1.

Introduction
1.1. Personal Engagement
While on a service trip to the rural and slum areas in India in the monsoon season, I noticed
that most of the houses were being flooded from within due to the leakage of rainwater
through the roofs. The roofs were mostly made of steel as they were cheap and easy to
obtain, and hence was the primary option for most of the residents who were stuck in
poverty. Hence, prolonged exposure to rain led to the corrosion of the iron in the steel and in
turn holes were formed on the surface, leading to the leakage. Owing to their poverty, most
of the residents were unable to change their roofs and in turn, used buckets to collect this
rainwater. This proved to be ineffective and inefficient, as seen through the frequent flooding
from within. As such, I had hoped to find a viable, easily accessible and eco-friendly solution
to this problem.

Since replacement of the steel was not a viable option, the use of corrosion inhibitors was
the only feasible option. Upon further research, I had found that chemical corrosion inhibitors
were not in use due to their toxicity and also was not a cheap resource that could be easily
accessible to these people. Hence, I looked into green inhibitors, and learnt that Moringa
oleifera, was known for its corrosion inhibitive properties. Since it is cultivated in India, it is
highly accessible and is cheap to attain. This then led me to my interest in investigating the
effectiveness of Moringa oleifera extracts at inhibiting corrosion.

2. Background Information
2.1. Steel
Steel, an alloy of primarily constituting carbon and iron, contains trace amounts of
manganese, sulfur and oxygen. It is one of the world’s most sought after material, for uses in
industries such as engineering and construction. Steel is primarily produced in 2 ways: the
blast furnace-basic oxygen furnace (BF-BOF) method and electric arc furnace (EAF)
method. Most of the steel for commercial use is produced using the BF-BOF method,
whereby iron ores are reduced to form iron, which is then converted to steel in the BOF. The
steel is then cast, rolled, and is formed into coils, plates, sections and bars. Steel is
produced from recycled steel in the EAF method, using electricity. The chemical composition
of the steel formed us altered using alloys as additives. Steel has more than 3500 different
grades with a myriad of chemical and physical properties.1

2.1.1. Mild steel

Mild steel falls under ”low-carbon steel”, which is a group of steel with low amounts of
carbon. The carbon content in the steel is highly dependent on the source of production and
the amount of carbon found in mild steel ranges between 0.05% and 0.25% by weight,
whereas high-carbon steel contains approximately 0.30-2.0% carbon, by weight. Mild steel is
not an alloy steel, and hence, other alloying elements such as chromium and molybdenum
are not present. Owing to the low carbon content, mild steel is typically more ductile,
machinable and weldable. At the same time, it is almost impossible to harden and
strengthen through heating and quenching. Due to the low carbon content, mild steel
generally has very little carbon and other alloying elements to block dislocations in its crystal
structure, resulting in less tensile strength, as compared to high carbon and alloy steels. Mild
steel contains a large amount of iron and ferrite, making it magnetic. The presence of little to
no allying elements that are commonly found in stainless steel, makes the iron in mild steel
more susceptible to corrosion.2

1
About Steel(n.d.). Retrieved August 8, 2019, from https://www.worldsteel.org/about-steel.html.
2
What is Mild Steel? (2019, March 14). Retrieved August 8, 2019, from
https://www.metalsupermarkets.com/what-is-mild-steel/.
 2.2. Corrosion

Corrosion refers to the deterioration of a metal, due to the chemical reactions between the
metal and its surrounding environment, in particular the gases. Most metals can corrode,
some at a faster rate than others. Noble Metals are metals that can be found in nature in
their pure form, i.e. do not occur in ores, and this is because they are much less reactive and
hence almost never corrode. These metals include rhodium, palladium, silver, platinum and
gold.3

2.2.1. Processes Involved in Corrosion

When a metal such as iron comes in contact with water in the presence of atmospheric
oxygen, corrosion occurs. The overall reaction, when the iron in steel undergoes corrosion is
as follows:

4Fe2+ + 2H2O + 3O2  4FeO(OH)

FeO(OH) forms the rust-red deposits that are typical of iron corrosion. However, the
corrosion of iron is in actuality a series of separate reactions occurring at different places on
the surface of the metal.

In some areas, iron, Fe, is oxidised to form iron (II) ions, Fe2+, and the excess electrons
produced enter the metal, this is an anodic reaction, that occurs in the anodic region. This
reaction is then summarised according to the following equation:

Fe  Fe2+ + 2e-

In other areas, known as the cathodic region, where oxygen will be reduced by accepting
electrons from the metal, in the presence of water to form hydroxide ions, in the cathodic
reaction. This reaction can be summarised according to the following equation:

O2 + 2H2O + 4e-  4OH-

The above reaction is the atmospheric cathodic reaction but for the experiment, the chemical
cathodic reaction will considered, wherein hydrogen ions are reduced to evolve hydrogen
gas, according to the following equation:

2H+ + 2e-  H2

So as to maintain charge neutrality, both the anodic and cathodic reactions occur at the
same rate, i.e. the number of moles of electrons consumed and produced have to be the
same. Additionally, at the cathodic regions, anions are produced, while at the anodic regions
cations are produced and to maintain net neutrality, there must be a net diffusion of cations
to the cathodic regions and anions to the anodic regions. This diffusion occurs readily in
solutions with high ionic conductivity, as such, corrosion usually occurs more readily in salt
water than in freshwater.4

2.2.2. Types of Corrosion

3
Bell, T. (2019, May 16) How and Why do Metals Corrode? Retrieved August 8, 2019, from
https://www.thebalance.com/what-is-corrosion-2339700
4
North, N.A., &Mac Leod, I.D. (1987). Corrosion of metals. Corrosion of Marine Archaeological
Objects, 68-98. Retrieved August 8, 2019 from
https://www.researchgate.net/publication/300945553_Corrosion_of_metals
There are eight forms of corrosion and they are as follows:

2.2.2.1. Uniform Attack

This is the most common type of corrosion, and is characterised by chemical or electro-
chemical reactions that occur uniformly over the entire exposed surface. As corrosion
increases, the metal becomes thinner and eventually fails. This is not too much of a threat
from a technical standpoint as the life of the metal used can be determined.

2.2.2.2. Intergranular Corrosion

Intergranular corrosion consists of selective or localised attack at the boundaries of the

metallic crystals, leading to the entire grain to be loosened and fall away. Complete
disintegration of the metal may occur even if only a small portion of the metal corrodes on a
weight loss basis. Chromium-nickel stainless steel are particularly susceptible to
intergranular corrosion. Intergranular corrosion is temperature dependent, with the rate of
corrosion increasing with temperature, until the metal is melted.

2.2.2.3. Pitting
Pitting is known to be the most destructive type of corrosion, wherein the corrosion cannot
be determined using experimental methods as the life of the metal is uncertain. However,
pitting can be easily recognised with most of the surface shows no attack, and the corrosion
is occurs only in isolated areas. Halogens are typically considered pitting agents. 5

2.2.2.4. Galvanic Corrosion

Galvanic corrosion occurs when two or more dissimilar metals are brought into electrical
contact under water. When a galvanic couple forms, one of the metals in becomes the
anode and the other becomes the cathode.6

2.2.2.5. Concentration Cell Corrosion

Concentration cell corrosion is the deterioration of portions of a metal surface at different

rates due to the surface coming into contact with different concentrations of the same
electrolyte. The differing concentrations result in some parts of the metal acquiring different
electric potentials. The degree of this type of corrosion is directly proportionate to the
difference in concentrations at the respective contact points, and also varies with the type of
electrolyte. The part of the metal corrodes faster when the electrolyte closer to the metals
shows a lowered concentration of metal ions, causing the region to turn anodic.
Concentration cell corrosion is most prevalent in the presence of oxygen. While corrosion is
enabled when the metal surface comes in contact with oxygen, it is most severe when there
is minimal contact with oxygen.7

5
Fontana, M.G., & Mitra, M.S. (n.d.). THE EIGHT FORMS OF CORROSION AND CORRECTIVE
MEASURES. The Eight Forms of Corrosion and Corrective Measures. Retrieved August 8, 2019 from
http://eprints.nmlindia.org/3414/1/137-148.PDF
6
Dexter, S.C.(n.d.). Galvanic Corrosion Caused by Corrosion Products. Galvanic Corrosion.
Retrieved August 8, 2019, from
https://www.researchgate.net/publication/26990121_Galvanic_Corrosion/link/
0deec52ba181638117000000/download
7
What is Concentration Cell Corrosion? (n.d.). Retrieved August 8, 2019, from
https://www.corrosionpedia.com/definition/310/concentration-cell-corrosion
 2.2.2.6. Dezincification

Dezincification is a type of corrosion in which an alloy containing zinc is de-alloyed, with the
zinc being removed, via selective leaching. Brass is an zinc-containing alloy that undergoes
dezincification under the presence of sparse amounts of water under stagnant conditions.8

2.2.2.7. Erosion-Corrosion

Erosion corrosion is a result of a high velocity between the corrosive environment and the
surface. Erosive corrosion produces a distinctive surface finish, wherein there are grooves,
waves, gullies and holes on the surface of the metal, with respect to the pattern of the fluid
flow. While most metals and alloys are susceptible to erosion corrosion, metals that rely on
surface film for protection against corrosion are particularly vulnerable. 9

2.2.2.8. Stress-Corrosion Cracking

Stress-corrosion cracking (SCC) occurs by slow, environmentally induced crack propagation,

as a result of combined and synergistic interaction of mechanical stress and corrosion
reactions. Environments that result in SCC are usually aqueous and can be either
condensed layers of moisture or bulk solution. In addition, SCC is alloy and environment
specific, that is, it is frequently the result of a specific chemical species in the environment. 10

2.3. Corrosion Inhibitors

Corrosion inhibitors are substances or mixtures that in low concentration and aggressive
environment inhibit, prevent or minimise corrosion.11

2.3.1. Mechanisms of Corrosion Inhibitors

Generally, the mechanism of corrosion inhibitors is one or more of the three that are cited
below:
- the inhibitor is chemically adsorbed on the surface of the metal and forms a
protective layer with inhibitor effect or by combination between inhibitor ions and
metallic surface
- the inhibitor leads a formation of a film by oxide protection of the base metal
- the inhibitor reacts with a potential corrosive component present in aqueous media
and the product is a complex.12

2.4. Moringa oleifera

Moringa oleifera is a small medium seized tree that is vastly cultivated in South Asian
regions, and is a rich source of nutrients and bioactive materials. It is used in curing ailments
due to its antibiotic, anti-hypertensive, anti-spasmodic, antiulcer, anti-inflammatory, anti-

8
Ahmad, Z. (2006) Types of Corrosion. Principles of Corrosion Engineering and Corrosion Control.
Retrieved August 8, 2019 from https://www.sciencedirect.com/topics/materials-science/dezincification
9
Lister, D.H. (n.d.) Erosion Corrosion. Corrosion for Engineers. Retrieved August 8, 2019, from
https://canteach.candu.org/Content Library/20053210.pdf
10
Jones. R.H. & Ricker. R.E. (n.d.) Mechanisms of Stress-Corrosion Cracking. Retrieved August 8,
2019 from https://canteach.candu.org/Content Library/20053210.pdf
11
Obot. I.B., Obi-Egbedi & Umoren. S.A. (2009) Antifungal drugs as corrosion inhibitors for aluminium
in 0.1M HCl from https://www.sciencedirect.com/science/article/pii/S0010938X09002121
12
Dariva. C.G. & Galio. A.F.(2014) Corrosion Inhibitors – Principles, Mechanisms and Applications.
Retrieved August 8, 2019 from
https://pdfs.semanticscholar.org/91db/8b9a33cef82560650c8740dfa152c4b1ed71.pdf
asthmatic, hypocholesterolemic and hypoglycaemic properties.13 Moringa oleifera extracts
are considered green inhibitors, that contain alkaloids, tannins and flavonoids and other
active agents, which contribute to their inhibitory properties. Moringa oleifera is especially
effective at corrosion inhibition as ascertained by multiple studies. It is an inhibitor that forms
a protective layer with inhibitive properties on the surface of the metal.

3. Research Question
My research question is as follows:

What is the effect of varying concentrations of ethanolic extracts(0.2, 0.4, 0.6, 0.8 and 1.0
g/L) from Moringa oleifera leaves on inhibition of corrosion of mild steel in 2M hydrochloric
acid (HCl), determined using gasometric and gravimetric methods?

3.1. Hypothesis
The higher the concentration of Moringa oleifera(MO) extracts, the greater the inhibition
efficiency. As such, as the concentration of MO extract increases, the amount of hydrogen
gas evolved decreases and the amount of weight loss recorded decreases.

4. Methodology
4.1. Variables
Type of Variable Name of Variable Description/Significance
Independent variable Concentration of MO Leaves of Moringa
extract oleifera (MO) were
washed, cut into pieces,
then dried and
pulverised.14 Stock
solutions of the leaves
were prepared by soaking
200 g of the powder in
500 cm3 of ethanol. The
resultant solution is kept
for 24 hours and filtered.
The resulting solution was
then subject to
evaporation at room
temperature to obtain the
extract without ethanol.
The inhibition test
solutions were prepared
from the extract 0.1g,
0.2g, 0.3g, 0.4g and 0.5g
in 500 cm3 of 2M
hydrochloric acid (HCl).15
Each test solution was
250 cm3 of the solution
13
Singh. Y. & Prasad. K.
14
Odiongeyi. A.O., Odoemelam. S.A. & Eddy. N.O.(2008, December 4). Corrosion Inhibition and
Adsorption Properties of Ethanol Extract of Vernonia Amygdalina for the Corrosion of Mild Steel in
H2SO4. Retrieved August 8, 2019 from
http://www.peacta.org/articles_upload/PEA_27_1_2009_33_45.pdf
15
Odusote. J.K., Owalude. D.O., Olusegun. S.J.&Yahya. R.A.(2015, December 15) Inhibition
Efficiency of Moringa Oleifera Leaf Extract on the Corrosion of Reinforced Steel Bar in HCL Solution.
Retrieved 8 August from https://sta.uwi.edu/eng/wije/documents/WIJE_v38n2_Jan2016Completed.pdf
- page=66
 prepared.

A control test was

conducted with 0g/L of
MO extract, where the
steel sample was
immersed in 250 cm3 of
HCl.
Dependent variables Weight loss from steel When the corroded steel
due to the removal of rust is immersed in NaOH and
Zn solution after each 24h
period, the iron(III)
hydroxide is removed,
leaving behind only the
un-corroded steel. As
such the loss in mass (as
compared to the initial
mass) indicates the
inhibition of corrosion.
Wherein, the lesser the
decrease in mass, the
greater the efficiency of
corrosion.
Volume of hydrogen gas Hydrogen gas is evolved
evolved from the cathodic
reaction. The total volume
of hydrogen evolved at
the end of the 3 hour
interval will indicate the
amount of corrosion that
the metal has undergone,
and as the concentration
of MO extract increases,
the total volume of H2
evolved decreases.
Control variables Maintenance of set up Since corrosion is
temperature dependent,
to ensure that only the
effect of increasing
concentration of MO
extract was being
measured, the
experiment was
conducted at 30°C.
Volume of HCl used As mentioned earlier,
halides are corrosion
agents, and increasing
volume or concentration
of HCl used will
accelerate the corrosion
of the iron, and to ensure
that a fair test was
conducted, only 250cm3
of 2M HCl was used in
 each trial.
Duration of contact with The set-up was allowed
solution to set for 72 hours, after
adding the steel, with the
corroded steel being
washed in a solution of
zinc and NaOH every
24h.
Initial mass of steel The initial mass of the
steel has to be kept
constant to measure the
weight loss due to the
removal of the rust.
Type of steel used The type of steel has to
be kept constant so as to
ensure that the iron
content is consistent, as
well as to attain
consistent volumes of
hydrogen gas.
Volume of NaOH and Zn NaOH and Zn are used to
used remove the rust formed
on the steel.

4.2. Chemicals and Apparatus Used

Apparatus Uncertainty Quantity Purpose
Conical flask - 5 To immerse steel
sample in test
solution and
prepare test
solution
Filter funnel - 1 To filter the stock
solution
Electronic ±0.001 g 1 To weigh the steel
weighing scale sample as well as
the MO powder
Gas syringe (100 ±1 cm3 5 To measure the
cm3) volume of H2
evolved
Measuring cylinder ±5 cm3 2 To measure
(500 cm3) volumes of ethanol
and HCl
Steel - 150 g To prepare steel
samples for test
Volumetric flask - 1 To prepare stock
(500 cm3) solution
Weighing bottle - 2 To measure the
change in mass of
the steel sample

Chemical used Chemical formula Purpose

Deionised water H2O To dilute stock solution to
prepare test solutions
Ethanol C2H5OH To prepare stock solution
 Hydrochloric acid HCl To immerse the steel
sample in
Sodium hydroxide NaOH To remove the rust on the
steel to measure the
weight loss

4.3. Methodology
4.3.1. Preparing Steel Sample
Mild steel of composition (wt.%) Mn (0.6), P (0.36), C (0.15), S (0.07) and Fe (98.79) was
used for the study. The sheet was mechanically press-cut to form different coupons, each of
dimension, 5x4x0.3 cm. Each coupon was degreased by washing with ethanol. 16

4.3.2. Extraction of Moringa oleifera

Leaves of Moringa oleifera (MO) were washed, cut into pieces, then dried and pulverised.17
Stock solutions of the leaves were prepared by soaking 200 g of the powder in 500 cm3 of
ethanol. The resultant solution is kept for 24 hours and vacuum filtered. The ethanol is then
removed by using the rotary evaporator. The residue will be the MO extract that will be used
in the experiment

4.3.3. Gasometric Method

The gasometric technique is based on the principle that corrosion reactions in aqueous
acidic media are characterised by the evolution of gas due to the cathodic reaction of the
corrosion process, and the rate at which the gas is evolved is directly proportional to the rate
of corrosion. The gasometric analysis was conducted at 30°C for 3h. The rate of evolution of
the gas (RH) is determined from the slope of the graph of volume of gas evolved (V) versus
time (t) and the degree of surface coverage (θ) and hence inhibition efficiency (η%)
determined using equations (1) and (2), respectively.

θ = (1 – RHi/ RHo). (1)

η% = θ x 100 (2)

where RHo and RHi are the rates of hydrogen evolution in the absence and presence of the
inhibiting molecules, respectively. Results obtained using the gasometric technique have
been corroborated by other well established corrosion rate determination techniques,
including weight loss, thermometric and electrochemical techniques.18
16
Odiongeyi. A.O., Odoemelam. S.A. & Eddy. N.O.(2008, December 4). Corrosion Inhibition and
Adsorption Properties of Ethanol Extract of Vernonia Amygdalina for the Corrosion of Mild Steel in
H2SO4. Retrieved August 8, 2019 from
http://www.peacta.org/articles_upload/PEA_27_1_2009_33_45.pdf
17
Odiongeyi. A.O., Odoemelam. S.A. & Eddy. N.O.(2008, December 4). Corrosion Inhibition and
Adsorption Properties of Ethanol Extract of Vernonia Amygdalina for the Corrosion of Mild Steel in
H2SO4. Retrieved August 8, 2019 from
http://www.peacta.org/articles_upload/PEA_27_1_2009_33_45.pdf
18
Ulaeto S.B., Ekpe U.J., Chdiebere. M.A., & Oguzie. E.E.(2012) Corrosion Inhibition of Mild Steel in
Hydrochloric Acid by Acid Extracts of Eichhornia
Crassipes.https://pdfs.semanticscholar.org/9613/2c5e65fb6fb32dc5ad955261cebf58f9f464.pdf
 4.3.4. Gravimetric Analysis

In gravimetric experiment, a previously weighed metal (mild steel) coupon was completely
immersed in 250 mL of the test solution, in an conical flask. The beaker was inserted into a
water bath maintained at a temperature of 30 °C. After every 24 hours, each sample was
withdrawn from the test solution, washed in a solution containing 50% NaOH and 100 g/L of
zinc dust. The washed sample was dried with acetone before re-weighing. The difference in
weight for a period of 72 h was taken as total weight loss. From the weight loss results, the
inhibition efficiency (I%) of the inhibitor and degree of surface coverage were calculated
using Equations 6 and 7, respectively,

I% = (1 – W1/W2) x 100 (5)

θ = 1 - W1/W2 (6)

where W1 and W2 are the weight losses (g/dm3 ) for mild steel in the presence and absence
of the inhibitor in HCl solution, respectively, and θ is the degree of surface coverage of the
inhibitor.19

4.3.5. UV-Vis Analysis

4.3.5.1. Preparing Ferrous Chloride Stock Solution
.
1.2675g of FeCl2 xH2O crystals was measured out using the electronic weighing balance.
This mass of ferrous chloride was then dissolved in 50 cm3 of deionised water, with constant
stirring. This solution was then transferred into a 100 cm3 volumetric flask, and was topped
up with deionised water until the 100 cm3 mark was reached. The concentration of the
resultant solution is 0.1M.
4.3.5.2. Obtaining the Calibration Curve
Samples containing five different concentrations of FeCl2 were prepared by diluting the 0.1M
solution using different volumes of the stock solution and different volumes of deionised
water. The following table shows the volumes and concentrations of the samples used for
obtaining the calibration curve.

Concentration Volume of stock Volume of Total volume of

of in sample /M solution used / deionised water sample / cm3
cm3 used / cm3
0000 0 10 10
0.02 2 8 10
0.04 4 6 10
0.06 6 4 10
0.08 8 2 10
0.10 10 0 10

5. Results
5.1. Gasometric Analysis

Interval (min)

19
Odiongeyi. A.O., Odoemelam. S.A. & Eddy. N.O.(2008 December 4). Corrosion Inhibition and
Adsorption Properties of Ethanol Extract of Vernonia Amygdalina for the Corrosion of Mild Steel in
H2SO4. Retrieved August 8, 2019 from
http://www.peacta.org/articles_upload/PEA_27_1_2009_33_45.pdf
 Concentration Trial 0 20 40 60 80 100 120 140 160 180
of MO extract
(g/L)
0 1 0 0.2 0.6 1.4 2.6 3.7 4.6 5.4 6.2 6.8
2 0 0.3 0.7 1.1 2.7 3.9 5.1 5.8 6.4 6.9
3 0 0.2 0.5 1.2 2.7 3.8 4.9 5.6 6.1 6.6
4 0 0.4 0.8 1.1 2.5 4.0 4.5 5.9 6.0 6.4
5 0 0.3 0.6 1.2 2.8 3.7 5.0 5.5 6.2 7.0

5.2. Gravimetric Analysis

Concentration of MO Trial Initial Mass (g) Final Mass(g) Mass Lost (g)
Extract (g/L)
0 1 23.52 23.14 0.38
2 23.53 22.90 0.63
3 23.54 23.08 0.46
4 23.55 23.05 0.50
5 23.55 23.01 0.54

Follow-up

I initially tried to extract the ethanolic extracts by letting the solution sit at room temperature
for 24h, but it did not work, so I am going to extract it using a rotary evaporator after soaking
the solution for 24h. Moreover, I tried using the UV-Vis to measure the absorbance of the
resultant solution after 3h and it had an absorbance of 0.133 A with the lambda max value
being 313 nm (according to lit value), so I will be trying to do a UV-Vis analysis along with
the gasometric and gravimetric analysis.