasticizers. Scrutinization was done on the effect of thermo-

compression molding parameters and the impact of plasticizers on mechanical, optical,

water resistance and morphological properties of the films. The variation of plasticizer,

its quantity and the duration of compression affects the pectin thermoplastic formulations

significantly. Films were yellow in color, visually homogenous, semi-transparent, which

do not have pores or cracks. A reduction in the compression time seemed to lower the

roughness of the films. The pectin/glycerol films showed higher tensile strength values

than films containing NADES or ChCl plasticizers. An escalation of water resistance

values in pectin/Gly films was evident upon use of NADES and ChCl plasticizers

(Gouveia, Biernacki, Castro, Goncalves, & Souza,2019).

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 In this research, the effects of eggshell powder and citric acid on the properties of

thermoplastic starch (TPS) were analyzed. Using an internal mixer, all parts were

dissolved. Citric acid led to the formation of crosslinking structures (as shown in the

FTIR spectra at 1730 cm−1) and resulted to a prompt sample biodegradation with

accelerated hydrolysis. On the contrary, the biodegradation was slowed down due to the

addition of eggshell powder. After keeping the samples for 30 days, CaTPS (Cassava root

TPS) without eggshell powder showed erosion over almost the whole surface, while the

surface of CaTPS containing 20 phr of eggshell powder (CaTPSES20) are still unloaded.

The residual TGA weight at 400 °C and the change in carbonate FTIR intensity peak of

CaTPSES20 after the storage duration given that both quantitative and qualitative

evidence that eggshell powder can be considered a potential hydrolytic retardant for

citric-acid-filled TPS(Prapruddivongs, & Wongpreedee, 2020).

This analysis illustrates the development of a model for Nd:YAG laser ablation of

cyclic olefin polymer (COP) films. Two Taguchi orthogonal array experimental designs

were conducted to fabricate a model for the prediction of microchannel depth and width

produced on ZeonorFilm® ZF14 and ZF16 polymer films via laser ablation. The width

and depth of the created microchannels were measured using 3D optical profilometry.

Microchannels produced were identified to range in depth of up to 50 µm, and widths of

112 µm via single-pass laser depending on the grade of COP, with feature size expanding

as the number of laser passes increased. The models are considered in terms of adjusted

coefficient of determination, signal to noise ratio and model significance. The effect of

the process parameters used such as fluence and scan speed on three different grades of

COP was scrutinized with an aim to make a simple model suitable for predictive control

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of surface microstructuring of COP(McCann, Bagga, Duaux, Stalcup, Vasquez, &

Brabazon, 2018).

Finite element (FE) modelling of a vertebral body (VB) is considered difficult due

to the many parameters intricated such as the size of element, type, and its material

properties. Recent researches have revealed how these parameters affect the mechanical

behaviour of a VB model; but most studies just compared results without any specific

statistical tool to quantify their impact. The Taguchi Method (TM) has been successfully

used in manufacturing and biomechanics to investigate process parameters and to identify

optimum set-up conditions. This study wants to know the ompact of the main finite

element modelling parameters on the mechanical behaviour of a VB model using the

Taguchi Method. A FE model was improved based on a C2 juvenile porcine vertebral

body and three of the most commonly used modelling parameters were assessed using

TM in terms of the change in the predicted stiffness in comparison to experimental

values: element size, number of different material properties for VB (based on grey-scale

bins) and calibration factor for grey-scale to density to Young's Modulus equation.

Evaluation was made on the impact of the combined factors. The three factors are

independent based on the Taguchi analysis. The calibration factor is the main contributor,

accounting for 97% of the predicted stiffness, with the value of 0.03 most closely

aligning the numerical and experimental results (Hernandez, Gill, & Gheduzzi, 2020).

Element size accounted for 2% of the predicted stiffness, with 0.75 mm being the ideal,

while the number of grey-scale bins influenced the outcomes by less than 1%. Our

discovery says that the calibration factor is the main modelling parameter, with the

element size and number of bins accounting for less than 3% of the anticipated stiffness.

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Therefore, basis of calibration of material properties should be on many samples to

guarantee valid results.

In this paper, it is ventured to give a discernment into the injection processability

of three self-prepared polymers from A to Z. This report depicts material analysis,

injection molding simulation, design of experiments alongside considering all interaction

effects of controlling parameters carefully for green biodegradable polymeric systems,

including polylactic acid (PLA), polylactic acid-thermoplastic polyurethane (PLA-TPU)

and polylactic acid-thermoplastic starch (PLA-TPS). Injection molding simulation

software was used to accomplish the experiments. A software was employed in order to

minimize warpage and volumetric shrinkage for each of the mentioned systems, which is

the Autodesk Moldflow®. Evaluation was done by changing five significant processing

parameters, including coolant temperature, packing time, packing pressure, mold

temperature and melt temperature. Taguchi's L27 (35) orthogonal array was chosen as an

efficient method for design of simulations for consideration of the interaction effects of

the parameters and reduce spurious simulations. On the other hand, for pattern

recognition and optimization through modifying the processing conditions, artificial

neural network (ANN) was also conducted. The Taguchi coupled analysis of variance

(ANOVA) and ANN analysis resulted in definition of optimum levels for each factor by

two completely different methods (Oliaei, Heidari, Davachi, Bahrami, Davoodi, Hejazi,

& Seyfi, 2016). There is a significant influence on the shrinkage and warpage on the

melting temperature, coolant temperature and packing time, based to the results. The

ANN optimal level selection for minimization of shrinkage and/or warpage is in good

agreement with ANOVA optimal level selection results. This study indicates that PLA-

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TPU compound exhibits the highest resistance to warpage and shrinkage defects

compared to the other studied compounds.

The extensive usage of petrochemical plastic has become an actual issue for

health and the environment. This issue can be associated to the non-biodegradable

character of an exceptional majority of these plants and to the existence of particular

chemical substances sometimes toxic within their composition. Alternative to the

petroleum plastic are represented by the improvement of biodegradable and less harmful

plastics. Two types of bioplastics were premeditated from cassava and corn starch. The

basic bioplastic was acquired from starch only while the complex bioplastic were

acquired by putting an authentic ingredient extracted from the species Cola cordifolia to

the starch. The biodegradability was evaluated by conducting burial test in soil and was

confirmed through the burial pH measurement. The burials in soil were carried out,

considered the impact of abiotic such as humidity and temperature and biotic which is

enrichment in microorganism factors. The analysis showed that the biodegradability of

bioplastic can be related to the nature of starch used. The degradation of cassava-based

bioplastic is faster that the corn-based bioplastic. The Cola cordifolia significantly

enhances the biodegradability of complex bioplastic compared to simple bioplastic. On

the other hand, the difference on environmental factors can be an advantage or

disadvantage to the biodegradability. Humidity triggers the biodegradability of

bioplastics, mainly on composite bioplastics, in a maximum rate of 15%. Enrichment in

microorganisms is disadvantageous beyond 10% enrichment for simple corn bioplastic

and beyond 20% enrichment for composite and simple cassava-based bioplastics

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(Zoungranan, Lynda, Dobi-Brice, Tchirioua, Bakary, & Yannick, 2020). The burial

temperatures above 30 °C lead to a reduction in the biodegradability of bioplastics.

The declining supply of petroleum across with the pollution caused by the

petroleum-based plastic for its non-biodegradability has resulted to expand interest in the

field of bioplastics. The primary sections of this research will begin with the plastic’s

history and then about bioplastics. A short economic study of bioplastic has also been

tackled in this report. Other topics such as applications, disadvantages and advantages

were also discussed, for the further understanding of the reader in a different scenario.

The final section of the project ventures to study a novel method in the production of

biopolymers using waste banana peels. The differences in the synthesis parameters like

pH, plasticizer choice and hydrolysis times were extensively checked, and the optimum

combination was acquired (Mohapatra, Prasad, & Sharma, 2014).

Composite bioplastic is a substitute solution to answer the plastic waste issue in

the environment. For a reason that a composite bioplastic is one material that can easily

degraded in nature and environmentally friendly. This study aims to create a complex

bioplastic composed of environmentally friendly materials, which is tapioca starch and

sugarcane bagasse fiber or SBF. The addition of SBF into the tapioca matrix serves as a

structural reinforcement of complex bioplastics. Sugarcane bagasse was added by 1 wt%

(from dry weight of starch basis) and kept with the equal measurement for each different

of the sample. The construction of composite bioplastic was obtained by casting method.

The difference in time duration of ultrasonication on complex bioplastic (tapioca starch

and 1 wt% bagasse fiber) includes 0, 5, 10 and 15 min. Tensile testing, observation of

fiber morphology, fracture surface characteristics, moisture absorption rate were

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conducted through tensile test, scanning electron microscope (SEM), and moisture

absorption test, respectively. The addition of ultrasonication increases the tensile strength

of composite bioplastic samples based on the results. It is seen that the highest tensile

strength value was achieved by a sample with 15 min ultrasonication for 2.5 MPa which

can be supported by fracture morphology which shows a compact structure (Asrofi,

Sapuan, Ilyas, & Ramesh, 2020). Furthermore, the moisture absorption rates also are

lessened with increasing ultrasonication. Preparation and giving ultrasonication on

composite bioplastic samples was highly recommended for enhancing the properties of

the sample.

As the synthetic plastics creates a negative environmental impact, the growth

of biodegradable plastics for both industrial and commercial applications become

important. Researcher have flourished different starch-based composite for various

applications. The current work scrutinizes the corn and rice starch-based bioplastics for

packaging application. A variety of samples of bioplastics are produced, with various

structure of corn and rice starch, glycerol, citric acid, and gelatin. It enhanced the tensile

property after adding rice starch, but water absorption and water solubility were reduced.

Based on these results, the finest sample was examined for thickness testing,

biodegradability properties, SEM, hydrophilicity, thermogravimetric analysis, and sealing

properties of bioplastic. The results display the suitability of rice and corn-based

thermoplastic starch for packaging applications (Marichelvam, Jawaid, & Asim, 2019).

The bioplastics fabricated are still not so developed compared to commercial

plastics, because of to the cost and weak mechanical properties. The objectives of the

study is to test a variety of physical strengthening methods and also to investigate the

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reinforcement of soy protein-based bioplastics: mold temperature increase (from 70 °C to

130 °C), as the application of a dehydrothermal (4 and 24 h at 50 °C) or ultrasound (for 5

and 45 min at 20 kHz) treatment. In this sense, the crosslinking degree, the mechanical

properties, water uptake measurements and scanning electron micrographs of the diverse

bioplastics were compared. It is concluded that suitable processing conditions and post-

treatments could favor some characteristics of bioplastics (such as maximum stress (∼5

times) or strain at break (∼3 times)), although worsening others (such as water uptake

capacity (∼50%)) based on the results ( Rosada, Bouroudian, Puyana, Guerrero, &

Romero, 2020). Specifically, a thermal treatment enhances the mechanical properties of

the structures acquired, whereas the ultrasound treatment leads to the creation of a

structure with smaller pores.

The harmful impact on environment due to landfill disposal of non-biodegradable

polymer has to be lessened and preferentially wiped out. It can be resolve by relying on

the usage of biopolymers for packaging, environment and biomedical applications. In this

study, starch and chitosan were used to prepare composites with PVA (poly vinyl

alcohol) as an additive, glycerol as a plasticizer and glutaraldehyde as a crosslinker. The

composites were developed by solution casting technique at optimum gelatinization

temperature. The effect of PVA concentration ranging from 0 to 10 wt% and glycerol

concentration ranging from 0 to 5 wt% were used to prepare composites. This study also

wants to scrutinize and create a comparison on the effect of addition of PVA on

behaviour of water absorption and its effect on the tensile properties of synthesized

composites. Using Scanning Electron Microscopy (SEM), X-Ray Diffraction (XRD) and

Fourier Transform Infrared Spectroscopy (FTIR), characterization of the prepared

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samples were carried out, The validity of the biodegradability test was evident as the

composites were found to be degraded by 40–60% after 90 days (Karua, & Sahoo, 2020).

In a wheat straw with an alkaline peroxide solution, hemicelluloses have been

extricated. Hemicelluloses which can be a component for the production of biodegradable

films that is used for food packaging was mixed with glycerol and various concentrations

of citric acid that serves as a crosslinking agent with or without sodium hypophosphite

which can be the catalyst to a crosslinking reaction. Curing treatment was done in a dried

film at 150 °C, in order to boost the formation of ester bonds between citric acid and

hemicelluloses. Water resistance and water vapor barrier properties of the films are

enhanced through crosslinking reaction which can be seen in FTIR spectra. Meanwhile,

the citric acid effects on film tensile properties were more uniform with those of a

plasticizer than of a crosslinker, which might be attributed to a flexible crosslinking

(Azeredo, Kontou-Vrettou, Moates, Wellner, Cross, Pereira, & Waldron, 2015). The

properties of crosslinked films were not affected by Sodium hypophosphite (SHP). FTIR

spectra say that some crosslinking reaction takes place even in a non-cured film.

(McCann, R., Bagga, K., Duaux, G., Stalcup, A., Vázquez, M., & Brabazon,

D., 2018). The experimental design chosen for the study of laser ablation of ZF14 was a

Taguchi orthogonal array L16 (with three factors at four levels,) and was produced and

analysed using the Design-Expert 7 (Stat-Ease Inc., USA) and Minitab 17 (Minitab Inc.,

USA) software packages. The minimum fluence level of the design was chosen to be

above the threshold fluence for ablation. Previous work by our group determined a

threshold fluence for ZF14-188 of 0.32 J/cm2 for a single laser pass and a beam scan

speed of 1.2 mm/s. A reduced quadratic model was developed using a backwards

xxi
elimination to remove insignificant terms and increase model simplicity while

maximising the adjusted coefficient of determination.

METHODOLOGY

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General

Potato bulbs and eggs were purchased from (place) public market. Glycerol and Citric

acid were chemicals purchased from a chemical online shop in Shopee.

Powdering of eggshells and extraction of starch

Starch were prepared by extracting starch from dispersing potato peels in lukewarm water

until the starch suspended. It was then cooled and poured on a filter to separate the

soaked potato peels and the starch-water solution. The filtered slurry was left untouched

until the starch suspended at the bottom. The water was removed gradually until the wet

starch is left. Three or more washes were done for the starch to achieve a white color.

The washed starch is then left on an open container dried under the sun for a day. The

eggshells were pounded on a mortar and pestle and grinded by the use of a household

grinder until it becomes a powder.

Polymerization of glycerol and citric acid

Glycerol-citric acid solution was done from mixing pure liquid vegetable glycerin and

citric acid (varying in percent weight). Afterwards, the solution was exposed in heat by

the use of an oven or pan maintained at above 100 degrees Celsius for 30 minutes for

curing to occur. The product of heat and glycerol-citric acid solution was a glycix

thermoset polymer.

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Preparation of Polymeric films

The glycix thermoset polymer, starch and eggshell powder were mixed together over a

pan heated to over 100 degree Celsius. The mixture was stirred until the components

were completely incorporated, almost as if it was opaque in appearance. The mixture was

cooled down to 65 degree Celsius and poured onto a Teflon-coated glass plates and the

thickness was uniformly made by the use of a bar-type or automatic film applicator. As

the films were casted, it was then placed under the heat of the sun and air dried for 48

hours.

Density of Samples

The density of the sample was tested through the standards of ASTM D792-00. Water

was used as the immersion liquid. The sample was weighed in air and in distilled water.

A beaker was used as an immersion vessel to contain the water. If the specific gravity of

the plastics is less than that of water, a sinker is used.

xxiv
 Figure 2: This shows the computation of Density by ASTM D792-00 standard

Sampling Technique

Taguchi method were done to specify which sample was going to be tested to reduce cost

of failure. The parameters that were studied in order to identify which sample would be

tested were the concentration of citric acid, glycerol and eggshell powder that would

affect the density of the product upon testing its specific gravity by ASTM D792-00. The

concentration of citric acid, glycerol and eggshell powder varied from 1, 2, and 3 ratio by

weight; whichever ratio by weight was at the lowest peak at the signal to noise ratio

graph dependent on the smaller-is-better ratio will be used as the sample for the testing

methods. The Taguchi method in designing experiments was done by the use of Minitab

software version 19.1.

xxv
Figure 3: This shows the computation of Signal-to-noise ratio of the Taguchi Design and

the Format of Taguchi DOE in Minitab 19.1

Testing Methods

Fourier-transform infrared

Attenuated Total Reflection Fourier Transformation Infrared Spectroscopy (ATR-FTIR)

is used to determine the cross-linkage between the starch polymer chains and

esterification of glycerol-citric acid reaction.

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Tensile Properties

The tensile properties of the starch films were determined on an UTM by ASTM D882

standards. Testing was done on samples which were starch films with no eggshell powder

and a starch film that passed the Taguchi optimization. Both of the samples were tested

for its maximum load, Maximum stress, elongation yield point and Modulus.

RESULTS AND DISCUSSION

The quick brown fox jumped over the lazy dog.

SUMMARY AND CONCLUSION

The quick brown fox jumped over the lazy dog.

RECOMMENDATIONS

The quick brown fox jumped over the lazy dog.

xxvii
 LITERATURE CITED

The quick brown fox jumped over the lazy dog.

APPENDIX

The quick brown fox jumped over the lazy dog.

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