CORROSION INHIBITION OF CALAMANSI (Citrus microcarpa) FRUIT

EXTRACT ON MILD STEEL IN MURIATIC ACID (HCl)

________________________________________________________________________

A Research Paper Presented to

Ms. Davy T. Vacal
Science, Technology, Engineering, and Mathematics (STEM)
Leyte National High School
Tacloban City, 6500
_______________________________________________________________________

In Partial Fulfillment of the Requirements in

Work Immersion/Research/Career Advocacy/Culminating Activity

_______________________________________________________________________

By:

Cabataña, Jolina Mae A.

Cua, Bianca Jane A.

Daymon, Judel Ralph B.

Fabella, Marianne Lovella KZ3 R.

Lengwa, Cristal Dawn P.

Lucañas, Lyden Mael Y.

Martinez, Gea Samantha R.

Mora, Maybelle P.

Regis, Allyssa Mae M.

Regorosa, Lenuel Karl A.

Urmeneta, Roxanne Dale F.

3 March 2019
 ABSTRACT
Metals have played a vital role in the lives of human beings, even dating back to the

Bronze Age. As a result, these substances have become a prominent part in the industry and

economy. Mild steel is a type of metal often used for construcion. However, it is also prone to

corrosion, hereby causing widespread loss in the economy. The study aimed to use

Calamansi (Citrus microcarpa) fruit extract as a possible corrosion inhibitor for mild steel in

industrialized muriatic acid by Gravimetric Technique (Weight Loss Method). Different

concentrations; 2%, 5%, 7%, 10%, and 15% were used to test its inhibitory effect. The result

showed that there is a corrosion inhibition of Calamansi (C. microcarpa) fruit extract. The

15% v/v concentration showed the highest inhibition efficiency among the different

concentrations of Calamansi (C. microcarpa) fruit extract. Based on the Scheffe test,

significant differences occur between the Inhibition efficiency of the different Calamansi (C.

microcarpa) concentrations except for 5% and 7%, and 10% and 15%. For further

investigation, highly recommended for future researchers to analyze the morphology of Mild

steel surface in Industrialized Muriatic acid in the presence and absence of Calamansi (C.

microcarpa) fruit extract using Scanning electron microscopy (SEM) and the use of other

methods aside from the Gravimetric Technique

 ACKNOWLEDGEMENT

This study will not be possible if not for the individuals who have supported as

throughout our journey towards the success of this research. The researchers would like to

extend their outmost gratitude to the following persons for their contribution in the success

and completion of the study.

To our research advisers, Ms. Davy T. Vacal and Benjie G. Arias for their time and

effort in guiding us throughout the conduct of our study.

To the President of Leyte Normal University, Mr. Jude A. Duarte for allowing the

researchers to conduct their study inside the University.

To the faculty and staff of Leyte Normal University, Ms. Neuville Abenis and Mr.

Jefferson Flores, for their valuable help and teachings during our laboratory activities.

To the parents of the researchers, for their financial support, guidance and motivation

that greatly helped and inspired the researchers.

To the researchers, for their time, effort and patience in conducting this study.

Above all, to God, for his showers of blessings and unconditional love that

strengthens us to make this research possible.

The Researchers
Table of Contents

Abstract………………………………………………………………………………...……....i
Acknowledgement…………………...……………………………….………………………..ii
Table of Contents…………..…………………………………………………………….…...iii
Chapter 1 – Introduction………………..……………………………………………………..1
Background of the Study……………………..…………………………………...…..1
Statement of the Problem…………………..………………………………………….3
Research Objectives.…………..……………………………………………….…...…3
Significance of the Study………………..…………………………...………………..4
Scope and Delimitation………………………………………………………..………4
Chapter 2 – Review of Related Literature and Studies and the Conceptual Framework…..…5
Related Literature……..………….……………………………………………………5
Related Studies….………..……………………………………………………………9
Conceptual Framework…………………………………………..……….………….16
Hypotheses………………………………………………..………………….………17
Definition of Terms………………………………………………..…………………18
Chapter 3 – Methodology…………………………………..….…………………………..…19
Research Design………………………………………..………………………….…19
Sample and Sampling Method……………………………………………..………...19
Research Instruments…………………………………..…………………………….19
Procedure……………………………...……………………………………………...24
Data Analysis……………………………………..………………………………….28
Chapter 4 – Results and Discussion……………………………..………………………….29
Chapter 5 – Summary and Conclusion…………………………………...………………….33
Bibliography………………………………...………………………………………………..36
Appendices……………………………..……………………………………………………38
 Chapter I

INTRODUCTION

A. Background of the Study

Metals have played a vital role in the lives of human beings, even dating back to the

Bronze Age. As a result, these substances have become a prominent part in the industry and

economy. During the year 2013, the production of raw steel from all around the world totaled

up to 1.6 billion tons, while the production of aluminum, the next most important metal used

in engineering, amounted to 47 million tons.1 An example of a metal utilized commonly is the

Mild steel. This is a type of Mild steel containing very low amounts of carbon, ranging from

0.05% to 0.3%. Additionally, its low carbon content allows the Mild steel to be cut, joined,

and shaped with little difficulty into various products.2 Furthermore, its relatively low price

and standard durability made it possible to be commonly used as a material for building the

world’s industries and infrastructures.3 However, the greatest drawback for this metal is that

it easily degrades and corrodes because of the effects of moisture and oxygen. Due to

corrosion, economic loss occurs because it damages metal works in vehicles and makes the

framework of buildings unstable, thus, affecting the economy. Hence, the problem of

corrosion in metals inhibits the path towards achieving sustainable development.

Different approaches have been made in order to solve the problem of corrosion in

metals. As a result, considerable efforts were exerted in order to come up with possible

solutions in order to minimize corrosion, specifically, employing green inhibitors or the use

of organic substances as a medium in slowing down the decay of metals. These have been

proven to be effective in inhibiting corrosion because they exhibit alkaloids, flavonoids, and

1
Wondris, E.F., et al. “Steel.” Encyclopædia Britannica, Encyclopædia Britannica, Inc., 14 Dec. 2017,
www.britannica.com/technology/steel.
2
Lambert, P. "Sustainability of metals and alloys in construction." Sustainability of Construction
Materials (Second Edition). 2016. 105-128.
3
Dunee, and Dunee. “Difference Between Carbon Steel and Mild Steel.” DifferenceBetween.com,
Difference Between, 10 Mar. 2012, www.differencebetween.com/difference-between-carbon-steel-
and-vs-mild-steel/.
antioxidants essential to inhibit the corrosion of metals. To illustrate, several studies have

been carried out to examine different green inhibitors’ effectivity in inhibiting corrosion in

metals, such as Winged prickly ash plant (Zenthoxylum alatum)4, Marigold flower (Tagetes

erecta)5, Aloe leaf (Aloe vera)6, and guava leaves (Psidium guajava)7.

This study aims to utilize a plant extract as an inhibitor for corrosion that is readily

available, cheap, and environmentally-friendly. Citrus microcarpa, or locally known as

Calamansi, is a fruit tree home to the Philippines. Among the citrus species in the country,

the Calamansi (C. microcarpa) is the most commonly grown by the people. Studies have

been made to prove the antioxidant activity and presence of phenolic compounds in the fruit

extract of the Calamansi (C. microcarpa).8

Studies have been made to prove the corrosion inhibition of citrus fruits such as

Orange9, Pomelo10, and Lemon Balm11. However, no study has been made to determine the

corrosion inhibition of the citrus fruit, Calamansi. Therefore, the purpose of this study is to

investigate the inhibitive effect of Calamansi (C. mircocarpa) as a cheap, eco-friendly,

readily available, and efficient inhibitor for the corrosion of Mild steel in commercially

available Muriatic acid (HCl) using Gravimetric analysis (Weightloss method).

4
Chauhan, L. R., and G. Gunasekaran. "Corrosion inhibition of mild steel by plant extract in dilute HCl
medium." Corrosion Science 49.3 (2007): 1143-1161.
5
Mourya, Punita, Sitashree Banerjee, and M. M. Singh. "Corrosion inhibition of mild steel in acidic
solution by Tagetes erecta (Marigold flower) extract as a green inhibitor." Corrosion Science 85
(2014): 352-363.
6
Cang, Hui, et al. "Corrosion inhibition of mild steel by aloes extract in HCl solution
medium." International Journal of Electrochemical Science 8.1 (2013): 720-734.
7
Victoria, S. Noyel, Rohith Prasad, and R. Manivannan. "Psidium guajava leaf extract as green
corrosion inhibitor for mild steel in phosphoric acid." Int. J. Electrochem. Sci 10 (2015): 2220-2238.
8
“Philippine Calamansi.” Philippine Calamansi Association Inc,
www.philippinecalamansi.org/p/philippine-calamansi.html.
9
M’hiri, Nouha, et al. "Corrosion inhibition of carbon steel in acidic medium by orange fruit extract and
its main antioxidant compounds." Corrosion Science 102 (2016): 55-62.
10
Nurdin, Irwan, Elwina Elwina, and J. S. Maulana. "Pomelo fruits extract as green corrosion inhibitor
for mild steel in hydrochloric acid 1 m." Proceedings. Vol. 1. No. 1. 2018.
11
Asadi, Najmeh, et al. "Utilizing Lemon Balm extract as an effective green corrosion inhibitor for mild
steel in 1M HCl solution: A detailed experimental, molecular dynamics, Monte Carlo and quantum
mechanics study." Journal of the Taiwan Institute of Chemical Engineers (2018).
B. Statement of the Problem

This study intends to determine the corrosion inhibition of Calamansi (Citrus

microcarpa) fruit extract on Mild steel in Muriatic acid.

Specifically, it aims to answer the following questions:

1.) Which concentration of Calamansi (C. microcarpa) fruit extract is the most effective in

the corrosion inhibition on Mild steel in Muriatic acid?

a. 2% (v/v)

b. 5% (v/v)

c. 7% (v/v)

d. 10% (v/v)

e. 15% (v/v)

2.) Is there a significant difference between the different levels of concentration of

Calamansi (C. microcarpa) fruit extracts on Mild steel?

C. Research Objectives

The main objective of the study is to determine the corrosion inhibition of Calamansi

(C. microcarpa) fruit extract on Mild steel in hydrochloric acid.

Specifically, it seeks to determine:

1. The corrosion inhibition effect of Calamansi (C. microcarpa) fruit extracts at different

concentrations on Mild steel in Muriatic acid.

2. The significant difference between the different levels of concentration of Calamansi (C.

microcarpa) fruit extracts on Mild steel.

D. Significance of the Study

This study aims to determine the corrosion inhibition of Calamansi (C. microcarpa)

fruit extract on Mild steel in Muriatic acid. If the study provides a positive result, show that

Calamansi (C. microcarpa) fruit extract has a corrosion inhibition on Mild steel in Muriatic

acid, it will be beneficial to the following.

The Researchers. The result of this study will let the researchers gain additional

knowledge and can be used as a basis of information for the future studies the researchers

want to conduct.

School Administrators. This study will help the school administrators come up with

organized policies that might help the students when it comes to research.

Construction Industry. The outcome of this study will provide the construction

industry and researchers background knowledge about the corrosion inhibition of Calamansi

(C. microcarpa)

E. Scope and Delimitation

This study deals with the corrosion inhibition of Calamansi (C. microcarpa) fruit

extract on Mild steel in Muriatic acid. This study is limited to the use of the Calamansi (C.

microcarpa) fruit extract. To test the effectiveness, Mild steel plates will be immersed in the

solution containing the Calamansi (C. microcarpa) fruit extract and Muriatic acid.

The Calamansi (C. microcarpa), Mild steel and hydrochloric acid will be acquired

within Tacloban City. The different treatments and concentrations of Calamansi

(C. microcarpa) will be tested on the Mild steel in Muriatic acid from Tacloban City. The

researchers will conduct the experiment and gather all the necessary data needed within

January 2019 to February 2019.

 Chapter II

REVIEW OF RELATED LITERATURE AND STUDIES AND THE CONCEPTUAL

FRAMEWORK

Related Literature on Corrosion

Metals have been an integral part of human life. It is used for an array of purposes

important and vital to the daily lives of people. Moreover, it has been a part of the industry,

dating back to Georgian times. However, due to corrosion, these metals, through a natural

and normal process, return to their lowest energy state.2

When a metal weathers, decays, and is vexed, it physically corrodes. Kelly et al.

defined degradation of metals properties caused by the chemical reaction with its

surroundings. Corrosion happens when metals come in contact with moisture or water bases

(H2O, NaOH, CaCO3, NaHCO3, etc.), acids such as hydrochloric acid, salts, liquid chemicals,

gases such as formaldehyde, ammonia and sulfur containing gases.12

The corrosion process does not happen immediately, it requires an initiation period to

make the material surface subject for sulfur oxidation. However, in a study conducted by

Jiang, et al. (2015), they identified the controlling factors for the initiation of corrosion of

fresh concrete sewers. Wherein one significant step during the stage is the dissociation of

Hydrogen Sulfide to HS in the adsorbed film of water on the said concrete. In addition, the

oxidation rate of chemical sulfide doubles up when exposed to an increase in temperature of

9 ֯C by the same study. Thus, the relative humidity, concentration and the temperature are the

parameters that affects the initiation period of corrosion.13

2
12
Ibid 105-128.
Raja, Pandian Bothi, et al. "Reviews on corrosion inhibitors: a short view." Chemical Engineering
Communications 203.9 (2016): 1145-1156.
13
Jiang, Guangming, et al. "Identification of controlling factors for the initiation of corrosion of fresh
concrete sewers." Water research 80 (2015): 30-40.
 According to Lambert, there are five types of corrosion, namely: general corrosion,

pitting corrosion, crevice corrosion, galvanic corrosion, and high temperature corrosion. In

general corrosion, it is a result of the damage on the surface of the metal. Upon close

examination, an “orange peel” effect will be identified, wherein; the individual anodes are

surrounded by the cathodic area. The corrosion is spread evenly, and can produce a great

amount of corrosion product, which may somehow cause a case with aesthetics and

contamination. In addition, another type of corrosion is pitting corrosion. It occurs commonly

due to chlorides, which disarrays the passive oxide film protecting metals. On the other hand,

crevice corrosion happens when differences in the oxygen levels between the crevice and the

exterior of a metal forms a corrosion cell. Furthermore, the relatively small anodic area is run

by the larger external cathode, causing high rates of corrosion. Next, galvanic corrosion takes

place when two dissimilar metals subjected to the same electrolyte, are electrically connected.

Lastly, high-temperature corrosion occurs when metals like steel react with gases like oxygen

or oxides like Sulphur and carbon, which results to loss of metal, bringing about the loss of

metal, and the possibility of the alteration of the mechanical characteristics in the metal

alloy.2

Tangible corrosion is a costly problem in the sewer system industries worldwide.

Corrosion, in the long run gradually affects the structural capacity and leads to collapse of the

structure. In USA alone, approximately $14 billion dollars, the annual economic cost is lost

in sewer assets. This economic cost is expected to gradually increase when deteriorations due

to corrosion continue.13

_________________________
2
Ibid 105-128.
13
Ibid 30-40.
 Important considerations that inhibitors must possess are: its solubility in corrosive

medium, compatibility in corrosive solvent, stability in varying pH levels and temperature,

cost of inhibitor, eco-friendliness, and its efficiency as inhibitor.12

Studies on corrosion have great significance categorized into three aspects, in

economics, safety, and in the conservation of metal resources. Corrosion inhibition

regulations are appropriate to abstain from variety of severe damages like economy loss,

water reservoirs, ecological pollution and human values. Consequently, material engineers

and corrosion scientists aim to prevent and lessen the impacts of corrosion on water

resources, pipelines, machine equipment, bridges and other structural materials so as to

provide its significance on the three categories.12

The effects of corrosion can be detrimental in the industry, such impacts cause

failures in pressure basins, boiler tanks, chemical containers, blades of turbines, or motors,

aero-plane parts, and other automotive devices. Another serious concern of it is the safety of

nuclear power plants in terms of nuclear waste disposal and construction of equipment.

Although corrosion often mars metals, it can also influence water reservoirs, energies, and

manual efforts during the manufacture of metals.12

Corrosion may produce a certain texture on a metal, the texture features may vary for

different types of corrosion damage. They stated texture analysis should relate brightness

parameters of rough surface images to the visual perception characteristics.14

In order to identify corroded objects, the color characteristics should be determined

based on a definite color model. The authors recommended to use the HSI model when

identifying the attributes of color characteristics because it describes color characteristics and

14 12
Ibid 1145-1156.
Choi, Ki-Young, and S. S. Kim. "Morphological analysis and classification of types of surface corrosion
damage by digital image processing." Corrosion Science 47.1 (2005): 1-15.
brightness characteristics separately. It makes use of hue, saturation, intensity and

brightness.14

Color feature analysis, which utilized red(R), green (G) and blue (B) was used as the

primary color features which related to corrosion damage in the study of Pidaparti,

Hinderliter, and Maskey. The study made use of a commercial desktop scanner to identify the

colors at different points. Results of the study showed that as the time increased the R color

value increases while the G and B color values decreased.15

Related Literature on Factors Affecting Corrosion

The condition of the metal surface may affect the corrosion of a metal such as the

possibility of pitting. In addition corrosion is fairly unaffected by the pH of the environment

as long as the pH level is 4-10, but is greatly affected when pH level drops below 4.

Moreover, corrosion is also affected by the oxygen content; corrosion rate normally increases

as the oxygen content increases.16

The atmospheric condition in the corrosion of mild steel is a topic that has been

extensively studied by researchers. Some of the products formed from the exposure of mild

steel to the atmosphere are a group of Fe (II/III) hydroxy salts, commonly detected from

atmospheric corrosion products, such as Hematite (α-Fe2O), Maghemite (γ-Fe2O3), Magnetite

(Fe3O4), Ferrihydrite (Fe5HO8. 4H2O), Ferrous hydroxide (Fe(OH)2), Ferric hydroxide

(Fe(OH)3), Goethite (α-FeOOH), Akageneite (β-FeOOH, Lepidocrocite (γ-FeOOH) and

Feroxyhyte (δ-FeOOH).17

15 14
Ibid 1-15.
Pidaparti, Ramana M., Brian Hinderliter, and Darshan Maskey. "Evaluation of corrosion growth on SS304
based on textural and color features from image analysis." ISRN Corrosion 2013 (2013).
16
Ashworth, V., C. Booker, and H. Charlton. "A short introduction to corrosion and its
control." Corrosion & Protection 1.6 (2011).
17
Morcillo, Manuel, et al. "Atmospheric corrosion of mild steel." (2011)
 Related Studies on Corrosion in Metals

In an attempt to find an alternative to synthetically-made corrosion inhibitor, a study was

carried out by Singh18, by using a plant common to tropical India, the Adhatoda vasica, and by

using aqueous extraction and applying it to the mild steel plate in H 2SO4, the experimentation

showed that the Adhatoda vasica plant’s inhibition efficiency is directly proportional to the

concentration level of the plant and inversely proportional to the temperature of the extract. This

study shows that inhibition efficiency of naturally occurring substance may depend on the

temperature, which is why this current study will only focus on a definite temperature in order to

avert major differences in corrosion inhibition rate. However, in a similar study conducted by

Gunasekaran & Chauhan19 where they exposed the mild steel plates to varying concentration of

phosphoric acid containing 3200 ppm of the plant extract of Zenthoxylum alatum, in the

temperature range of 50-80 degrees Celsius, it showed that inhibition efficiency is almost

constant to a certain temperature, which significantly contradicts the latter’s results which shows

the inverse proportionality of inhibition efficiency to the temperature.

In the study of Suzumura and Nakamura 20, surveys showed corrosion of suspension

bridge cables because of water and high temperature. The wires were normally wet at the sides,

top, bottom and humid at the center. The study made use of galvanized steel wires showing that

the side and bottom wires were corroded while the upper and center wires were barely corroded.

They stated that the galvanized steel wires showed no sign of corrosion when the humidity was

kept below 60%, but started showing signs of corrosion when the humidity was higher than 60%.

The corrosion rate increased along with the amount of sodium chloride and temperature.

18
Singh, M. Ramananda. "A green approach: a corrosion inhibition of mild steel by Adhatoda vasica
plant extract in 0.5 MH 2 SO 4." environments 10 (2013): 19
19
Gunasekaran, G, and L.r Chauhan. “Eco Friendly Inhibitor for Corrosion Inhibition of Mild Steel in
Phosphoric Acid Medium.” Electrochimica Acta, vol. 49, no. 25, 2004, pp. 4387–4395.,
doi:10.1016/j.electacta.2004.04.030.
20
Suzumura, Keita, and Shun-ichi Nakamura. "Environmental factors affecting corrosion of galvanized
steel wires." Journal of materials in civil engineering 16.1 (2004): 1-7.
 Related Literature on Mild Steel

One specific example of a metal most often used, particularly in construction, is the

Mild steel. The carbon content of this alloy, emerging from iron and carbon, is 0.05 to 0.3%.

Furthermore, the advantage of Mild Steel is its ductility. It can be cut, shape, and joined

easily in order to make a variety of products.2

In a study by Osarolube, Owate, and Oforka, results showed that mild steel has a

faster corrosion rate in nitric acid, hydrochloric acid, and perchloric acid solutions when

water, air and hydrogen ions were present. Results also showed that weight loss increased as

the time and concentration increased. The researchers concluded that the carbon in mild steel

had little if any effect to the corrosion resistance of steels as it was higher than the corrosion

resistance of high Mild steel.21

Related Studies on Plants that Inhibit Corrosion

In considering one important factor, several studies have been conducted to find

naturally occurring substances as corrosion inhibitors. The plant extracts of Henna, Oxandra

asbecki, Argemone mexicana, Isertia cocccinea and Palicourea guianensis have been tested

as natural corrosion inhibitors. These inhibitors are significant in terms of its practical use,

and its environment-friendliness.22

The study conducted by Raja et al. shows that the different extracts of N. cadamba

leaves and bark extract, as well as its pure alkaloid, the 3β-isodihydrocadambine

demonstrates high corrosion inhibition through adsorption and the inhibition efficiency was

determined by polarization, electrical impendance, and SEM analysis. These green inhibitors,

as tested in the study, showed to follow the Langmuir adsorption isotherm. The electrical

impendance test showed that the green inhibitors suppressed the corrosion by increasing the
2
21
Ibid 105-128.
Osarolube, E., I. O. Owate, and N. C. Oforka. "Corrosion behaviour of mild and high carbon steels in various
acidic media." Scientific Research and Essay 3.6 (2008): 224-228.
22
Krishnegowda, Pavithra M., et al. "Acalypha torta leaf extract as green corrosion inhibitor for mild
steel in hydrochloric acid solution." Industrial & Engineering Chemistry Research 52.2 (2013): 722-
728.
mild steel’s resistance. The inhibitors also acted as mixed-type of inhibition mechanism as it

was tested in the potentiodynamic polarization study. Also, as recorded in the SEM analysis,

the inhibitors formed a protective layer thus impending the rate of corrosion off the mild steel

plate. This study suggests that by using the different test procedures, like the SEM analysis,

electrical impendance, and polarization studies, it can be concluded that the alkaloids of the

N. ccadamba are potential corrosion inhibitors and that may be useful for industrial

purposes.12

A study was conducted to investigate the effect of Zenthoxylum alatum (Winged

prickly ash) plant extract for the inhibition of Mild Steel corrosion in aqueous Hydrochloric

acid (HCl) solution. The study probe the inhibitive properties of Zenthoxylum alatum

(Winged prickly ash) plant extract for Mild steel corrosion in HCl by examining its weight

loss electrochemical impedance spectroscopy (EIS) at two concentrations namely, 5% and

15%. Adding the plant extract till 2400 ppm makes the corrosion inhibition efficiency also

increases. It is also investigated in the temperature range of 50-80° Con how the temperature

may effect on the corrosion behaviour of the mild steel in two concentrations of HCl

specifically 5% and 15% with the inclusion of the zenthoxylum alatum (Winged prickly ash)

plant extract. In indicating the inhibitive property of the plant extract in HCl solution, the

researchers used the Surface Analysis namely the Scanning electron microscope (SEM),

Electron spectroscopy for chemical analysis (ESCA) and FT-IR studies that uses the KBr

method. The conclusion shows that the zenthoxylum alatum (Winged prickly ash) is effectual

in 5% HCl rather that in 15% HCl since it able to decrease the corrosion of mild steel.4

________________________
4
Ibid 1143-1161.
12
Ibid 1145-1156.
 A study was conducted to investigate the effect of Tagetes erecta (Marigold flower)

plant extract as an inhibitor for Mild Steel corrosion in Sulfuric acid ( H 2 SO4 ) solution. The

study probe the inhibitive properties of Tagetes erecta (Marigold flower) plant extract for

Mild steel corrosion in H 2 SO4 by examining its gravimetric, potentiodynamic polarization

and electrochemical impedance spectroscopy measurements. In gravimetric measurements,

3x4x0.1 cm soaked in 0.5 M ( H 2 SO4 ) for 24 hrs in the absence and presence of 0.1, 0.2, 0.3,

0.5 and 1.0 g L−1 of the inhibitor at 30℃. In potentiodynamic polarization, the polarization

curves were noted from 250 to +250 mV with respect to corrosion potential at a scan rate of

0.5 mV/s. In electrochemical impedance spectroscopy measurements were executed in a

convectional three electrode assembly. In this assembly, it consists of a flat bottom Pyrex

glass flask with three openings each for counter electrodes, reference and working. A

rectangular working electrode of MS with an exposed surface area of 1 cm2 was attached to a

self designed holder and the rest of the surface was covered with lacquer. The platinum wire

and silber-silver chloride electrode (3 M KCl) were used as a counter and reference

electrodes, separately. Using the Tafel polarization, it was known that the Tagetes erecta

(Marigold flower) plant extract acts an effective mixed inhibitor.5

A study was conducted to evaluate the inhibition performance of Aloes (True aloes)

leaf extract on Mild Steel corrosion in 1.0 M Hydrochloric Acid (HCl) through the use of

weight loss methods, potentiodynamic polarization and electrochemical impedance

spectroscopy techniques. It is also investigated on how temperature affect the corrosion

behaviors of mild steel in 1 M HCl with the addition of Aloes (True aloes) leaf extract.

Langmuir adsorption isotherm was used by the researchers in testing the adsorption of the

extract molecules on the mild steel surface with the temperature of 30 ℃. The researchers

________________________
5
Ibid 352-363.
calculated the activation energy and the other thermodynamic parameters for the inhibition

process and it shows that there is a strong interaction between inhibitor and mild steel

calculated the activation energy and the other thermodynamic parameters for the inhibition

process and it shows that there is a strong interaction between inhibitor and mild steel

surface. The results show that if the Aloes (True aloes) leaf extract concentration increases

the inhibition efficiency also increases.6

Psidium guajava (guava) leaf extract on mild steel in 1 M Phosphoric acid ¿ ¿PO4)

was examined in the study using weight loss, potentiodynamic polarization and

electrochemical impedance spectroscopy techniques. The inhibition efficiency increases with

the inhibitor concentration up to 800 ppm and slightly decreased at 1200 ppm. In weight loss,

before doing the experiment the steel coins were polished with six various grades of Silicon

Carbide (SiC) sand paper namely 200, 400, 600, 800, 1000 and 2000. Then it was washed

using the acetone and double distilled water. After the washed coins were dried it was

weighed before soaking into the leaf extract. At the time range of 60 min the steel coins was

observed by the researchers if the inhibitor concentration had an effect on soaking the coin,

including the time of 15 min in which a different inhibitor concentrations was used.

Temperature was also studied if it had a possible effect with and without 800 ppm inhibitor

with a soaking time of 15 min. The steel coins which was soaked in the leaf extract was taken

out, washed and weighed upon drying. With the fix period of time which is one hour was

given for potentiodynamic polarization and electrochemical impedance spectroscopy (EIS). It

was found out that the adsorption follow a comprehensive type of adsorption dominated by

chemisorptions. The potentiodynamic polarization revealed that the Psidium guajava (guava)

leaf extract acted as mixed-type inhibitor. 7

__________________________
6
Ibid720-734.
7
Ibid 2220-2238.
 Another study examined the corrosion inhibitory action of Hibiscus sabdariffa on

Mild steel in acidic bath by corrosion-monitoring techniques with the following

concentrations; 2, 5, 10 and 15g /100ml. Four adsorption isotherms were tested for the data,

namely Langmuir, Frumkin, Florry–Huggins, and Langmuir–Freundlich isotherms. The

inhibition efficiency is calculated from the weight loss experiments performed for Mild steel

in 1.2 N HCl and 1.2 N H2SO4 at temperature of 30 ± 1°C. The leaves were washed with

deionized water and then dried in oven at 80 ± 1°C for a period of one hour. The study

proved that AELHS inhibits corrosion of Mild steel in 1.2 N H2SO4 much better than in 1.2

N HCl environment for a time period of three hours at all inhibitor concentrations.23

Saratha et. al investigated the corrosion inhibition of Citrus aurantiifolia leaves

extract as corrosion inhibitors for Mild steel in 1 M HCl. It was found out that the extract

could be a possible and efficient medium for inhibiting corrosion in mild steel with HCl as a

medium. Additionally, the results showed that the addition of inhibitors increased the

Inhibition efficiency, disregarding the time of immersion which may be due to the adsorption

of the inhibitors on the metal surface.24

Related Literature on Green Corrosion Inhibitors

Over the course of two years, researchers have reviewed relevant and dynamic studies

on natural plant extracts as corrosion inhibitors for mild steel. The adsorption of such natural

inhibitors on surfaces if metal were characterized by several influences like, nature of metal,

testing media, chemical structure and substituent make-up of inhibitors, presence of additives,

solution temperature and concentration. The green inhibitors were mainly subjected to

sulphuric, hydrochloric acid, and in certain case either media, so as to show balanced

representation of reality in the industry, where steels were exposed under such acids. In
23
Murthy, Z. V. P., and K. Vijayaragavan. "Mild steel corrosion inhibition by acid extract of leaves of
Hibiscus sabdariffa as a green corrosion inhibitor and sorption behavior." Green Chemistry Letters and
Reviews 7.3 (2014): 209-219.
24
Saratha, R., S. V. Priya, and P. Thilagavathy. "Investigation of Citrus aurantiifolia leaves extract as
corrosion inhibitor for mild steel in 1 M HCl." Journal of chemistry 6.3 (2009): 785-795.
addition, nitric acid and salt media were also explored but in different cases. The application

of green corrosion inhibitors in industrial seepage by the said research has potential to lead in

a large scale implementation. These naturally occurring-plant extracts submerged to

Hydrochloric acid (HCl) such as Molasses, Pentaclethra macrophylla, Anibarosaeodor,

Adenopusbrevifloru, Cucurbitamaxima, Terminalia chebula, Turmericand ginger rhizomes,

Musa paradisiaca, Pecti, Ligularia fischeri, Phyllanthus amarus, Elaeis guineensis, and Aloe

Vera have shown an increase in inhibition efficiency when tested to the effect concentration.

Findings of the study proved the effectiveness of the abovementioned green inhibitors

through the methods of gravimetric analysis, weight loss, electrochemical impedance, and

potentiodynamic polarization.25

Patni et. al defined corrosion inhibitors as “a substance which, when added in small

concentration to an environment, effectively reduces the corrosion rate of a metal exposed to

that environment”. It can be categorized in two, namely, those that strengthen the generation

of film protecting oxide through an oxidizing effect, and those who inhibit corrosion by

adsorbing selectively on the surface of metals thereby creating a barrier that blocks corrosive

substances from entering the metal’s surface. Additionally, almost all molecules that are

organic contain heteroatoms such as nitrogen, sulphur, phosphorus, and oxygen show

promising inhibition of corrosion. Fortunately, these organic substances are found in plants,

and studies have been made to examine different plant extracts to be used as corrosion

inhibitors. Some of these are tobacco, black pepper, acacia gum, castor seed, and lignin.26

Related Literature on Calamansi (C. microcarpa)

25
Chigondo, Marko, and Fidelis Chigondo. "Recent natural corrosion inhibitors for mild steel: an
overview." Journal of Chemistry 2016 (2016).
26
Patni, N., et al. "Greener Approach Towards Corrosion Inhibition, Greener Approach Towards Corrosion
Inhibition." Chin. J. Eng. Chin. J. Eng 2013 (2013): e784186.
 Some of the physical properties of Citrus microcarpa, or commonly known as

Calamansi, are its moisture content, its mean value of length, width, and thickness, sphericity,

aspect ratio, weight, surface area, volume, true and bulk density, and porosity. The fruit’s

moisture content 84.14 – 85.95%. Its mean value of length, width, and thickness of the fruits

are 26.36, 26.40, 25.26 mm respectively. Additionally, the mean of sphericity and aspect ratio

are 98.87 and 100.23 respectively while its mean mass is 10.007 g. Aside from that, its

surface 2125.07 mm2, and its volume amounted to 8800.00 mm3. True density and bulk

density of the fruits were 1002.87 and 501.70 kgm -3. The fruit’s average porosity produced a

result of 49.89.27

Calamansi (C. microcarpa) is a fruit rich in phenols and flavonones. Some of the

phenols found in the juice of Calamansi (C. microcarpa) are: 9.5% (0.23 mg/g) fl avone/ fl

avonol, 77.4% (1.19 mg/g) fl avanone, 0% psoralen, and 3.7% (0.03 mg/g) coumarin. Among

the flavanones reported to be found in the fruit’s juice are: didymin 3% (traces), eriocitrin 3%

(traces), hesperidin 40% (0.5 mg/g), naringin 50% (0.6 mg/g), naringin–6″–malonate (open

form) 4% (traces mg/g). The percentage and concentration of flavone reported in Citrus

microcarpa were as follows: flavedo: diosmin 6% (0.1 mg/g); juice diosmin 14% (traces).28

Conceptual Framework

27
Abdullah, M.H.R.O., P.E. Ch'ng and N.A. Yunus. "Physical Properties of Musk Lime (Citrus Microcarpa)."
International Journal of Agricultural and Biosystems Engineering 6.12 (2012): 1122-1125. Document.
28
LIM, T. K. EDIBLE MEDICINAL AND NON-MEDICINAL PLANTS: Volume 4, Fruits. SPRINGER, 2016
 The conceptual framework of this study is presented in an input-process-output

model. The input frame presents the corrosion inhibition on Mild steel in hydrochloric acid in

different concentration of Calamansi (C. microcarpa), positive and negative control. The

process frame describes the steps that the researchers would undertake in order to gather data;

which are the measurement and calculation of the corrosion inhibition of Calamansi (C.

microcarpa) fruit extract on Mild steel in muriatic acid (HCl) through gravimetric analysis

and data analysis of the gathered information to determine if there are significant differences

occurring. On the other hand, the output frame shows the implications of the gathered data

and the Corrosion inhibition of Calamansi (C.microcarpa) fruit extract on Mild steel in

Muriatic acid (HCl).

Input Process Output

Corrosion inhibition on Measurement and The Corrosion inhibition of

mild steel in hydrochloric calculation of the Calamansi (C.microcarpa)
acid in different corrosion inhibition of fruit extract on Mild steel in
concentration of calamansi (C. Muriatic acid (HCl).
Calamansi (C. microcarpa) fruit extract
microcarpa), positive and on mild steel in muriatic
negative control. acid (HCl) through
gravimetric analysis.

Data analysis of the

garnered information to
determine if there are
significant differences.

Hypotheses

1. Calamansi (C. microcarpa) fruit extracts have no inhibitive effect on Mild steel

corrosion in Muriatic acid solution.

2. No concentration of Calamansi (C. microcarpa) will have an inhibitory effect on Mild

steel corrosion in Muriatic acid solution.

 3. There is no significant difference between the corrosion inhibition efficiency of the

different concentrations of Calamansi (C. microcarpa) fruit extract on Mild steel in

Muriatic acid.

Definition of Terms
This section provides definition of terms that may be unusual or unfamiliar with the

readers.

The following terms are given in the conceptual and operational forms:

Analytical balances are highly sensitive lab instruments designed to accurately

measure mass. It is the instrument used to measure the mass of Mild steel precisely.

Corrosion inhibition is a decrease in the corrosion rate of a metal. It is the decrease in

corrosion due to the application of the Calamansi (C. microcarpa) on Mild steel.

Corrosion rate is the speed of deterioration of metals when exposed to harsh

environment. It is the rate at which the Mild steel is corroded.

Gravimetric analysis is a technique through which the amount of an analyte (the ion

being analyzed) can be determined through the measurement of mass. A technique in which

the inhibition efficiency is measured through comparing the mass of the Mild steel before and

after the immersion in HCl corrosive medium.

Inhibition efficiency is the effectiveness of the extract in inhibiting Mild steel

corrosion. It is the effectiveness of the Calamansi (C. microcarpa) in inhibiting the corrosion

of Mild steel.

Mild steel is a malleable and ductile type of metal that is prone to corrosion which is

composed of 0.05%-0.25% of carbon and 0.4% Manganese. This type of steel will be

immersed in the hydrochloric acid to observe the corrosion rate.

mmpy is millimeter per year. It is the unit for corrosion rate of Mild steel

Muriatic acid (HCl) is a strong corrosive acid on metals. It is the solution that the

Mild steel will be immersed into.

 Chapter III

METHODOLOGY

A. Research Design

The research design used in this study is the experimental design and was conducted to

determine the corrosion inhibition of Calamansi (C. microcarpa) on mild steel in Muriatic

acid with 29% Hydrogen Chloride (HCl). Five various concentrations 2%, 5%, 7%, 10%, and

15% were used for Calamansi (C. microcarpa) fruit extract and another a 100% of an

Muriatic acid with 29% Hydrogen Chloride (HCl). Five treatments of Calamansi (C.

microcarpa) fruit extract, and an Muriatic acid with 29% Hydrogen Chloride (HCl) content

were administered to three replicates of mild steel for each treatment.

B. The Sample

The variables for this study were selected in accordance with the random sampling

method. The researchers selected a portion from the population of Calamansi (C.

microcarpa), mild steel and Muriatic acid with 29% HCl content that were located in

Tacloban City.

C. Research Instrument

The research instrument used in the study was a checklist. It was utilized to determine

the corrosion inhibition of Calamansi (C. microcarpa) on carbon steel in Muriatic acid with

29% HCl. It contains the possible criteria that can be marked as present and absent, and also

provides space for the comments of the researchers.

 Sample Checklist
2% (v/v)
First replicate
Present Absent Observation
Change in color

Change in Texture

Weight Loss

Second Replicate

Present Absent Observation

Change in color

Change in Texture

Weight Loss

Third Replicate

Present Absent Observation

Change in color

Change in Texture

Weight Loss

5% (v/v)

First replicate

Present Absent Observation

Change in color

Change in Texture

Weight Loss
Second Replicate

Present Absent Observation

Change in color

Change in Texture

Weight Loss

Third Replicate

Present Absent Observation

Change in color

Change in Texture

Weight Loss

7% (v/v)

First replicate

Present Absent Observation

Change in color

Change in Texture

Weight Loss

Second Replicate

Present Absent Observation

Change in color

Change in Texture

Weight Loss

Third Replicate
 Present Absent Observation
Change in color

Change in Texture

Weight Loss

10% (v/v)

First replicate

Present Absent Observation

Change in color

Change in Texture

Weight Loss

Second Replicate

Present Absent Observation

Change in color

Change in Texture

Weight Loss

Third Replicate

Present Absent Observation

Change in color

Change in Texture

Weight Loss

15% (v/v)
First replicate

Present Absent Observation

Change in color

Change in Texture

Weight Loss

Second Replicate

Present Absent Observation

Change in color
Change in Texture
Weight Loss

Third Replicate

Present Absent Observation

Change in color
Change in Texture
Weight Loss

100% Muriatic acid with 29% HCl content.

First replicate

Present Absent Observation

Change in color

Change in Texture

Weight Loss
Second Replicate

Present Absent Observation

Change in color

Change in Texture

Weight Loss

Third Replicate

Present Absent Observation

Change in color

Change in Texture

Weight Loss

D. Research Procedure

A. Collection of Calamansi (Citrus microcarpa) fruit

The fruit of Calamansi (C. microcarpa) was collected in Tacloban City. Fresh, ripe

fruits was garnered and was used for testing. The researchers ensured that the gathered

Calamansi (C. microcarpa) fruits were not overripe or yellowish in color. It was then

brought to the office of the City Agriculturist to be identified.

B. Mild steel preparation

Mild steel bar was obtained locally and confirmed by the Technical Education and

Skills Development Authority (TESDA) Region 8. The steel bar was mechanically cut into

18 pieces using the dimensions 2cm x 2.3cm x 0.3cm (Adapted from: Shivakumar and

Mohana). These pieces of Mild steel bar were degreased with 70% isopropyl alcohol, dried

with clean tissue and stored in an air tight container containing silica gel desiccants.

C. Obtaining HCl solution

 Two thousand (2000) ml of Muriatic acid with 29% Hydrogen Chloride (HCl) content

was obtained around Tacloban City.

D. Preparation of Calamansi (C. microcarpa) fruit extract

200 pieces of Calamansi (C. microcarpa) fruit worth 160 pesos were gathered from

Tacloban City Public Market. The researchers prepared the tools needed for the preparation

of Calamansi (C. microcarpa) fruit extract, knives, chopping boards, funnel, fine strainer,

glass jar and a basin. The 200 pieces Calamansi (C. microcarpa) fruit were washed

thoroughly with running tap water and put it in a basin. Each Calamansi (C. microcarpa) fruit

were sliced with a half inch deep. Afterwards, the researchers manually squeezed the

Calamansi (C. microcarpa) fruit and strained to separate the seed from the juice. The extract

was transferred in to the glass jar using a funnel.

E. Weighing of the Mild Steel

The researchers weighed the Mild steel with an analytical balance.

F. Treatments

These treatments were done inside the fume hood since the researchers dealt

with a highly corrosive chemical content which may cause harmful effects.

I. 2000 ml solution of Muriatic acid was obtained in the experiment.

II. 2% concentration of Calamansi (C. microcarpa) fruit extract and Muriatic acid

with 29% HCl content solution.

98 ml of Muriatic acid with 29% HCl content was added to a beaker

containing 2 ml of of Calamansi (C. microcarpa) fruit extract obtaining a total

volume of 100 ml.

II. 5% concentration of Calamansi (C. microcarpa) fruit extract and HCl solution.
 95 ml of Muriatic acid with 29% HCl content was added to a beaker

containing 5 ml of of Calamansi (C. microcarpa) fruit extract obtaining a total

volume of 100 ml.

III. 7% concentration of Calamansi (C. microcarpa) fruit extract and HCl solution.

93 ml of Muriatic acid with 29% HCl content was added to a beaker

containing 7 ml of of Calamansi (C. microcarpa) fruit extract obtaining a total

volume of 100 ml.

IV. 10% concentration of Calamansi (C. microcarpa) fruit extract and HCl solution.

90 ml of Muriatic acid with 29% HCl content was added to a beaker

containing 10 ml of of Calamansi (C. microcarpa) fruit extract obtaining a

total volume of 100 ml.

V. 15% concentration of Calamansi (C. microcarpa) fruit extract and HCl

solution.

85 ml of Muriatic acid with 29% HCl content was added to a beaker

containing 15 ml of of Calamansi (C. microcarpa) fruit extract obtaining a

total volume of 100 ml.

VI. 100% Muriatic acid with 29% HCl content.

100 ml of Muriatic acid with 29% HCl content obtaining a total volume of 100

ml.

G. Application of Treatments

18 pieces of mild steel were exposed to the treatments. The carbon steel was

divided into five groups; with three mild steel for each group, and according to the

treatment they were exposed to. For each concentration, three replicates of mild steel

were immersed simultaneously with one-minute interval for varying concentration.

Using the analytical balance, the mild steel bars were initially weighed before
 immersing it in the solution for 16 hours (Adapted from; Nnanna, Nnanna and

Nakaife). After the immersion period, the mild steel bars were removed from the

concentrations simultaneously. Then the mild steel bars were placed in petri dish.

H. Neutralizing the Muriatic Acid

A. Preparing Phenolphthalein solution with ethanol

The phenolphthalein powder was measured in the analytical balance with a

watch glass having a weigh of 0.506 g and 120 ml of ethanol measured through a

graduated cylinder. Then the solution was mixed together in a giant graduated

cylinder. The phenolphthalein solutions served as an indicator if the solution is basic.

B. Diluting the Solutions

The researchers prepared water in a 1000 ml beaker. Slowly poured the

solution in to the water while checking the temperature in order to prevent the

concentrations from heating up. Two molars of sodium hydroxide (NaOH) was added

to the diluted solution. Then, with enough amount of the indicator, the

phenolphthalein solution was poured to the diluted solution. Immediately after

pouring, the diluted solution turned pink, in which it indicates that the solution is

already basic and ready to be disposed.

I. Gravimetric Technique

With the gravimetric measurements, the corrosion rate of each concentration was

calculated using the formula:

∆ mx 87.6
CR = where CR is the corrosion rate (mmpy) of mild steel bar, ∆ m is the
DSt

mass loss (g), D is the density of Mild steel (g/cm 3), S is the surface area of the specimen

(cm2), t is the immersion period (h) and 87.6 is a conversion factor. (Adapted from; Sharma,

Mudhoo and Jain)

 The inhibition efficiency was calculated using the equation;

CR (a)−CR ( p)
IE(%)= x 100 , where IE is the inhibition efficiency of Calamansi (C.
CR(a)

microcarpa) fruit extract, CRa and CRp are the corrosion rates of mild steel in the absence

and presence of the inhibitor in different concentrations. (Adapted from: Shivakumar and

Mohana)

E. Plan for Data Analysis

The means of corrosion rate and inhibition efficiency was compared. Results were

analyzed using Analysis of Variance (ANOVA) test to determine if there is a significant

difference between the inhibition efficiency of Calamansi (C. microcarpa) fruit extract in

different concentrations and Scheffé test was calculated to locate where the significant

differences lie.
 Chapter IV

RESULTS AND DISCUSSIONS

Reconceptualized Framework

The reconceptualized framework of this study, which is based on the results, is

presented in an input-process-output model. The input frame presents the inhibition

efficiencies and corrosion rates on Mild steel in hydrochloric acid of the different

concentration of Calamansi (C. microcarpa) and the negative control. The process frame

describes the steps that the researchers had undertaken in order to validate the data, utilizing

data analysis with One-Way Analysis of Variance (ANOVA), and the Scheffe’ test. On the

other hand, the output frame shows the implications of the gathered data, showing that the

Calamansi (C. microcarpa) fruit extract inhibits the corrosion of mild steel in Muriatic acid

(HCl).

Input Process Output

Inhibition efficiencies
and corrosion rates on Data analysis with One- Calamansi (C. microcarpa)
Mild steel in Muriatic Way Analysis of Variance fruit extract inhibits the
acid of the different (ANOVA), and the corrosion of mild steel in
concentration of Scheffe’ test Muriatic acid (HCl)
Calamansi (C.
microcarpa) and the
negative control
Table 1. Mean Corrosion Rate of Mild steel in all replicates.

Concentrations of Calamansi (C. microcarpa) Fruit Extracts and Muriatic acid

Muriatic acid
Corrosion 2% v/v 5% v/v 7% v/v 10% v/v 15% v/v
Solution
Rates
(mmpy) of 347.40 219.47 163.24 158.00 127.14 104.61
Mild steel mmpy mmpy mmpy mmpy mmpy mmpy

As observed in the table, the corrosion rate of mild steel decreases as the

concentration of the fruit extract increases. There is an inverse relationship between the two

variables: the concentration of the fruit extract and the corrosion rate of Mild steel. The

corrosion rate of the Mild steel is dependent on the concentration of fruit extract and the

Muriatic acid. As the Mild steel was submerged in the Calamansi (C. microcarpa) fruit

extract solutions with lower concentrations, the more weight was lost due to the exposure to

the Muriatic acid. This validates the claims of Murthy and Vijayaragavan that the corrosion

rate of a substance to a metal increases with an addition to the inhibitor concentration for the

acidic media.
Table 2. Mean Inhibition Efficiency of the Different Concentration of Calamansi (C.
microcarpa) Extract in Muriatic Acid on Mild steel Corrosion

Inhibition Efficiency of the Different Concentration of Calamansi (C. microcarpa) Extract

in Muriatic Acid on Mild steel Corrosion
2% v/v 5% v/v 7% v/v 10% v/v 15% v/v
Inhibition
Efficiency % 36.825 53.010% 54.519% 63.402% 69.888%

From the data shown above, this implies that the Inhibition efficiency of the

Calamansi (C. microcarpa) increases as its concentration increases. This signifies that the

inhibition efficiency is dependent on the concentration of Calamansi (C. microcarpa) and the

acidic media which supports the claim the study of Murthy and Vijarayagavan. Aside from

that, it correlates with the findings of Saratha et. al, showing that the addition of inhibitors

increased the inhibition efficiency, which may be due to the adsorption of the phytochemical

components of the plant extract on the surface of the metal.

Table 3.Analysis of Variance for the Significant Differences between the Inhibition
Efficiency of the Different Concentrations of Calamansi (C. microcarpa) Fruit Extract and
Muriatic Acid
Source of SS df MS F P-value F crit
Variation
Between 1876.032978 4 469.008244 68.2401010 3.213-E07 3.478-
Groups 5 1 49691
Within Groups 68.72912519 10 6.87291251
9
Total 1944.762103 14        

Table 3 exhibits that there is a significant difference between the inhibition efficiency

of the different concentrations of Calamansi (C.microcarpa) fruit extract and the Muriatic

acid. The null hypothesis is rejected because the calculated P-value is less than the alpha level
(α), and the F-value is greater than the F critical value, thus, there are significant differences

occurring between groups.

Table 4. Scheffe test on the Inhibition efficiency of the different concentrations of Calamansi
(C. microcarpa) Fruit Extract on Muriatic acid

Concentration of Calamansi fruit extract Scheffe crit. Scheffe stat. Results

2% vs 5% 57.175 Significant
2% vs 7% 68.328 Significant
2% vs 10% 154.15 Significant
2% vs 15% 238.57 Significant
5% vs 7% 0.49655 Not significant
13.912
5% vs 10% 23.566 Significant
5% vs 15% 62.162 Significant
7% vs 10% 17.220 Significant
7% vs 15% 51.547 Significant
10% vs 15% 9.1799 Not significant

Table 4 shows the comparison between the Inhibition efficiency of each treatment.

The five concentrations of Calamansi (C. microcarpa) fruit extract (2%, 5%, 7%, 10%, and

15%) were efficient in inhibiting corrosion than the Muriatic acid solution without the fruit

extract. In terms of inhibition efficiency, the results show that there are significant differences

occurring between the different concentrations of Calamansi (C. microcarpa) fruit extract

except for the 5% vs. 7% and 10% vs. 15% concentrations.

 Chapter V

SUMMARY, CONCLUSION, AND RECOMMENDATIONS

SUMMARY

The researchers assessed the corrosion inhibition efficiency of Calamansi (C.

microcarpa) leaf extracts on Mild steel corrosion in Muriatic acid. From the five

concentrations: namely, 2%, 5%, 7%, 10%, and 15%, the study aimed to distinguish which of

the following concentration can effectively inhibit Mild steel corrosion by Gravimetric

Technique (Weight Loss Method). Based on the conducted experiment the following findings

were observed:

1. The Industrialized Muriatic solution without the fruit extract has exhibited the highest

mean of corrosion rate (347.40 mmpy) whereas the 15% concentration of leaf extract

has yielded the least mean for corrosion rate (104.61 mmpy).

2. The 15% concentration of the fruit extract and HCl solution revealed the highest mean

for inhibition efficiency with 69.888%.

3. The difference between the inhibition efficiency of the different concentrations of rice

ethanol leaf extract on mild steel corrosion was found significant obtaining a p value

of 3.21 x 10-7.

4. Based on the Scheffe test, significant differences occur between the Inhibition

efficiency of the different Calamansi (C. microcarpa) concentrations except for 5%

and 7%, and 10% and 15%.

CONCLUSION

1. Calamansi (C. microcarpa) fruit extract has the ability to inhibit corrosion on Mild

steel in Muriatic acid solution.

2. The 15% v/v concentration showed the highest inhibition efficiency among the different

concentrations of Calamansi (C. microcarpa) fruit extract

3. There is a significant difference between the inhibition efficiency of the different

concentrations of Calamansi (C. microcarpa).

RECOMMENDATIONS

1. It was concluded from the study that the Calamansi (C. microcarpa) fruit extract can

inhibit corrosion on Mild steel in Muriatic acid solution, with the said results, it is

highly recommended to use the said fruit extract as green corrosion inhibitor for they

are biodegradable, ecofriendly and non-toxic.

2. For further investigation, it is recommended to isolate and confirm the active

phytochemicals present in Calamansi (C. microcarpa) fruit extract that inhibits Mild

steel corrosion.

3. It is recommended for further research to assess the behavior of Mild steel in Muriatic

acid by potentiodynamic polarization.

4. It is highly recommended for future researchers to analyze the morphology of Mild

steel surface in Muriatic acid in the presence and absence of Calamansi (C.

microcarpa) fruit extract using Scanning electron microscopy (SEM).

5. Also, it is suggested to examine the inhibition efficiency of Calamansi (C.

microcarpa) fruit extract at various temperatures, different immersion periods and at

larger concentrations.

6. For further research, it is recommended to use other extraction process and equipment

for efficient and potent production of the different concentrations of the Calamansi

(C. microcarpa) fruit extract.

7. For future researchers, it is advisable to administer a study on the inhibition efficiency

of a different plant extract, a different metal and a different corrosive medium.

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