UTILIZATION OF UBE PEEL WASTE STARCH

AND BROWN SEAWEED CELLULOSE AS A

BIOPLASTIC COMPOSITE

__________________

A Research Paper
presented to the Faculty of the
College of Engineering
Eastern Visayas State University
Tacloban City

__________________

In Partial Fulfillment of
the requirements for the Degree of
Bachelor of Science in Chemical Engineering

__________________

By
MARY GRACE PROGELLA
NIOX B. GONZALES
February 2019
 APPROVAL SHEET
In partial fulfillment of the requirements for the degree of Bachelor of Science in
Chemical Engineering, this research entitled: “UTILIZATION OF UBE (Dioscorea alata)
PEEL AND BROWN SEAWEED (Sargassum muticum) AS BIOPLASTIC COMPOSITE”
has been prepared and submitted by NIOX B. GONZALES and MARYGRACE S. PROGELLA
who are recommended for Oral Examination.

ENGR. EVELYN A. CARDOSO

Adviser

Approved by the Committee on Oral Examination with a rating of __________.

ENGR. EVELYN A. CARDOSO

Chairperson

ZENAIDA L. ANDRADE, Ph.D. MARIA LINA A. DOLLETE, Ph.D.

Member Member

ELVIRA DOLORES URGEL, DM. PROF. RICHARD S. BRUN

Member Member

Accepted in partial fulfillment of the requirements for the course, CHE 362 (Methods of
Research II), Bachelor of Science in Chemical Engineering.

ENGR. EVELYN A. CARDOSO

Instructor, CHE 362 (Methods of Research II)
Eastern Visayas State University, Tacloban City

Date of Oral Examination

February 22, 2019

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 ACCEPTANCE SHEET

This research hereto attached entitled: “UTILIZATION OF UBE (Dioscorea alata) PEEL
AND BROWN SEAWEED (Sargassum muticum) AS BIOPLASTIC COMPOSITE” prepared
and submitted by NIOX B. GONZALES and MARYGRACE S. PROGELLA in partial
fulfillment of the requirements for the course, CHE 362 (Methods of Research II), Bachelor of
Science in Chemical Engineering, is hereby accepted.

ZENAIDA L. ANDRADE, Ph.D. MARIA LINA A. DOLLETE, Ph.D.

Member, Oral Examination Committee Member, Oral Examination Committee

ELVIRA DOLORES URGEL, DM. PROF. RICHARD S. BRUN

Member, Oral Examination Committee Member, Oral Examination Committee

ENGR. EVELYN A. CARDOSO

Chairperson, Oral Examination Committee

Accepted in partial fulfillment for the requirements for the course, CHE 362 (Methods of
Research II), Bachelor of Science in Chemical Engineering.

ENGR. EVELYN A. CARDOSO

Instructor, CHE 362 (Methods of Research II)

MARIA LINA DOLLETE, Ph.D.

Head, Chemical Engineering Department
Eastern Visayas State University, Tacloban City

ANNABELLE B. PILAPIL, Ph.D.

Dean, College of Engineering
Eastern Visayas State University, Tacloban City

JANUARY 2019

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 ACKNOWLEDGEMENT
The researchers would like to thank to the following who are in one way or another
extended their guidance and expertise in making this whole research possible:

To the Almighty God, for all the strength, endurance, wisdom and shower of
blessings he gave in finishing this study and for pushing the researchers to the best of their
ability.

To the researcher’s parents and family who gave their love, prayers, and best in
supporting the researcher’s financial needs in completing the research.

To the Researchers ‘supportive research adviser, Engr. Evelyn Cardoso for the
continuous support, providing invaluable guidance, for sharing her wisdom and expertise
to the researchers as well as for her patience, motivation and immense knowledge
throughout this project.

To the Chemical Engineering Department for providing all the laboratory

equipment and materials needed in conducting the research experiment.

To the Department of Agriculture for all the efforts in helping the

researchers during the analysis of the soil used in biodegradability test.
This research study will not be possible without your help and for that, the
researchers are very grateful.

-NIOX BERNAL GONZALES

-MARYGRACE SANTIAGO PROGELLA

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TABLE OF CONTENTS

Title ...................................................................................................................................... i

Approval sheet .................................................................................................................... ii

Acceptance sheet ................................................................................................................ iii

Acknowledgements ............................................................................................................ iv

Table of Contents .................................................................................................................v

List of Figures ........................................................................................................................

Chapter I ..........................................................................................................................1

Background of the Study ..................................................................................................1

General Objectives ...........................................................................................................3

Null Hypothesis ................................................................................................................4

Conceptual Framework ....................................................................................................5

Significance of the Study .................................................................................................6

Scope and Delimitations...................................................................................................7

Definition of terms ...........................................................................................................8

Chapter II ......................................................................................................................10

Review of Related Literature ......................................................................................10

v|Page
 Review of Related Studies............................................................................................22

On Bioplastics ........................................................................................................22

On Starch based Bioplastics ..................................................................................23

On Bioplastic yields ...............................................................................................24

On Physical Properties of Bioplastics ....................................................................25

Chapter III ....................................................................................................................26

Research Design ..............................................................................................................27

Research Subject and Sampling Procedure.....................................................................33

Research Procedure .........................................................................................................34

Research Instrument........................................................................................................38

Statistical Analysis ..........................................................................................................39

Chapter IV.....................................................................................................................26

Appendix

Appendix A

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Bibliography

References .......................................................................................................................46

LIST OF FIGURES

Figure I-1 Conceptual Framework Flow .......................................................................................... 5

Figure II-1 Amount plastic contributed to ocean pollution, in pounds (2010) .............................. 12
Figure IV-3 .................................................................................................................................... 33

LIST OF TABLES

Table IV-1 ...................................................................................................................................... 31

Table IV-2 ...................................................................................................................................... 32
Table IV-3 ...................................................................................................................................... 33
Table IV-4 ...................................................................................................................................... 34
Table IV-5 ...................................................................................................................................... 34

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 CHAPTER I
INTRODUCTION
Background of the Study

Plastic is a type of synthetic or man-made polymer composed of various complex

organic compounds produced by polymerization, capable of being molded, extruded, cast

into various shapes and films, drawn into filaments or used as textile fiber. With the

discovery of plastics, life became much more convenient because it is used to make a wide

array of useful materials. But these plastics are so durable that it will take many centuries

to completely degrade (Gyandarshan, 2017). Plastics creates severe challenges for waste

management and has a great impact on the environment, considering that only a small

fraction of plastic waste is being recycled. Thus, producing biomaterials with potentially

better rates of decomposition is one of the possible alternatives to combat the spread of

waste plastic in the natural environment.

Bioplastics in a general sense are basically all types of plastics made materials or

products that are at least partly derived from biomass, plant matter. Examples of biomass

used in bioplastics include corn, sugarcane, tapioca, or other forms of cellulose. For this

reason, the Researchers aim to develop a biomass-based plastic from brown seaweed

(Sargassum muticum) cellulose and Ube (Dioscorea alata) peel starch which has the

capability to degrade a short period of time only.

Dioscorea alata, or more commonly known in the Philippines as Ube, has the

distinction of having of a purple or lavender color. In the Philippines, the natural sweetness

of the ube yam is often used in desserts such as cakes, pastries and ice cream. The nutrition

profile of an ube yam is generally similar to that of a regular yam. Like other yams,
Dioscorea alata contains high amounts of starch making it a viable variable for the

production of bioplastic.

Brown seaweed on the other hand, are best known for the natural polysaccharides

that can be extracted from them which are widely used particularly in the fields of food

technology, biotechnology, microbiology and even medicine. Sargassum muticum is large

brown seaweed for the genus Sargassum (Venkatesan, 2017). Marine algae are used in the

production of plastic due to its advantage as a biodegradable plastic where it can be

decomposed into smaller substance by living organisms. Seaweed, as one of the variables

of this research can serve as alternatives for the production of bioplastics because of its

high biomass, its ability to grow in a wide range of environments and its cultivation in

natural environment when compared to other microbial sources which require a specific

environment for their cultivation (www.jpronline.info).

Within this study, the production of the bioplastic utilizes the starch in the

polymerization reaction. The polymerization reaction uses a free radical, in most cases a

strong acid, in order to create polymers, this polymer in turn if need be can then be modified

by plasticizers and other additives. Bioplastics in general, behaves mostly like any other

plastic. And so, by extension it can be measured and characterized under the same

parameters and properties. Some of the properties include the production yield, those that

qualify under physical, and those that qualify under chemical properties.

2|Page
General Objectives

This study will be geared with the development of a bioplastic using the natural

polysaccharides from brown seaweed (Sargassum muticum) and Ube (Musa paradisiaca)

peel waste. Specifically, it will aim to answer the following questions:

1. Will there be significant differences in the mass of the bioplastic composite from

brown seaweed (Sargassum muticum) and Ube (Musa paradisiaca) peel waste,

from the control bioplastic, and the control bioplastic variant with brown seaweed

(Sargassum muticum) cellulose, after undergoing biodegradation?

2. Will there be significant differences in the mass of the bioplastic composite from

brown seaweed (Sargassum muticum) and Ube (Musa paradisiaca) peel waste,

from the control bioplastic, and the control bioplastic variant with brown seaweed

(Sargassum muticum) cellulose, after submersion in various chemicals.

Particularly;

a) Hydrochloric Acid

b) Sulfuric acid

c) Sodium hydroxide

3. bioplastic composite from brown seaweed (Sargassum muticum) and Ube (Musa

paradisiaca) peel waste, from the control bioplastic, and the control bioplastic variant with

brown seaweed (Sargassum muticum) cellulose, after submersion in various chemical?

3|Page
Null Hypothesis

In the production of bioplastic composites from ube peel waste starch and brown

seaweed cellulose, there will be no significant differences between it and the control

samples made up of a cornstarch-based bioplastic with a variation of adding seaweed

cellulose, in :

1. Biodegradability (Amount degraded)

2. General Chemical Resistance (Amount Corroded)

3. Tensile Strength

4|Page
Conceptual Framework

The study is based on Figure I-1, which acts as a theoretical general flow of how the study

is to be conducted. The research will proceed firstly with the production of the starch from

the raw Dioscorea alata peel and cellulose from Sargassum muticum. After which, the

bioplastic composites are produced; purely ube starch, ube starch with brown seaweed

cellulose, cornstarch, and corn starch with brown seaweed cellulose. The produced

bioplastic is to be tested for the properties indicated within the general objectives. After

obtaining the properties, the physical and chemical properties of the bioplastic composites,

all the data is then interpreted and then the results made.

Production of Ube Peel

Production of Bioplastic
starch and Brown Corn starch
Composites
Seaweed cellulose

Bioplastic Composites

Testing of Properties

Analysis and
Interpretation of data

Figure I-1
Conceptual Framework Flow

5|Page
Significance of the Study

The section will provide brief description on the various significances of the

study within the following fields as well as specific people;

To the Researchers. This study provides an opportunity to gain experience in the

field of research, as well as in bioplastics. This also gives the researcher knowledge and

knowhow in the various subtopics involved in the production and testing of bioplastics.

To those in the field of Chemical Engineering. This study will serve as viable

reference or jumping off point for others looking for topics to delve deeper into. This study

may also serve the purpose of presenting a viable alternative source of raw materials for

bioplastic production to those aiming to produce renewable plastics.

To the Ube and Seaweed farmers. This provides them with possibly a new

revenue of income; selling their Ube peels and Brown seaweed to the bioplastic industries

and thermoplastic producing companies.

To the Community. This research will also be significant to the whole scientific

community since it would provide added information about how to make a better,

environment-friendly, inexpensive and toxic-free plastic.

To the Environment. This research will be helpful to the present world where the

consequences of plastic products used and the waste management of these products when

they become waste, is a current and pressing issue because of the impact of conventional

plastics they cause to the environment. This bioplastic from seaweed and banana peels will

not fill up the landfills because they are biodegradable for a short period of time unlike

petroleum-based plastics which takes about many centuries to degrade.

6|Page
Scope and Delimitation

The study covers the production of bioplastic from Ube Dioscorea alata peel starch

and Brown seaweed Sargassum muticum cellulose, notably the traits in terms of physical

and chemical properties. This also includes harvesting and extraction of seaweed,

collecting Ube peels, making of the bioplastic, testing the biodegradability, tensile strength

and general chemical resistance, gathering and analysis of data and finally, arriving the

conclusions. Some of the materials will be borrowed from the Eastern Visayas State

University- Tacloban Campus (Research Laboratory). It will take two weeks to finish the

making of the bioplastic since there are parts where drying is needed. The study will only

measure the following chemical properties: Biodegradability, and Chemical Resistance.

Under this, the research will only study the chemical resistance of the bioplastic with a few

select liquids and biodegradability using compost ability in soil. Another couple of days

for the tensile strength test using an Instron machine. The research will not be further

extended on the massive production of the bioplastic for commercial use.

7|Page
Definition of Terms

Definition of Terms

Bioplastic. Bioplastics consist in a large part, or even completely, of renewable

resources. Thus, bioplastics are bio-based plastics. Biodegradable, but petroleum-based

plastics, are not considered as bioplastics.

Starch. An odorless tasteless white substance occurring widely in plant tissue and

a polysaccharide that functions as a carbohydrate.

Plasticizer. Organic esters added to polymers to facilitate processing and to

increase the flexibility and toughness of the final product by internal modification of the

polymer molecule.

Density. Density is the relationship between the mass of the substance and volume

the substance has. The mass of atoms, their size, and how they are arranged determine the

density of a substance.

Tensile strength. This is the capability of resisting a load for a given cross section,

typically measured in psi. the force per unit area (MPa or psi) required to break a material

in such a manner is the ultimate tensile strength or tensile strength at break.

Plasticity. This is the ability of certain solids to flow or to change shape permanently

when subjected to stresses of intermediate magnitude. Plasticity enables a solid under the

action of external forces to undergo permanent deformation without rupture.

Biodegradation. This is the breaking down of large or complex organic substances into

simpler substances through the action of enzymes from microorganisms. If this process is

8|Page
complete, the initial organic substances are entirely converted into simple inorganic

molecules such as water, carbon dioxide and methane.

General Chemical Resistance. It tells the set of chemicals a material can resist

from the deterioration of its fundamental properties and to the chemicals that deteriorates

its fundamental properties. It is one of the properties of the bioplastic which will be

determined.

Polysaccharides. A carbohydrate (e.g., starch, cellulose, or glycogen) whose

molecules consist of a number of sugar molecules bonded together.

9|Page
 CHAPTER II
Review of Related Literature

This chapter presents the various literary works and studies reviewed by the

researchers, which provide more insights and substance to this study. All information in

this chapter also provides a basis for some of the procedures and methods stated in the later

chapters.

The world that exists today is a world where plastic is one of the key materials in

keeping it running. According to Gaelle Gourmelon, “for more than 50 years, global

production of plastic has continued to rise. Some 299 million tons of plastics were produced

in 2013, representing a 4 percent increase over 2012” (Gourmelon, 2015). Plastic is not

biodegradable, but photodegradable. And in reality, most plastic does not ever disappear,

but becomes long-lasting “plastic dust”. When items like plastic bags break down, they

readily release toxins that then contaminate soil and water, as well as harming animals that

ingest plastic fragments. Even when the recycling concept was introduced to the plastic

industry. This information is compounded by the facts in figure 1 that we contribute so

largely to the plastic pollution in the ocean. Mark Contorno remarks, “And there’s no

winning: producing recycled materials uses copious amounts of energy. A better solution

would be to reduce use of plastics altogether, but they are not” (Contorno, 2013). Even

when producing plastic, pollution is already present, this is compounded by the fact that

large amounts of plastic are being produced daily. According to Mark Contorno, “the

production of plastic for the U.S. alone uses 331 billion barrels of petroleum” (Contorno,

2013). On this note taking a look at the statistics would shed some light on how bad the

plastic problem has gotten in our times; The European Commission writes, “Global plastic
production has risen from 1.5 million tonnes per year in the 1950s to 288 million tonnes a

year in 2012. This staggering increase has been driven by the low cost and range of physical

properties that plastics can provide. However, the waste generated can be devastating to

ecosystems. All five major oceanic gyres contain substantial amounts of plastic waste,

which can injure or kill wildlife and spread invasive species. Furthermore, plastic does not

biodegrade but remains in the environment for hundreds of years.” (European Commission

, 2014).

Figure II-1
Amount plastic contributed to ocean pollution, in pounds
(2010)
A viable solution for the ever-increasing amount of plastic waste in the word is

bioplastic and research. Bioplastics consist in a large part, or even completely, of renewable

resources. Mariastella Scandola writes, “This creates severe challenges for waste

management and has a great impact on the environment, since only a small fraction of

plastic waste is being recycled. If we want to control and reduce these negative impacts on

the environment it is essential that we move to the production and use of plastics with a

higher level of sustainability, in particular biodegradable and bio based plastics.”

(Scandola, 2013).

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 These bioplastics are believed to answer the problem about plastic waste disposal.

They are convenient to use since they are almost similar to those of conventional plastics.

The only difference is that most bioplastics are biodegradable. They are free from any

allergens or toxins that can harm us particularly our health.

The Fachagentur Nachwachsende Rohstoffe writes, “Starch based bioplastic or

otherwise known as thermoplastic starch (TPS) also falls under a set of bioplastics called

Polysaccharide-based plastics. “Starch consists of two component polymers, amylose

(AM) and amylopectin (AP). Amylose is the linear polysaccharide, poly(α-1,4-

glucopyronosyl). Amylopectin is poly(α-1,4-glucopyronosyl) with many a -1,6-

glucopyronosyl branches.” (Robert Shanks, 2012). Fachagentur Nachwachsende Rohstoffe

writes, “In order to destructure the starch it must be subjected to sufficient physical energy

and heat in the presence of so-called plasticizers. The best plasticizer for starch is water at

a concentration of 45 %. Other plasticizers are glycerin, sorbitol, etc.” (Fachagentur

Nachwachsende Rohstoffe , 2014).

Ube, purple yam, or Dioscorea alata is a root crop or tuber found and grown in

various places all around the world. Even in some Asian countries, some edible tubers are

also used as traditional medicinal. A variety of foods can be prepared using tubers and they

may also be used in industrial applications. Anoma Chandrasekara and Thamilini Josheph

Kumar write, “Yam is a member of the monocotyledonous family Dioscoreaceae and is a

staple food in West Africa, Southeast Asia, and the Caribbean regions. Yam is consumed

as raw yam, cooked soup, and powder or flour in food preparations. Yam tubers have

various bioactive components, namely, mucin, dioscin, dioscorin, allantoin, choline,

13 | P a g e
polyphenols, diosgenin, and vitamins such as carotenoids and tocopherols.” (Anoma

Chandrasekara, 2016).

The Ube peel starch is to be used as the major resource in producing bioplastic,

since a solid factor to consider in deciding what raw material to use can be the starch

content of biological material. Ube, like most root crops, has a high amount of starch

content per unit mass, about 25% of it is starch. Aglaee Jacob writes, “Yams have average

158 calories per cup. Most of the calories in yams and other starchy vegetables come from

their carbohydrates, more precisely in the form of starches. A 1-cup serving of Ube yams

contains 37 grams of carbohydrates, of which 5.3 grams are fiber, 0.7 gram is sugar and

the remaining 31 grams are starches. Ube yams contain very little protein, about 2 grams

per cup, and almost no fat.” (Jacob, 2011) . This coupled with its high abundance within

the Philippines makes it a very favorable variable for the production of bioplastic.

Brown Seaweed as one of the variables of this research can serve alternatives for the

production of bioplastics because of its high biomass, its ability to grow in a wide range of

environments and its cultivation in natural environment when compared to other microbial

sources which require a specific environment for their cultivation.

There are three common polysaccharides derived from marine seaweed. These are

Floridean starch, Agar, and Alginate. Floridean starch is a special type of starch that is

primarily found in red seaweed but it can also be found in green ones. It acts as the major

cellular storage units of molecules and energy in these organisms. To extract Floridean

starch, one usually boils the seaweed in water until particles settle at the bottom. The

particles will be collected and dried Invalid source specified.

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 Figure 2.1 Chemical Structure of Floridean Starch

Agar is a cell wall constituent of red algae. It I a natural polymer made from repeating

units of galactose. It is an odorless, slightly transparent and sugar reactive substance which

takes the form of a gel. Unlike gelatin which is a protein-based gel derived from animals,

agar is a polysaccharide extracted primarily from red seaweed Invalid source specified.

Figure 2.2 Chemical Structure of Agar

Alginate is a cell wall constituent of brown algae. It is a natural polymer made from

repeating units of mannuronic acid and guluronic acid. It is an odorless, slightly transparent

and viscous gum which takes the form of a liquid gel. It has a hydrophilic nature that makes

alginate capable of absorbing water much greater than its weight Invalid source specified.

Figure 2.3 Chemical Structure of Alginate

The cellulose from seaweed particularly brown seaweed are widely used in the field

of food technology, biotechnology, microbiology, and medicine. Their water absorbent

15 | P a g e
capacities are used as thickening, emulsifying and stabilizing agents in confectioneries and

pastries like ice-cream and jelly-aces.

The effectiveness of Bioplastic must be evaluated according to its biodegradability,

tensile strength and general chemical resistance. According to the American Society for

Testing Materials (2010), for a bioplastic to be defines as biodegradable, it should meet the

following specifications:

1. The material has to degrade at least 60% of its total mass within 180 days only;

2. The material has to disintegrate into very small pieces;

3. The residue has to contain certain specified limits of heavy metals and other

contaminants.

Usually the bioplastic is immersed in different substrates. Some common substrates

used in testing biodegradability are loam soil, compost soil, freshwater, salt water, and

activated sludge Invalid source specified.. Using the initial weight and the dry weight of

the plastic strips, the amount degraded, amount left, and the percent weight loss can be

calculated for a certain period of time.

AMOUNT DEGRADED = INITIAL WEIGHT – FINAL WEIGHT

AMOUNT LEFT = INITIAL WEIGHT – AMOUNT DEGRADED

PERCENT WEIGHT LOSS = (AMOUNT DEGRADED/INITIAL WEIGHT) x 100%

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 Tensile strength. It is the maximum stress that a material can withstand while

being pulled or stretched to the point that it breaks Invalid source specified.. It is also the

maximum load that a material can support without fracture when being stretched, divided

by the original cross-sectional area of the material Invalid source specified.. To measure

Tensile Strength, a machine called Instron is used. A gradually increasing force is applied

to the material and the Instron Machine will generate the force vs. elongation curve that

can be used to obtain a complete tensile strength profile of the material Invalid source

specified..

Materials are being tested first before they are being sold in the market. One of the

properties being verified is the General Chemical Resistance which refers to the chemicals

that it can resist from deterioration and to the chemicals that destroy its fundamental

properties Invalid source specified..

General Chemical Resistance. When testing for the General Chemical Resistance of a

material particularly a plastic, thin strips of it are cut and initially weighed and it will be

soaked to some corrosive chemicals. After couple of minutes, the plastic strips will be

weighed again Invalid source specified.. Using the initial and the final weight, the amount

corroded, amount left, and the percent weight loss can also be computed.

AMOUNT CORRODED = INITIAL WEIGHT – FINAL WEIGHT

AMOUNT LEFT = INITIAL WEIGHT – AMOUNT CORRODED

PERCENT WEIGHT LOSS = (AMOUNT CORRODED/INITIAL WEIGHT) x 100%

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Review of Related Studies

The world in which it exists today is one that relies heavily on the production and

use of petroleum-based plastics. Lillian Liu writes, “Without question, the challenges

surrounding plastics waste treatment are multifaceted and complex – and, as numerous

studies have indicated, are further being compounded as time progresses. It will be up to

future generations of society to produce the necessary resources to address this growing

environmental concern with viable, long-term solutions. Truly innovative global research

and development has resulted in today’s emerging field of bioplastics.” (Liu, 2006).

Even today, there are countless researches and journal entries that aim to pioneer

and strive in bioplastics. Lillian Liu adds, “A number of bio-based materials and their

innovative applications in food-related packaging have gained much attention over the past

several years. These new materials include starch, cellulose, and those derived from

processes involving microbial fermentation. Bioplastic development efforts have focused

predominantly upon starch, which is a renewable and widely available raw material.” (Liu,

2006).

In bioplastics, various raw materials can be used as a base for creating a product,

but starch stands out due to its economics value and availability. “In 2012, the two most

influential commercial biodegradable (and bio-based) polymers were Poly-Lactic Acid

(PLA) and starch-based polymers, accounting respectively for about 47% and 41%, of total

biodegradable polymer consumption.” (N.A. Mostafa, 2015). Lillian Liu writes, “Starch is

economically competitive with petroleum and has been used in several methods for

preparing compostable plastics. Corn is the primary source of starch for bioplastics,

18 | P a g e
although more recent global research is evaluating the potential use in bioplastics for

starches from potato, wheat, rice, b`arley, oat and soy sources.” (Liu, 2006)

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 CHAPTER III
METHODOLOGY

This research is focuses on the utilization of Ube peel waste starch and brown

seaweed cellulose as a bioplastic composite. This chapter of the Research, specifically will

consist of methods and general procedures that will be used in the gathering and

interpretation of the data.

Research Design

The research design used in this study is experimental in nature. The general

process for testing is divided into parts; the production of Dioscorea alata peel starch and

Sargassum muticum cellulose, the production of pure bioplastics and the variants with the

Sargassum muticum cellulose, and the testing process for each question stated in the pretext

to the research design.

Research Procedure

This research aims to study the characterization of Bioplastic Production from Ube

(Dioscorea alata) Starch, and subsequently, all the inquiries mentioned within the general

objectives. To produce a sample to be tested, the following steps are to be followed entirely:

The process will start by readying the following ingredients and equipment: Raw

Dioscorea alata, distilled water, glycerin, hot plate, stirring rod, 250mL beaker, mortar and

pestle, cloth sieve, drying pan, and an oven. After preparation, the Dioscorea alata will be

peeled as uniformly as can be. The peeled Dioscorea alata will then be washed with water,

and then cut into an average of 1-inch cubes. The Dioscorea alata pieces will then be

grinded down into a paste using a blender. Before blending it is important to heat a 20%
vinegar solution and add it to blender before starting the blending, this lowers the viscosity

of the solution after, and allows it to settle much faster. After grinding, the paste at this

point will be processed using a cloth sieve to remove moisture left from the washing. After

sieving, the Dioscorea alata paste is then successively washed. After removing the majority

of the excess water, the solution is then decanted to remove the supernant, in order to obtain

the actual starch that precipitated to the bottom. This process was adapted from extraction

method of Delpeuch (F. Delpeuch, 1978). The original method involved included the use

of 100 micrometer sieves and the and for the washing, 4%NaCl solution, and did not

include the use of an acetic acid solution.

The next step in the production process is the mixing of 100mL of the starch

solution for the purely starch based bioplastics, and 80 mL with 100mL of distilled water,

in a 500mL beaker. In a separate beaker dissolve 10g of Plaster of pa in 20mL Distilled

water. Both mixtures are then combined and stirred until the final solution is uniform. In

this step the ingredients need to be mixed thoroughly and evenly before proceeding to the

next point, it should be expected that the mixture will look opaque for the purely starch

based bioplastics, and slightly sprinkled with dark bits for the composite samples. Heat the

mixture on a hotplate, at 90oC. The mixture should be mixed continuously as the viscosity

increases, to avoid the solution burning at the bottom of the beaker. The final step is to dry

the mixture until the solution becomes a solid. This final step can be done in molders to

accommodate the needed shapes for the testing methods used. This production method mas

adopted from a common set of instructions used in a classroom environment experiment,

The production of thermoplastic from potato starch. Only a substitution in the raw material

is needed in order to use it for the experiment; Dioscorea alata starch in place of potato

26 | P a g e
starch. The steps presented in Figure III-2 are accurate to the experiment it was adopted

from.

Density. The measurement for density will take the average mass of 10 samples

and the average volume of 10 samples. The steps presented in Figure III-4

Density testing Flowchart will be followed for the testing procedure. The weights will be

taken using the Mettler Toledo™ MS-TS Analytical Balances with an accuracy of

0.00001g (Mettler Toledo, 2017). The volumes are to be taken using a graduated cylinder,

and measuring the displacement done by the sample (NCCHEMIST, 2012). The liquid used

in the graduated cylinder will be ethanol diluted to 80%. After gathering the data, the

masses and volumes will be averaged using EquationIII-2Averaging formula. After being

averaged the values will then be used in calculating for the density.

Tensile strength and Elasticity. The measurement of Tensile strength and

elasticity will use 10 repeat experiments and the error reported as the standard deviation.

The test will proceed with the use of Instron 3343 tensile apparatus thickness was measured

by a micrometer, and then was subjected to strain at a rate of 2 mm/min using an Instron

3343 tensile apparatus with a load cell of 500 N (Instron, 2018). The Instron Bluehill 2

software program will record the maximum tensile strength, extension at maximum tensile

strength and Young’s modulus (Instron, 2018). All results will be placed in Appendix 3.

Compressive strength. The measurement of Compressive strength will use 5

repeat experiments and the error reported will be said as the standard deviation. The test

will proceed with the use of Electronic Compression Testing Machine. With the use of its

built-in software, from each test we can acquire the load at rupture, deflection at rupture,

work at rupture, stress, and strain. All results will be placed in Appendix 4

27 | P a g e
 Biodegradability. The test for biodegradability will comprise of 3 trials and have

a run time of 6 weeks per trial. Each trial will start by weighing each sample before getting

buried in four types of soil. After being buried the samples were to be washed and then

weighed weekly, after weighing the samples are to be buried in their respective soil types.

The weights will be taken using the Mettler Toledo™ MS-TS Analytical Balances with an

accuracy of 0.00001g (Mettler Toledo, 2017). The results are to be presented in Appendix

5.

Chemical resistance. The Chemical resistance test will be conducted with 3 trials

and have a run time of 3 hours per trial. Each trial will start by weighing each sample before

getting submerged in Sulfuric acid (70%, 50%, 30%), Sodium Hydroxide (70%, 50%,

30%), and distilled water respectively. After being submerged the samples were to be

lightly dried and then weighed every 30 minutes. After weighing, the samples are to be

submerged in their respective solutions. The weights will be taken using the Mettler

Toledo™ MS-TS Analytical Balances with an accuracy of 0.00001g (Mettler Toledo,

2017). The results are to be presented in Appendix 6.

Water absorption. The water absorption test will be conducted with 5 trials and

have a run time of 3 hours per trial. Each trial will start by weighing and measuring the

volume of the sample before submerging the sample in distilled water. After being

submerged the samples were to be lightly dried and then weighed every 30 minutes. After

weighing, the samples are to be submerged back in distilled water. The weights will be

taken using the Mettler Toledo™ MS-TS Analytical Balances with an accuracy of

0.00001g (Mettler Toledo, 2017). The volumes are to be taken using a graduated cylinder,

and measuring the displacement done by the sample (NCCHEMIST, 2012). The liquid used

28 | P a g e
in the graduated cylinder will be ethanol diluted to 80%. The results are to be presented in

Appendix 7.

Research Instrument

In order to complete the study on the characterization of bioplastic production from

Dioscorea alata starch, the researcher will need the following equipment for the production

process: a hot plate, stirring rod, two 250mL beakers, blender, cloth sieve, drying oven, and

wax paper, and a drying pan. The stirring rods and beakers are to be used in order to contain

and mix the solutions for the process, and to be used as containers for the solutions at any

particular point in the process. The hot plate is to be used in order to heat the bioplastic

solution at a temperature of 130oC. The mortar and pestle are used in order to ground the

cut Dioscorea alata pieces into a uniform paste. The cloth sieve is used to separate the

unneeded larger particles from the Dioscorea alata slurry. The drying oven is to be used to

heat the wet starch at a temperature of 65oC, to remove all the moisture content from the

bioplastic slurries. After the heating the bioplastics and bioplastic composites, they are laid

out on the drying pan for a period of time and turn solid.

For the testing, the following equipment are needed: a Mettler Toledo™ MS-TS

Analytical Balance, 250mL graduated cylinder, Instron 3343 tensile apparatus, and an

Electronic Compression Testing Machine. The Mettler Toledo™ MS-TS Analytical

Balance is used for weighing samples in most tests. The 250 mL graduated cylinder is used

in conjunction with ethanol, to perform volumetric analysis on the samples. The Instron

3343 tensile apparatus is used to test for the tensile strength and elasticity of the samples.

The Electronic Compression Testing Machine is used to test for the compressive strength

of the samples.

29 | P a g e
Statistical Analysis

Through the study, the researcher will use the ANOVA statistical analysis. It will

also require the following basic formulae.

Mean

Equation III-1

Variance (s2):

Equation III-2

SSF (Sum of Squares due to the Factor)

SSF = N1(𝑥̅1−𝑥̿)2 + N2(𝑥̅2−𝑥̿)2 + N3(𝑥̅3−𝑥̿)2 + N4(𝑥̅4−𝑥̿)2 Equation III-3

SSE (Sum of Squares due to error)

SSE = (N1-1)(s1)2 + (N2-1)(s2)2 + (N3-1)(s3)2 + (N4-1)(s4)2 Equation III-4

MSF (Mean of the Squares due to the Factor)

MSF = SSF/(n-1) Equation III-5

MSE (Mean of the Squares due to Error)

MSE = SSE/(N-n) Equation III-6

Get F

F = MSF/MSE Equation III-7

30 | P a g e
 CHAPTER IV

Results and Discussion

This chapter includes the findings and analysis of the results of the experiments

during the research process. The data points were shown, interpreted, analyzed and

validated to come up with significant results.

Bioplastic Yields

Starting with the production process, below is the comparison of the raw

materials used to the mass of bioplastic produced per type.

Raw material to Product Data

Water Plaster of Glycerol Acetic Starch Cellulose Bioplastic
(mL) Paris (g) (mL) acid (mL) (g) (g) (g)
Ube Peel
100 10 30 20 12 0 54.629
starch
Corn
120 10 30 0 12 0 60.215
starch
Ube Peel 52.357
starch
100 10 30 20 9 3
with
variant
Corn 58.674
starch
120 10 30 0 9 3
with
variant
Table IV-1

The table above shows the various masses and volumes needed to bake each type

of bioplastic used in the research. For the first bioplastic; no cellulose is added but it

contains acetic acid left over from the extraction process. It will be the reference as to what

properties an ube based bioplastic has. For the second; it serves as the main control

bioplastic of the study, since it is so simple and common. The third contains both

experimental variables in the study; the ube peel starch and the brown seaweed cellulose.

31 | P a g e
The last contains cornstarch and seaweed cellulose, it serves as a reference for the

effectiveness of the seaweed as something that will modify the base-bioplastic.

It was observed that the amount of yield of the ube starch peel-based bioplastic less

by 9.277% when compared to the cornstarch control. This was most likely due to the poor

quality and purity of the starch that could be extracted from the ube peel, seeing as their

might have been other non-reactive substances along with the starch that was carried along.

It was also observed that the yield of the bioplastic went down by an average of 3.359%

when the brown seaweed cellulose was added.

Biodegradation of the Bioplastic Samples

The biodegradation test was conducted with three samples for each bioplastic type,

and the data averaged before further analyzing.

%W/W of Bioplastic Sample Remaining

Days used for Biodegradation
0 2 4 6 8 10 12
Ube Peel starch 100 99.8421 99.5855 99.2321 98.7845 98.2461 97.6211
Corn starch 100 99.3803 98.7676 98.1622 97.5647 96.9754 96.3947
Ube Peel starch
with variant
100 99.7124 99.4275 99.1452 98.8655 98.5883 98.3136
Corn starch with
variant
100 99.4867 98.9777 98.4728 97.9721 97.4755 96.9830
Table IV-2

The table above shows the degradation of the bioplastic sample over the testing

period. Through comparison we can see that there is a difference in the remaining masses

in the samples. Using the ANOVA statistical analysis, the difference can be verified if

indeed significant.

32 | P a g e
 ANOVA statistical analysis results of the Rate of biodegradation

Mass biodegraded Sum of Squares Df F Interpretation

Within the group 15.8370561 28 2.09149 significant

Between the groups 33.1230373 3

Table IV-3

Using the Sum of squares and the degrees of freedom, we can find for the statistical

significance. The F-value of 2.09149 that is greater than the p-level (.05), which implies that

there is a significant difference in terms of biodegradation between the bioplastic samples. The

graph below shows the trend taken by the rates in the experiment.

%w/w Biodegradation rates in the samples

20
18
16
14
12
Ube Peel starch
%w/w

10
Corn starch
8
Ube Peel composite
6
4 Corn starch composite

2
0
0 5 10 15
Interval (Days)

Figure IV-2

33 | P a g e
Water Absorption in The Bioplastic

Water Absorption test Data

Minutes
0 30 60 90 180 210
Mass (UPSB) 2.2673 2.287044594 2.32579038 2.37999709 2.48904218 2.65588745
Mass (CSB) 0.8807 0.890723653 0.91111451 0.94257936 1.00880647 1.09197521
Mass
1.7002 1.715504089 1.74652678 1.79411586 1.89321946 2.01578022
(UPSB+)
Mass (CSB+) 0.6332 0.639751471 0.65305847 0.67353974 0.71644944 0.76997789
Table IV-4

Table IV-4 includes the data connoting the capability of the bioplastics to hold

water. Comparing using the raw data, it can be inferred within the time frame that Ube peel

starch -based bioplastic is the most water absorbent. Using the data below we can also

verify statistically that the Ube peel-based bioplastic has significant differences to its corn

starch counterpart. The F-value of 4.538859 that is greater than the p-level (.05), which

implies that there is a significant difference in terms of water absorption between the

bioplastic samples. The graph below shows the trend taken by the rates in the experiment.

ANOVA statistical analysis results of the Rate of Water absorption

Mass of hydrated
Sum of Squares Df F Interpretation
Bioplastics
Within the group 0.45271586 28 4.538859 Significant
Between the groups 0.09974222 3
Table IV-5
Chemical Resistance in The Bioplastics

Within the experiment, the concentrations of the chemicals used, specifically the

acids were too high. Thus, the testing time for each sample was halved. The weights taken

at half the time were used instead, because the sample found in the acids fully dissolved.

34 | P a g e
 Chemical Resistance test Data
Weight(g)
0 30 60
Sulfuric acid (70%) (UPSB) 1.185 0.325431 n/a
Sulfuric acid (70%) (CSB) 0.492 0.081857 n/a
Sulfuric acid (70%) (UPSB+) 0.8134 0.133858 n/a
Sulfuric acid (50%) (CSB+) 0.4655 0.127249 n/a
Sodium hydroxide (70%) (UPSB) 1.217 0.932296 0.547117
Sodium hydroxide (70%) (CSB) 0.3973 0.314444 0.196967
Sodium hydroxide (70%) (UPSB+) 1.336 1.020105 0.594733
Sodium hydroxide (70%) (CSB+) 0.4655 0.367228 0.228543
Hydrochloric acid (70%) (UPSB) 1.3527 0.526223 n/a
Hydrochloric acid (70%) (CSB) 0.4573 0.114346 n/a
Hydrochloric acid (70%) (UPSB+) 1.8979 0.732264 n/a
Hydrochloric acid (70%) (CSB+) 0.5415 0.134757 n/a

Using the ANOVA statistical analysis, the significance was still able to be

computed. The F-value of 0.404995 that is greater than the p-level (.05), which implies that

there is a significant difference in terms of chemical resistance between the bioplastic

samples. The graph below shows the trend taken by the rates in the experiment.

ANOVA statistical analysis results of the Chemical resistance

Mass of hydrated
Sum of Squares Df F Interpretation
Bioplastics
Within the group 11.64748404 12 0.404995 Significant
Between the groups 28.75955815 3

35 | P a g e
 CHAPTER V

Conclusion and Recommendations

This chapter contains the conclusions based on the results found out in the study as

well as recommendations for improvement and parallel studies of this research.

Conclusion

Through the study, the researchers were able to discover properties of Ube peel

starch as a bioplastic and Seaweed Cellulose as something that can modify the properties

of a bioplastic. Specific achieved goals included:

1. That it is possible to create bioplastics from the starch found in the peel of

Ube. This was proven when the bioplastic was produced and tested, both as

a stand alone and with the adding of seaweed.

2. That their significant differences in the biodegradation of bioplastic

produced from Ube peel starch and brown seaweed cellulose, and the

cornstarch-based seaweed.

3. That their significant differences in the chemical resistances of bioplastic

produced from Ube peel starch and brown seaweed cellulose, and the

cornstarch-based seaweed.

36 | P a g e
Recommendations

All the future recommendations for any parallel or continuing researches are below:

1. It is recommended to any future researcher that continue in Ube peel starch-

based bioplastics that the mechanical properties of the bioplastic be heavily

prioritized. This due to the testing methods being un available to the

researchers at the current moment.

2. It is recommended that the ratios of the Ube peel starch to the brown

seaweed cellulose be varied. This is to see to what degree the brown

seaweed cellulose can affect the final bioplastic composite.

3. It is also recommended that other production methods be tested with the

same raw materials. This is to see which production methods would

improve further this type of bioplastic.

37 | P a g e
 Appendix

38 | P a g e
 Apendix A
Appendix A-1

Raw material to Product Data

Water Plaster of Glycerol Acetic Starch Cellulose Bioplastic
(mL) Paris (g) (mL) acid (mL) (g) (g) (g)
Ube Peel
100 10 30 20 12 0 54.629
starch
Corn
120 10 30 0 12 0 60.215
starch
Ube Peel 52.357
starch
100 10 30 20 9 3
with
variant
Corn 58.674
starch
120 10 30 0 9 3
with
variant

Appendix A-2

Tensile strength test Data

Samples Average
1 2 3 4 5 6 7 8 9 10
Young’s
Modulus
Maximum
tensile
strength
Maximum
elongation

39 | P a g e
 Appendix A-2

Samples Average
1
3 4 5 6 7 8 9 10

Load at
Rupture
Deflection
at Rupture
Work at
Rupture
Stress
Strain

Appendix A-4

Biodegradation test Data

Days
0 2 4 6 8 10 12
Ube Peel starch 1.4486 1.4443 1.4356 1.4227 1.4058 1.3848 1.3601
Corn starch 0.7652 0.7591 0.7470 0.7293 0.7063 0.6785 0.6466
Trial 1

Ube Peel starch

2.1246 2.1034 2.0617 2.0006 1.9219 1.8280 1.7213
with variant
Corn starch with
0.8002 0.7952 0.7854 0.7709 0.7520 0.7290 0.7024
variant
Ube Peel starch 2.7876 2.7792 2.7626 2.7378 2.7052 2.6648 2.6173
Corn starch 0.5121 0.5080 0.4999 0.4881 0.4727 0.4541 0.4328
Trial 2

Ube Peel starch

1.3363 1.3230 1.2967 1.2583 1.2088 1.1497 1.0826
with variant
Corn starch with
0.3662 0.3639 0.3594 0.3528 0.3442 0.3336 0.3214
variant
Ube Peel starch 0.4299 0.4286 0.4260 0.4222 0.4172 0.4110 0.4036
Corn starch 0.4573 0.4536 0.4464 0.4358 0.4221 0.4055 0.3865
Ube Peel starch
1.5271 1.5119 1.4819 1.4380 1.3814 1.3139 1.2372
with variant
Trial 3

Corn starch with

0.6386 0.6346 0.6268 0.6152 0.6002 0.5818 0.5605
variant

40 | P a g e
 Appendix A-5

Chemical Resistance test Data

Weight(g)
M 0mins 30mins 60mins
Sulfuric acid (30%) (UPSB) 1.185 0.325431 n/a
Sulfuric acid (30%) (CSB) 0.492 0.081857 n/a
Sulfuric acid (30%) (UPSB+) 0.8134 0.133858 n/a
Sulfuric acid (30%) (CSB+) 0.4655 0.127249 n/a
Sodium hydroxide (50%) (UPSB) 1.217 0.932296 0.547117
Sodium hydroxide (50%) (CSB) 0.3973 0.314444 0.196967
Sodium hydroxide (50%) (UPSB+) 1.336 1.020105 0.594733
Sodium hydroxide (50%) (CSB+) 0.4655 0.367228 0.228543
Hydrochloric acid (29%) (UPSB) 1.3527 0.526223 n/a
Hydrochloric acid (29%) (CSB) 0.4573 0.114346 n/a
Hydrochloric acid (29%) (UPSB+) 1.8979 0.732264 n/a
Hydrochloric acid (29%) (CSB+) 0.5415 0.134757 n/a

Appendix A-6

Water Absorption test Data

Minutes
0 30 60 90 180 210
Mass (UPSB) 2.3187 2.3485 2.3750 2.3987 2.4224 2.3187
Mass (CSB) 0.9051 0.9194 0.9320 0.9434 0.9548 0.9051
Mass (UPSB+) 1.7374 1.7591 1.7782 1.7954 1.8125 1.7374
Mass (CSB+) 0.6491 0.6584 0.6667 0.6741 0.6815 0.6491

41 | P a g e
 Appendix C

Documentation

C-1. Gathering of Raw Materials

42 | P a g e
C-2. Preparation of Raw materials

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C-3. Extraction of Raw materials to produce cellulose and starch

44 | P a g e
C-4. Making of the Bioplastic

45 | P a g e
C-5. Drying and weighing of the Bioplastic

46 | P a g e
C-7. Water Absorption Test

C-8. Chemical Resistance Test

47 | P a g e
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48 | P a g e
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