N-OCTACOSANOL DERIVED FROM TARO (COLOCASIA ESCULENTA) LEAVES

USED AS AN ULTRAHYDROPHOBIC AUTOMOTIVE GLASS COATING

A Thesis Proposal

Presented to the Materials Engineering Department

College of Engineering and Technology

University of Saint La Salle

Bacolod City

Presented by:

Arra Mae C. Pomarin

Maxiegene R. Nonaillada

Richard T. Rodillado III

Engr. Rafael Diamante

Co-researcher
 1

Background of the study

The Philippines is one of the world’s tropical country that experiences constant

raining, dirt road and busy highways along with pollution. Due to the rapid increase in

the economy and industrialization, most of the population have the capacity of owning a

vehicle due to its benefits like safety, convenience, and efficiency.

It is crucial for car owners to maintain their most valued cars and keep them

clean, especially when it comes to the glass panels that would affect their driving

experience. Neglected windshields and windows may affect the driving experience as it

may hinder the driver’s vision which is an important aspect in the road and it also

concerns the safety for both drivers and pedestrians.

Automotive coatings have a huge help in the maintenance of automobiles but on

the other hand, downsides cannot be avoided. Commercially available synthetic glass

coating uses compounds like manganese oxide polystyrene, zinc oxide polystyrene and

carbon nano tube structures which is harmful to the environment and expensive

(Streitberger et al., 2008).

Coatings that offer a hydrophobic  or superhydrophobic surface can impart

multiple advantages to the coating surface and substrate they are applied to. Advantages

may include decreased dirt retention, self-cleanability, improved moisture and corrosion

resistance, as well as extended life expectancy of the coating and substrate. The surface

characteristics can create different coatings, ranging from hydrophilic (water-loving)

coatings to superhydrophobic coatings, which are highly water-repellent (Gelest, 2006).

Interest in superhydrophobic surfaces has much increased in recent years. Much

of the inspiration for the recent interest has come from plant leaves, specifically the Lotus
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plant, for which superhydrophobicity underlies an effective self-cleaning mechanism

called the Lotus effect. Self-cleaning surfaces that are capable of repelling

contaminants, including solid particles, organic liquids, and biocontaminants (Bittuon et

al., 2009). Superhydrophobicity is the core property that leads to the Lotus effect-based

self-cleaning (Rohatgi et al., 2011).

Taro (Colocasia esculenta) leaves have been found to display surface

structures/features at both the micrometer and nanometer scale that have similar

characteristics to lotus leaves (Fawcett et al.,2011). The epicuticular waxes of vascular

plants like Taro have been shown to have n-alkanols with an even number of carbon

atoms (typically C22-C30). One of the most abundant n-alkanols in higher plants is 1-

octacosanol [CH3(CH2)26CH2OH]. Octacosanol is the main component of a natural

product wax extracted from plants which has a number of applications (Ahmed et

al.,2014).

With this, the researchers’ aimed to produce an ultrahydrophobic glass coating

derived from taro leaves that can be comparable to the commercially available glass

coating.

Statement of the problem

The main objective of the study is to determine the potential of n-octacosanol derived

from taro leaves as an ultrahydrophobic automotive glass coating.

Specifically, it aims to answer the following questions:

1. How many grams of taro leaves can be used to extract 1 gram of n-octacosanol?

2. Can the extracted n-octacosanol produce an ultrahydrophobic coating?

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3. What is the significant difference in the properties of the produced

ultrahydrophobic coating with the commercially available hydrophobic coating in

terms of:

a. Hydrophobicity test

b. Scratch Resistance

c. Chemical Resistance

d. Adhesion

Hypothesis

There is no significant difference in the properties of the produced ultrahydrophobic

automotive glass coating derived from taro leaves with the commercially available

hydrophobic automotive glass coating in terms of:

a. Hydrophobicity Test

b. Scratch Resistance

c. Chemical Resistance

d. Adhesion Test

Scope and Limitations

The study focused on the extraction of n-octacosanol, the determination of its

hydrophobicity and its application as a raw material for the production of

ultrahydrophobic automotive glass coating. Testings in this study was limited only to

hydrophobicity test, scratch resistance, chemical resistance and adhesion test. The

improvised test methods was done at the University of Saint La Salle Materials
 4

Engineering Laboratory. The extracted n-octacosanol from taro leaves was compared to

the commercially available automotive glass coating in terms of physical and chemical

properties only. The taro leaves that were used was collected from the municipality of

Isabela. The chloroform used for the extraction of n-octacosanol was acquired from

University of St. La Salle Baolod Chemical Laboratory and the Tetrahydrofuran (THF)

used for the production and application of the coating was acquired from Yana

Chemodities, Mandaue City, Cebu. The extraction of n-octacosanol and the production

and application of the coating was conducted at the University of Saint La Salle Materials

Engineering Laboratory. The characterization of the n-octacosanol via FTIR was

conducted at the University of the Philippines Visayas, Municipality of Miagao, Iloilo

Province.

Definition of Terms

Contact Angle. The contact angle is the angle, conventionally measured through the

liquid, where a liquid/vapor interface meets a solid surface. It quantifies the wettability of

a solid surface by a liquid via the Young equation.

In this study, contact angle is the basis used to determine the hydrophobicity of the

automotive glass coating.

FTIR (Fourier Transform Infrared). Is a test performing quantitative and

qualitative analysis of organic compounds and determines the chemical structure of of

many inorganic compounds. The FTIR microscope accessory permits analysis of

samples as small as a few microns in diameter

(http://photometrics.net/PhotoMetrics/fourier-transform-infrared-ftir-spectroscopy/)
 5

In this study, FTIR was used to identify the presence of n-octacosanol derived from

taro leaves.

Hydrophobicity. In greek words, hydro means water and phobicity means lack of

affinity. A surface is hydrophobic when Ø is >90 and the surface tends to repel or fails

to mix with water. It imparts multiple advantages to the coating surface and substrate

they are applied to. Advantages may include decreased dirt retention, self-cleanability,

improved moisture and corrosion resistance, as well as extended life expectancy of the

coating and substrate (Lewarchik, 2015)

In this study, hydrophobicity was used as the basis for the effectiveness of the

produced automotive glass coating.

N-octacosanol. N-octacosanol is a straight-chain aliphatic 28-carbon primary fatty

alcohol that is common in the epicuticular waxes of plants, including the leaves of many

species of Eucalyptus, of most forage and cereal grasses, of Acacia, Trifolium, Pisum and

many other legume genera among many others, sometimes as the major wax constituent

(https://pubchem.ncbi.nlm.nih.gov/compound/1-Octacosanol#section=Top).

In this study, it was used as the raw material for the production of the

ultrahydrophobic automotive glass coating derived from taro leaves.

Taro Leaves. Perennial, glabrous, herb growing to a height of 1 m or more, with a

massive, fleshy corm at the base, and lateral, thick, edible runners. Root system

adventitious, fibrous, and shallow. Storage stem (corm) massive (up to 4 kg), cylindrical

or spherical, up to 30 x 15 cm, usually brown, with lateral buds located above leaf scars

giving rise to new cormels, suckers or stolons. Leaves are arranged in a loose rosette;

blades pointing downward, 23-55 × 12-38 cm, cordate or lanceolate, sub-coriaceous,

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green above, glaucous below, the apex obtuse, acute or shortly acuminate, the base

peltate-cordate, the margins more or less wavy, with a submarginal collecting vein;

petioles erect, to 85 cm long, inserted 3-7 cm from base of blade. Inflorescences axillary,

ascending, solitary; peduncles nearly as long as the petiole, cylindrical; spathe fleshy, to

35 cm long, the tube green, the blade lanceolate, not much wider than the tube, yellow to

orange, flexing open near the base, then deflexing and dropped; spadix yellow, much

shorter than the spathe, the sterile flower zone and the distal appendage shorter than the

fertile zones. Fruit is a many-seeded berry, densely packed and forming a fruiting head.

Seeds are ovoid to ellipsoid, less than 2 mm long, with copious endosperm (Acevedo-

Rodríguez and Strong, 2005; Langeland et al., 2008).

In this study, taro leaves was used as the plant source for the n-octacosanol which is

primarily present in the leaf blade.

Ultrasonic Bath. Ultrasonic bath/cleaning is a process that uses ultrasound (usually

from 20–400 kHz) and an appropriate cleaning solvent (sometimes ordinary tap water) to

clean items. The ultrasound can be used with just water, but use of a solvent appropriate

for the item to be cleaned and the type of soiling present enhances the effect. Cleaning

normally lasts between three and six minutes, but can also exceed 20 minutes, depending

on the object to be cleaned (Badavinac et al.,2002).

In this study, ultrasonic bath was used after n-octacosanol was mixed with THF to

make the solution transparent.

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Significance of the Study

The study is significant to the following sectors:

Automobile Industry. The study can help the companies on having a new choice of

raw materials for their hydrophobic coating products and their automotive glasses which

are less expensive, easily acquired and non-toxic which can lessen their production

expenses and at the same time, enhance the quality of their product.

Automobile Owners. Car owners can benefit from the produced product because

with the automobile companies having a new raw material which is n-octacosanol that is

cheap and easily acquired and at the same time, with no significant difference to the

commercially available one, they can be assured of a quality and less expensive

ultrahydrophobic glass coating for their automobiles.

Environment. The production of an ultrahydrophobic automotive glass coating

using n-octacosanol extracted from taro leaves, if found feasible, can help prevent the use

of flourocarbons in water repellancy which is potentially hazardous and VOC’s (Volatile

Organic Compounds) which is at the same time, a threat to the environment.

Farmers. This study can help small time farmers to earn extra income from the

collection of taro leaves which was used as a raw material in the production of the

ultrahydrophobic automotive glass coating.

Future Researchers. This study can benefit the future researchers by giving them

information and knowledge about n-octacosanol extracted from taro leaves for a potential

widening of the product.

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Review of Related Literature

There have been several studies about using biowaxes for hydrophobic coatings in

order to eliminate the usage of petroleum based products. Some of which are wheat straw

wax, rice bran wax and cereal straw waxes. This section discusses about literatures

related to the present study. A synthesis is also provided to elaborate major findings

relevant to the study.

Glass

A glass is any of different amorphous materials produced from a melt by cooling to

rigidity without crystallization; it is a material that is usually transparent or translucent

that consists of a mixture of silicates and produced by the fast cooling of magma.

(https://www.merriam-webster.com/dictionary/glass, ND). The properties of glass have

been beneficial to man for the past years. However, the material itself is expensive, brittle

and melts in high temperature. (https://sites.google.com/site/thekacassite/glass/what-are-

the-advantages-and-disadvantages-of-glass)

Automotive Glass

Automotive glasses are divided into two types, TSG (Tempered Safety Glasses) and LSG

(Laminated Safety Glasses). TSGs are single layered, installed in a thickness of 3.15 mm

while LSGs are double layered with a thickness between of 5-6 mm and is made up of

two sheets of glasses with a thickness between 2.1-2.6 mm with an intermediate plastic

inner layer made up of PVB (Polyvinyl Butyral) and is limited by mechanical property

and stone impact protection (Gopinath,2012).

Coated glass
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Surface coatings can be applied to glass to modify its appearance and give it many of

the advanced characteristics and functions available in today's flat glass products, such as

low maintenance, special reflection/transmission/absorption properties, scratch

resistance, corrosion resistance, etc. (Retrieved from

http://www.glassforeurope.com/en/products/main-types-of-glass.php, September 2016).

Coatings are usually applied by controlled exposure of the glass surface to vapours,

which bind to the glass, forming a permanent coating. The coating process can be applied

while the glass is still in the float line with the glass still warm, producing what is known

as "hard-coated" glass (Retrieved from http://www.glassforeurope.com/en/products/main-

types-of-glass.php, September 2016). Coatings are usually applied by controlled exposure

of the glass surface to vapours, which bind to the glass, forming a permanent coating. The

application process of the glass coating is by pouring or pump-spraying it onto the

microfiber cloth to saturate it, and then wiping it into the glass surface in a criss-cross

pattern to ensure complete coverage. (Retrieved from

https://www.nanotechcoatings.com/media/2017/8/glass-hydrophobic-application)

Raw Materials

Taro Leaves

Taro leaves are the leaves of a taro plant which is grown as a root crop throughout

the humid tropics and is one of the most important food staples in the pacific. It needs a

long, frost free growing season and plenty of water. Taro has large, light green, heart

shaped leaves, fleshy stems and grows up to 1.5 m in height. Taro is suitable for both

wetland and dryland cultures. Taros are edible aroids, with large, broad leaves on stems

growing from a corm or enlarged starchy stem with numerous roots. The main difference
 10

between the two species of taro, X. sagittifolium and C. esculenta, is in the leaf shape;

Xanthosoma spp have sagittate, arrowshaped leaves whereas the leaves of Colocasia spp

are peltate or rounded/shield shaped (Goebel et al.,ND). The average weight percent of n-

octacosanol to one taro leaf is 0.15% (http://ndb.nal.usda.gov).

Figure 1. Colocasia Esculenta

N-Octacosanol

N-Octacosanol (C28H58O) with a molecular weight of 410.771 g/mol, is a type of a

straight chain aliphatic 28 carbon primary fatty alcohol usually found on epicuticular

waxes of plants including leaves of some eucalyptus, acacia, trifolium, pisum and

sometimes as a major wax constituent of legume genera

(https://cameochemicals.noaa.gov/chemical/20809).

Processes

N-Octacosanol Extraction

The precleaned Taro leaf blades were selected, prepared and washed with a

solution of chloroform to remove the surface waxes (Poinern, 2011). The first step in the

washing procedure is by slowly pouring a 50 mL chloroform solution over the entire

inclined leaf and collecting the run off in a beaker. The washing period of the chloroform
 11

would be 30 seconds. In this method, the n-octacosanol is efficiently extracted from the

leaf surface.

Characterization

FTIR (Fourier Transform Infrared)

FTIR is the preferred method of infrared spectroscopy. When IR radiation is passed

through a sample, some radiation is absorbed by the sample and some passes through (is

transmitted). The resulting signal at the detector is a spectrum representing a molecular

‘fingerprint’ of the sample. The usefulness of infrared spectroscopy arises because

different chemical structures (molecules) produce different spectral fingerprints. The

Fourier Transform converts the detector output to an interpretable spectrum and generates

spectra with patterns that provide structural insights

(https://www.thermofisher.com/us/en/home/industrial/spectroscopy-elemental-isotope-

analysis/spectroscopy-elemental-isotope-analysis-learning-center/molecular-

spectroscopy-information/ftir-information/ftir-basics.html).

Figure 2. FTIR Illustration

Coating Production and Application

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A typical spray coating process for rough polymer surface is as follows: 1 g of n-

octacosanol is dissolved in 25 mL of THF (Tetrahydrofuran) under ultrasonic bath

operating at 40 kHz to form a transparent solution. An airbrush was powered by air at 20

psi.

Tetrahydrofuran

Tetrahydrofuran (THF) is a general purpose, highly volatile organic solvent. It is a

colorless, water-miscible, mobile liquid that offers a very good solvent power for

numerous organic substances and is used as a starting material for various syntheses.

THF can be recovered easily, without decomposition, from off-gas streams and

contaminated solvents, making it suitable for closed-loop processes designed to avoid

pollution. THF is a clear, colorless, low-boiling, volatile, polar liquid. It is a cyclic,

aliphatic ether with a characteristic odor reminiscent of acetone. THF has excellent

solvent power for numerous organic substances. It is miscible with water and all common

organic solvents

(https://worldaccount.basf.com/wa/NAFTA/Catalog/ChemicalsNAFTA/doc4/BASF/

PRD/30076724/?asset_type=pi/

pdf&language=EN&urn=urn:documentum:eCommerce_sol_EU:09007bb280020780).

Product Testing

Hydrophobicity

Cohesive forces between molecules inside a liquid are balanced with adjacent ones.

Those on the surface of a liquid are unbalance and as an effect, they exhibit strong

attractive forces upon the surfaces where the liquid rests. This unbalanced intermolecular

forces at the surface of a liquid is called (causes) surface tension. Thus, the surface
 13

tension of a liquid along with external forces such as gravity are responsible for the shape

of the drop of a liquid when it comes in contact with another surface. This property can

be visualized through the behavior of a drop of liquid on a surface because surface

tension, along with gravitation force, is responsible for the shape of the liquid. When the

drop of a liquid comes in contact with a surface, three different surface tension interfaces

can be found. These interfaces are surface-vapor, surface-liquid, and liquid-vapor. These

three interfaces stop at the contact line where they come to equilibrium to minimize their

surface energy.

Figure 3. Balance and Unbalanced Molecules inside a Water Sample and at the

Surface of the Water

If the liquid-vapor surface tension is smaller than the solid-vapor surface tension, the

liquid-solid interface will increase in order to minimize energy. This will cause the

contact angle between the surface and the liquid to decrease. If the contact angle of the

liquid is less than 30 degrees, it is then said that the surface is hydrophilic, which means

that the liquid will wet the surface. This means that the surface-liquid interface was

nearly equal to the cohesive intermolecular forces inside the liquid. However, this does

not necessarily mean that the water will easily drain from the surface. If the contact angle

is less than 10 degrees, the surface is then said to be superhydrophilic and at this point,

the liquid was able to drain off the surface without showing resistance. On the other hand,
 14

if the contact angle is greater than 90 degrees, the surface is then hydrophobic, which

means that the liquid will not wet the surface. Surfaces that display contact angle greater

than 150 degrees are identified as super hydrophobic. The theoretical maximum contact

angle is 120 degrees on a chemically treated surface. This equation tells us that physical

treatments need to be introduced to enhance the hydrophobicity of a chemically treated

surface

(http://nascent-erc.org/wp-content/uploads/2016/03/TestingHydrophobicMaterials_Negle

y). The contact angle can also be determined using the ImageJ software plugin. In this

process, pictures of water droplets in a glass surface were taken and uploaded to the

software. For each measurement, two points were manually chosen to define the baseline

and three points along the drop profile. The program then fits the profile of the drop and

calculated the contact angle using the sphere approximation or the ellipse approximation

(http://www.temple.edu/borguet/publication/documents).

Scratch Resistance

Coating on substrates can be damaged by abrasion during manufacturing and service.

This test method has been useful in evaluating the abrasion resistance of coatings.

Ratings produced by this test method have correlated well with the ratings produced by

falling abrasive values in Test Methods D968. For some materials, abrasion tests utilizing

the Taber Abraser may be subject to variation due to changes in the abrasive

characteristics of the wheel during the testing. Depending on abrading type and test

specimen, the wheel surface may change due to the adhesion of debris generated during

the test and must be refaced at more frequent intervals as agreed upon by the interested

parties. To determine if more frequent refacing is required, plot the total weight loss
 15

every 50 cycles. If a significant negative change in slope is observed prior to 500 cycles,

the point at which the slope changes determines the refacing frequency (Gonzaga, 2017).

Chemical Resistance

The protective or decorative aspects of a coating depend on its survivability.

Coatings are made to enhance the enjoyment or utility of the coated device. But the

environment of use for the device may contain attacking agents, such as oxygen, ozone,

sulfur, or nitrogen acid anhydrides.The current method for testing consists of placing a

drop of fluid (the external chemical) on the clear coat. The test runs for two hours. It is

done by placing a piece of filter paper on the clear coat and applying the drops onto the

filter paper. Since evaporation still occurs in the hindered-evaporation test, the filter

paper is refilled with drops of fluid every 15 minutes during the two hours of testing. The

pieces of material tested are then washed with water and dish soap and then kept in a

tempered room. After 24 hours, the test subjects are evaluated with regard to swelling and

discoloration and was compared and evaluated with the standard values of Volvo

Standard (VCS 1026-81779), a bases for the standards of swelling and discoloration

(Rolka, 2013).

Adhesion Test

A-X Cut Tape Test was used to test the adhesion of the specimen. An X-cut is made

through the film to the substrate, pressure-sensitive tape is applied over the cut and then

removed, and adhesion is assessed qualitatively on the 0 to 5 scale. A lattice pattern with

either six or eleven cuts in each direction is made in the film to the substrate, pressure-
 16

sensitive tape is applied over the lattice and then removed.

Figure 4. 0-5 Scale for A-X Cut Tape Test

Methodology

This section explained the materials, equipment, procedures and methods that was

used in the study. This part discussed the process of extracting n-octacosanol derived

from taro leaves, the production ultrahydrophobic coating using n- octacosanol, the

determination of its hydrophobicity and its comparison to commercially available

automotive glass coating through testing parameters.

Research Design

The study focused on the experimental research method to describe the physical

and chemical properties of the ultrahydrophobic coating produced using n-octacosanol

derived from taro leaves. The methodology of the study specifically involved the

preparation or collection of raw materials, extraction of n-octacosanol and the production

and application of glass coating. Figure 6 below shows the flow chart of the study.

Preparation/Collection of Raw
Materials

Extraction of N-Octacosanol
 Production/Application of Glass
Coating
17
Product Testing

Statistical Analysis

Figure 5. Flow Diagram of the Production of Automotive Glass Coating using

N-octacosanol extracted from Taro Leaves

A. Raw Material Preparation and Collection

Figure 8 below shows the steps that is used to prepare the raw materials for the

production of automotive glass coating.

Collecting

Cleaning

Weighing

Rinsing

Drying

Figure 6. Raw Materials Preparation

A.1 Collection
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Fresh taro leaves was collected from the municipality of Isabela.

A.2 Cleaning

The taro leaves was placed in a water basin and washed thoroughly with tap water.

A.3 Weighing

The sample was weighed using a digital weighing scale at the University of St. La

Salle College of Engineering Laboratory.

A.4 Rinsing

The taro was rinsed with deionized water to remove any contaminants and was done

carefully to avoid damaging of the wax layers and structures.

A.5 Drying

After rinsing, the sample was dried under room temperature.

A.6 Extraction of N-Octacosanol

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Figure 9 shows the steps used to extract n-octacosanol from the dried taro

leaf blades.

Preparation of wax/chloroform solution

Collection

Evaporation

Crystallization

Determination of N-Octacosanol

Figure 7. Extraction of N-Octacosanol

B.1 Preparation of wax/chloroform solution

In this procedure, 50 ml of chloroform was slowly poured over the entire inclined

taro leaf for 30 seconds. With this, the n-octacosanol was efficiently extracted from the

leaf surface. The procedure will be repeated until 1 gram of n-octacosanol can be

achieved (Le, 2011).

B.2 Collection
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The remnants of the wax was collected in a beaker and prepared for the evaporation

process.

B.3 Evaporation

The wax/chloroform solution that was collected was used for treating the surface of

glass slides. A small pipette was used to liberally cover the large planar surfaces of the

glass slide with a layer of wax/chloroform solution. The glass slides that were coated

with the wax/chloroform solution was air dried in an ambient atmospheric conditions.

During that time, the chloroform evaporated, allowing a reassembling n-octacosanol layer

form on the glass slide surface (Fawcett, 2011).

B.4 Crystallization

After 2 hours, each glass slide became opaque and had a frost-like appearance. This

indicated the presence of the pure n-octacosanol that formed over the surface of the glass

slide.

B.5 Determination of N-Octacosanol

The extracted n-octacosanol sample of about 1 gram was brought to the University of

the Philippines- Miagao Laboratory. Fourier Transform Infrared Spectroscopy (FTIR)

will used KBr pellet procedure for solid samples. 1/8” of the solid sample was taken on a

microspatula and about 0.25-0.50 teaspoons of KBr. The two was mixed thoroughly in a

mortar while grinding with the pestle. Ample amount of sample was placed to cover

bottom in pellet die. It was placed in press and press at 5000-10000 psi. The pressed

sample was carefully removed from die and was placed in the FTIR sample holder.
 21

C. Production and application of Glass Coating

Hydrophobic coating was produced from the extracted n-octacosanol.

Tetrahydrofuran or THF was added to the crystallized n-octacosanol.

C.1 Addition of Tetrahydrofuran (THF)

The coating solution was prepared by dissolving 1 g of n-octacosanol in 25 mL of

THF under ultrasonic bath operating at 40 kHz to form a transparent solution (H.S.

Hwang, et. Al, ND) and was added to crystallized n-octacosanol that reinforced its

application as coating solution.

C.2 Glass Samples Preparation

A total of twenty four 2x2 inch automotive glass was bought from Citadel Auto

Glass Bacolod. Each testing had three trials for the glass coated with the commercially

available coating and another three trials for the glass coated with the produced n-

octacosanol coating

(http://standards.sae.org/automotive/materials/glass/standards/current/).

C.3 Application of produced Glass Coating

The n-octacosanol solution was poured into the sample and wiped the surface in a

criss cross pattern to get a complete coverage.

D. Product Testing
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The produced coating was tested for the following parameters: Hydrophobicity Test,

Scratch Resistance, Chemical Resistance and Adhesion Test. The methods and

procedures that was observed during testings are described below.

D.1 Contact Angle

In hydrophobicity test, a software called ImageJ was used to determine the contact

angle of a droplet on the automotive glass coated with the sample.

D.2 Scratch Resistance

This procedure may be used for assessing the scratch resistance of coated materials

and establishing whether the scratch resistance of a material or coating is at an adequate

level by using sand paper attached to a drill press. The change in thickness of the glass

was measured to determine how resistant the glass was to constant pressure and rotation.

D.3 Chemical Resistance

This test method measures the resistance of the glass when exposed to various

chemicals like gasoline, coolant, different types of oil and washer fluid. After the testing

period, the samples was evaluated with regards to swelling and discoloration.

Grade Explanation
0 No visible swelling
1 Film somewhat swollen
2 Film clearly swollen
3 Film heavily swollen

Table 1. Table Grading of Swelling in the Clear Coat

Grade Explanation
0 No discoloration of the film.
1 Slight discoloration of the film.
2 Clear discoloration of the film.
3 Heavy discoloration of the film.
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Table 2. Table Grading of the discoloration on the clear coat

D.4 Adhesion Test

The following steps was followed for performing the adhesion test for the produced

coating.

D.4.1

An area free of blemishes and minor surface imperfections, clean and dry was

selected.

D.4.2

Two cuts was made in the film each about 40 mm (1.5 in.) long that intersect near

their middle with a smaller angle of between 30 and 45°. When making the incisions, a

straightedge was used to cut through the coating to the substrate in one steady motion.

D.4.3

The incisions was inspected for reflections of light from the glass substrate to

establish that the coating film has been penetrated. If the substrate has not been reached,

another X was made in a different location. Deepening the previous cut was not

attempted as this may affect adhesion along the incision.

D.4.4
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Before initiation of testing, two complete laps of the pressure-sensitive tape was

removed from the roll and discard. Additional length was removed at a steady rate and a

piece was cut about 75 mm (3 in.) long.

D.4.5

The center of the tape was placed in the intersection of the cuts with the tape running

in the same direction as the smaller angles. The tape was smoothed into place by finger in

the area of the incisions and was rubbed firmly with the eraser on the end of a pencil. The

color under the transparent tape was a useful indication of when good contact has been

made.

D.4.6

Within 90 6 30 s of application, the tape was removed by seizing the free end and

pulling it off rapidly back upon itself at as close to an angle of 180° as possible.

D.4.7

The X-cut area was inspected for removal of coating from the substrate or previous

coating and adhesion was rated in accordance with the scale.

D.4.8

The test was repeated in two other locations on each test panel. For large structures,

sufficient tests was made to ensure that the adhesion evaluation is representative of the

whole surface.

D.4.9
 25

After making several cuts, the cutting edge was examined and if necessary, any flat

spots was removed or wire-edged by abrading lightly on a fine oil stone before using

again. Cutting tools that develop nicks or other defects that tear the film was discarded.

Figure 8. 0-5 Scale for A-X Cut Tape Test

E. Statistical Analysis

The paired (t-Test) and Wilcoxon Signed Rank Test was used for determining if

there is a significant difference of the produced ultrahydrophobic coating to the

commercially available hydrophobic coating in terms of hydrophobicity, scratch

resistance, chemical resistance and adhesion test.

Results and Discussion

This section shows the results of the study and its individual presentation, analysis,

comparison and discussion. Tables are showed to aid the presentation of datas from the

results of the testings.

A. N-octacosanol Product Composition

 26

Table 3 shows that 47.52 grams of taro leaves, 150 ml chloroform was needed to

produce 1 gram of n-octacosanol. In total, the experiment produced 1.87 grams of n-

octacosanol using 118.6 grams of taro leaves and 400 ml chloroform.

Table 3

Taro Leaves (Grams) Chloroform (ml) N-octacosanol (Grams)

20.3 50 0.48

18.4 50 0.39

16.9 50 0.30

16.9 50 0.29

12.7 50 0.15

12.6 50 0.12

11.1 50 0.09

9.7 50 0.05

B. Product Testing
 27

B.1 Hydrophobicity Test via Contact Angle

Table 4 shows that the average contact angle of the glass coated with the commercial

coating is 154.42 degrees while the average contact angle of the glass coated with the n-

octacosanol coating is 152.84 degrees which is less than the average contact angle of the

glass with the commercial coating but still qualified as ultrahydrophobic.

Table 4

Product Trial Contact Angle Average Contact

(degrees) Angle (degrees)

Commercial 1 158.02

2 152.89 154.42

3 152.36

N-Octacosanol 1 155.89

2 148.73 152.84

3 153.91

B.2 Scratch Resistance

 28

Table 5 shows that the average change in thickness of the glass coated with the

n-octacosanol coating is 0.31mm and the average change in thickness of the glass

coated with the commercial coating is 0.27 which is less than the average change in

thickness of the glass coated with the n-octacosanol coating.

Table 5

Product Trial Initial Final Change in Average

(mm) (mm) Thickness Change
(mm) in
Thickness
(mm)
Commercial 1 6.72 6.54 0.18

2 6.66 6.31 0.35 0.27

3 6.61 6.34 0.27

N- 1 6.83 6.47 0.36

Octacosanol

2 6.68 6.36 0.32 0.31

3 6.67 6.42 0.25

B.3 Chemical Resistance

 29

Table 6.1 shows the chemical resistance test for gasoline. The average grading of

discoloration for the commercially coated glass is 0 while the average grading of

discoloration for the n-octacosanol coated glass is 0.33. The average grading of swelling

for the commercially coated glass is 0.33 and the average grading of swelling for the n-

octacosanol coated glass is 0.67. The average grading for both the discoloration and

swelling of the n-octacosanol coated glass is more than the commercially coated glass.

Table 6.1 Gasoline

Product Trial Grading of Average Grading of Average

Discoloration Grading of Swelling Grading of

Discoloration Swelling

Commercial 1 0 0

2 0 0 1 0.33

3 0 0

N-octacosanol 1 0 0

2 0 0.33 1 0.67

3 1 1
 30

Table 6.2 shows the chemical resistance test for coolant. The average grading of

discoloration for the commercially coated glass is 0 while the average grading of

discoloration for the n-octacosanol coated glass is 0.67. The average grading of swelling

for the commercially coated glass is 0 and the average grading of swelling for the n-

octacosanol coated glass is 0.67. The average grading for both the discoloration and

swelling of the n-octacosanol coated glass is more than the commercially coated glass.

Table 6.2 Coolant

Product Trial Grading of Average Grading of Average

Discoloration Grading of Swelling Grading of

Discoloration Swelling

Commercial 1 0 0

2 0 0 0 0

3 0 0

N-octacosanol 1 0 0

2 1 0.67 1 0.67

3 1 1
 31

Table 6.3 shows the chemical resistance test for oil. The average grading of

discoloration for the commercially coated glass is 0 while the average grading of

discoloration for the n-octacosanol coated glass is 0.33. The average grading of swelling

for the commercially coated glass is 0 and the average grading of swelling for the n-

octacosanol coated glass is 0.33. The average grading for both the discoloration and

swelling of the n-octacosanol coated glass is more than the commercially coated glass.

Table 6.3 Oil

Product Trial Grading of Average Grading of Average

Discoloration Grading of Swelling Grading of

Discoloration Swelling

Commercial 1 0 0

2 0 0 0 0

3 0 0

N-octacosanol 1 1 0

2 0 0.33 1 0.33

3 0 0
 32

Table 6.4 shows the chemical resistance test for washer fluid. The average grading of

discoloration for the commercially coated glass is 0 while the average grading of

discoloration for the n-octacosanol coated glass is 0.33. The average grading of swelling

for the commercially coated glass is 0 and the average grading of swelling for the n-

octacosanol coated glass is 0.33. The average grading for both the discoloration and

swelling of the n-octacosanol coated glass is more than the commercially coated glass.

Table 6.4 Washer Fluid

Product Trial Grading of Average Grading of Average

Discoloration Grading of Swelling Grading of

Discoloration Swelling

Commercial 1 0 0

2 0 0 0 0

3 0 0

N-octacosanol 1 0 0

2 0 0.33 1 0.33

3 1 0
 33

B.4 Adhesion

Table 7 shows that the average result for the commercial coating is 6.5 and the

average result for the n-octacosanol coating is 5.

Table 7

Product Trial Scale for A-X Cut Tape Test Average

Commercial 1 5

2 4 6.5

3 4

N-octacosanol 1 4

2 3 5

3 3

C. Statistical Analysis

The results of the different parameters were statistically analyzed using paired t-test

and Wilcoxon Signed Rank Test. .

C.1 Hydrophobicity
 34

Table 8 shows that the n-octacosanol coating and the commercial coating is

comparable based on the tables interpretation.

Table 8

Product Mean t p Interpretation

Commercial 154.42

.945 .444 No Significant

Difference

N-octacosanol 152.84

C.2 Scratch Resistance

Table 9 shows that the n-octacosanol coating and the commercial coating is

comparable based on the tables interpretation.

Table 9

Product Mean t p Interpretation

Commercial .2667

-.634 .591 No Significant

Difference
 35

N-octacosanol .3100

C.3.1 Chemical Resistance for Swelling

Table 10.1 shows that the n-octacosanol coating and the commercial coating is

comparable based on the tables interpretation.

Table 10.1

Chemical Commercial N-octacosanol z P-value Interpretation

Gasoline 0.33 0.67 -1.00 .317

Coolant 0 0.67 -1.414 .157 No Significant

Difference
Oil 0 0.33 -1.000 .317

Washer Fluid 0 0.33 -1.000 .317

 36

C.3.2 Chemical Resistance Test fir Discoloration

Table 10.2 shows that the n-octacosanol coating and the commercial coating is

comparable based on the tables interpretation.

Table 10.2

Chemical Commercial N-octacosanol z P-value Interpretation

Gasoline 0 0.33 -1.000 .317

Coolant 0 0.67 -1.414 .157 No Significant

Difference
Oil 0 0.33 -1.000 .317

Washer Fluid 0 0.33 -1.000 .317

C.4 Adhesion Test

Table 11 shows that the n-octacosanol coating and the commercial coating is

comparable based on the tables interpretation.

 37

Table 11

Product Mean t p Interpretation

Commercial 6.5

-1.732 .083 No Significant

Difference

N-octacosanol 5

Conclusion

In this section, the methodology of the study that was used to achieve the

researcher’s objectives was summarized. Conclusions and generalizations of the study

were also presented.

 38

The produced n-octacosanol solution was used to coat glass samples that

underwent several testings like hydrophobicity, chemical resistance, adhesion test and

scratch resistance test. The contact angle of the produced n-octacosanol coating and the

commercial coating was determined through using the ImageJ software. After the test, it

showed that biowax from Taro leaves can be used to produce an ultrahydrophobic

coating.

Based on the observation and results of the research, the following conclusions were

drawn:

1. A total of 47.52 grams of taro leaves, 150 ml chloroform was needed to produce 1

gram of n-octacosanol.

2. Results show that the n-octacosanol extracted from the taro leaves can produce an

ultrahydrophobic coating.

3. Results show that there is no significant difference in the properties of the

produced ultrahydrophobic coating with the commercially available hydrophobic

coating in terms of hydrophobicity, scratch resistance, chemical resistance and

adhesion.
 39

Table 12. Summary for Overall Average Values

Parameter Average Value

Commercial Coating N-octacosanol Coating

Hydrophobicity 154.42 degrees 152.84 degrees

Scratch Resistance 0.27 mm 0.31 mm

Chemical Resistance: Gasoline Discoloration: 0 Discoloration: 0.33

Swelling: 0.33 Swelling: 0.67

Coolant Discoloration: 0 Discoloration: 0.67

Swelling: 0 Swelling: 0.67

Oil Discoloration: 0 Discoloration: 0.33

Swelling: 0 Swelling: 0.33

Washer Fluid Discoloration: 0 Discoloration: 0.33

Swelling: 0 Swelling: 0.33

Adhesion 6.5 5
 40

References

A. Taro Leaves

http://www.specialtyproduce.com/produce/Taro_Leaves_3409.php

http://aciar.gov.au/files/node/15487/factsheets_2_pdf_68100.pdf

https://www.sciencedirect.com/topics/agricultural-and-biological-sciences/colocasia-

esculenta

B. Glass Coating

https://www.detailxperts.net/blog/2015/10/15/glass-coating-what-is-it/

https://www.google.com/patents/US4517243

C. Hydrophobicity

http://citeseerx.ist.psu.edu/viewdoc/download?doi=10.1.1.625.340&rep=rep1&type=pdf

https://pubs.acs.org/doi/abs/10.1021/jz402762h

https://rd.springer.com/chapter/10.1007/978-1-4614-0926-7_11
 41

http://nascent-erc.org/wp-content/uploads/2016/03/

TestingHydrophobicMaterials_Negley.pdf

http://www.iccm-central.org/Proceedings/ICCM18proceedings/data/3.%20Poster

%20Presentation/Aug22%28Monday%29/P1-1~20%20Applications%20of

%20Composites/P1-9-IK0369.pdf

http://www.ipme.ru/e-journals/RAMS/no_11607/amin.pdf

https://www.researchgate.net/publication/

280115341_Superhydrophobic_materials_and_coatings_A_review

https://www.sciencefriday.com/educational-resources/hydrophobicity-will-the-drop-stop-

or-roll/

D. Coating

https://www.google.com/patents/US20140208978

https://scholarsarchive.byu.edu/cgi/viewcontent.cgi?referer=https://l.facebook.com/

&httpsredir=1&article=4858&context=etd

https://www.diva-portal.org/smash/get/diva2:860828/FULLTEXT01.pdf

https://www.sciencedirect.com/science/article/pii/S1878535213004516

https://www.scientific.net/AMR.1043.184

http://www.glassforeurope.com/images/cont/165_91347_file.pdf

E. Image J

https://www.temple.edu/borguet/Publication/Documents/pdf_files/2010-7
 42

F. Testings

http://file.yizimg.com/175706/2012061612023597.pdf

https://www.sciencedirect.com/science/article/pii/S0026057610802545

http://virtual.vtt.fi/virtual/proj6/coste18/abstractpodgorski.pdf

http://publications.lib.chalmers.se/records/fulltext/179154/179154.pdf

http://www.byk.com/fileadmin/byk/support/instruments/theory/physical-properties/en/

Intro_Adhesion.pdf

https://www.defelsko.com/resources/test-methods-for-coating-adhesion

https://www.temple.edu/borguet/Publication/Documents/pdf_files/2010-7.pdf

G. Automotive Glass

http://164.100.133.129:81/eCONTENT/Uploads/Session7%20Automotive

%20Glasses.pdf
 43

Appendix A

Taro Leaves (Grams) Chloroform (ml) N-octacosanol (Grams)

20.3 50 0.48

18.4 50 0.39

16.9 50 0.30

16.9 50 0.29

12.7 50 0.15

12.6 50 0.12

11.1 50 0.09

9.7 50 0.05

N-octacosanol Product Composition

 44

Appendix B

Product Trial Contact Angle Average Contact

(degrees) Angle (degrees)

Commercial 1 158.02

2 152.89 154.42

3 152.36

N-Octacosanol 1 155.89

2 148.73 152.84

3 153.91

Hydrophobicity Test Via Contact Angle

Product Trial Initial Final Change in Average

(mm) (mm) Thickness Change
(mm) in
Thickness
(mm)
Commercial 1 6.72 6.54 0.18

2 6.66 6.31 0.35 0.27

 45

3 6.61 6.34 0.27

N- 1 6.83 6.47 0.36

Octacosanol

2 6.68 6.36 0.32 0.31

3 6.67 6.42 0.25

Scratch Resistance

Appendix C

Product Trial Grading of Average Grading of Average

Discoloration Grading of Swelling Grading of

Discoloration Swelling

Commercial 1 0 0

2 0 0 1 0.33

3 0 0

N-octacosanol 1 0 0

2 0 0.33 1 0.67

3 1 1

Gasoline Chemical Resistance

 46

Appendix D

Product Trial Grading of Average Grading of Average

Discoloration Grading of Swelling Grading of

Discoloration Swelling

Commercial 1 0 0

2 0 0 0 0

3 0 0

N-octacosanol 1 0 0

2 1 0.67 1 0.67

3 1 1

Coolant Chemical Resistance

 47

Appendix E

Product Trial Grading of Average Grading of Average

Discoloration Grading of Swelling Grading of

Discoloration Swelling

Commercial 1 0 0

2 0 0 0 0

3 0 0

N-octacosanol 1 1 0

2 0 0.33 1 0.33

3 0 0

Oil Chemical Resistance

 48

Appendix F

Product Trial Grading of Average Grading of Average

Discoloration Grading of Swelling Grading of

Discoloration Swelling

Commercial 1 0 0

2 0 0 0 0

3 0 0

N-octacosanol 1 0 0

2 0 0.33 1 0.33

3 1 0

Washer Fluid Chemical Resistance

 49

Appendix G

Product Trial Scale for A-X Cut Tape Test Average

Commercial 1 5

2 4 6.5

3 4

N-octacosanol 1 4

2 3 5

3 3

Adhesion
 50

Appendix H

Parameter Average Value

Commercial Coating N-octacosanol Coating

Hydrophobicity 154.42 degrees 152.84 degrees

Scratch Resistance 0.27 mm 0.31 mm

Chemical Resistance: Gasoline Discoloration: 0 Discoloration: 0.33

Swelling: 0.33 Swelling: 0.67

Coolant Discoloration: 0 Discoloration: 0.67

Swelling: 0 Swelling: 0.67

Oil Discoloration: 0 Discoloration: 0.33

Swelling: 0 Swelling: 0.33

Washer Fluid Discoloration: 0 Discoloration: 0.33

Swelling: 0 Swelling: 0.33

Adhesion 6.5 5
 51

Summary for Overall Average Values

Appendix I
 52

FTIR Results