Corrosion Inhibitors

Chapter I Introduction to corrosion and corrosion inhibitors
INTRODUCTION TO CORROSION AND CORROSION INHIBITORS

SECTION - I: CORROSION
1.1.1. Introduction
Corrosion is the destructive attack of a material by reaction with its environment.
The serious consequences of the corrosion process have become a problem of
worldwide significance. In addition to our everyday encounters with this form of
degradation, corrosion causes plant shutdown, waste of valuable resources, loss or
contamination of product, reduction in efficiency, costly maintenance and expensive
overdesign. It also jeopardizes safety and inhibits technological progress. The
multidisciplinary aspect of corrosion problems combined with the distributed
responsibilities associated with such problems only increase the complexity of the
subject. Corrosion control is achieved by recognizing and understanding corrosion
mechanisms by using corrosion-resistant materials. Mild steel is widely used in many
industries because of economically cost-effective and easy fabrication, but it is prone to
undergo corrosion in aggressive environmental conditions. The environment may be a
liquid, gas or mixture of solid and liquid.
Corrosion intrudes itself into many parts of our lives. The damage it makes is very
clear. The economic costs of corrosion are obviously enormous. Like other natural
hazards such as earthquakes and severe weather disturbances, corrosion can cause
dangerous and expensive damages to infrastructure, waterways, ports, railroads,
hazardous materials storage, drinking water, sewer systems, electrical utilities,
telecommunications, automobiles, ships, aircrafts, mining, petroleum refining,
chemical, petrochemical and pharmaceutical production, pulp and paper, agricultural
production, food processing, electronics, defense, home appliances, gas transmission
pipelines and highway bridges. Losses sustained by corrosion amounts to many billions
of dollars annually. The economic factor is the main object for much of the current
research in corrosion. Another factor is the safety of operating equipments such as
pressure vessels, boilers, material containers for toxic materials and may be the most
important of all is the equipment for nuclear power plants and disposal of nuclear
wastes.
Corrosion problems also arise in the pipe lines due to aggressiveness of the liquid
which is being carried by them (Figs. 1.1-1.3). These liquids may be petroleum
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containing water and sulphur, high saline formation or sea water and pipes used in
cooling and heating systems in many operations. However, all kinds of water passes
through these lines contain very high chloride concentration and considerable amount of
sulfate and other ions of different metals. For this reason, the injection of corrosion
inhibitors through different sites of pipes is very important.
Mainly corrosion can have two forms, uniform and localized. Uniform corrosion
accounts for the greatest tonnage of metal consumed. Yet the localized forms of
corrosion are difficult to predict and control. Some forms of localized corrosion are
galvanic, crevice, pitting and erosion-corrosion. For uniform corrosion, the corrosive
environment must have the same access to all parts of the metal surface and the metal
itself must be metallurgically and compositionally uniform. Atmospheric corrosion is
probably the most prevalent example of uniform corrosion at a visually apparent rate
[1]. Of course since there are different types of atmospheres all over the world, the rate
of atmospheric corrosion will differ for each type.
Fig. 1.1: Oil pipeline corrosion.
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Fig. 1.2: Gas pipeline corrosion.
Fig. 1.3: Inner view of corroded pipeline.
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Pickling is a metal surface treatment used to remove impurities such as stains,

inorganic contaminants, rust or scale from ferrous metals, copper and aluminum alloys
(Fig. 1.4). A solution called pickle liquor which contains strong acids, is used to remove
the surface impurities. It is commonly used to descale or clean steel in various steel
making processes. Many hot working processes and other processes at high
temperatures leave a discoloring oxide layer or scale on the surface. In order to remove
the scale, the work piece is dipped into a vat of pickle liquor [2].
Pickling inhibitors are used to protect metal components from corrosive action
against acid effect while maintaining the pickling performance of the system. So,
cleaning ability of bath system directly intensifies on stains, residuals and oxide layers.
Thus, pickling bath solution will have a long-lasting lifetime with inhibitor addition and
acid consumption is appreciably minimized at plants. On the other hand, without
inhibitor usage, the corrosive effect of acid on parts will lead to a remarkable amount of
metal loss during pickling process. In pickling baths, hydrogen gas releases from the
surface of the metal due to the metal-acid interaction. The exposure of hydrogen to the
metal potentially brings a problematic issue known as hydrogen embrittlement where
diffusing of hydrogen through the metal makes it brittle [3]. In the case of inhibitor
usage, a barrier is formed on clean areas of metal surface, so excess hydrogen release
due to acid-metal interaction is strongly inhibited. Thus, hydrogen embrittlement risk on
metal parts is remarkably reduced with inhibitor addition to pickling baths.
Mild steel is widely used material in pipelines for domestic and industrial water
utilities and heat exchangers due to its good thermal conductivity and mechanical
workability. Scale and corrosion products have a negative effect on heat transfer and
they cause a decrease in heating efficiency of the equipment and transportation of the
liquid, which is why periodic descaling and cleaning using pickling solutions are
necessary. Most pickling inhibitors function by forming an adsorbed film on the metal
surface, probably no more than a monolayer in thickness, which essentially blocks
discharge of H+ and dissolution of metal ions. Dilute sulfuric or hydrochloric acids with
pickling inhibitors are used to clean out steel water pipes clogged with rust, to clean
boiler tubes encrusted with CaCO3 or iron oxide scales and to activate oil underground
wells. For example, boiler scale can be removed by using 0.1% hexamethylenetetramine
in 10 % HCl at a maximum temperature of 70 °C.
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Fig. 1.4: Stainless steel sheet before and after pickling.
Cooling and heating water circulation system can present several problems.
Formation of salt deposits and fouling by micro-organisms can appear when water is
used as thermal fluid (Fig. 1.5). These problems can occur jointly and reduce the
thermal efficiency of the circuits with significant economic repercussions. To reduce or
eliminate these problems, feed waters of boilers are treated with inhibitive formulations
composed of corrosion inhibitors associated with chemical reagents used both to reduce
corrosion of the boiler and auxiliary equipment and to reduce formation of inorganic
deposits in the boiler tubes (scaling), which interfere with heat transfer [4].
Fig. 1.5: Microbial corrosion in pipeline.
In oil production industries, economic losses and ecological damage caused by

corrosion stem from the very large amounts of metal equipment and structures that
come into contact with highly aggressive media. Stratal water content in oil and gas
industries often cause severe problems for steel pipelines of heat exchangers, boilers
and condensers (Figs. 1.6), and it negatively affects metal in oil production, refinery,
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transportation and processing operations. The most important tasks in the development
of an oilfield are reliable operation and long life of equipments and pipeline systems.
Acidic treatment is often used to intensify oil recovery and increase the efficiency of oil
deposits. Acidic fluids are very corrosive reagents to steel equipments. Dissolved metal
by acidic treatment can form precipitations of iron oxides or iron sulphides (in the
presence of hydrogen sulphide), which negatively affect the oil production equipments
and the quality of the crude oil. Under such conditions, a technically justified and
efficient method of protection is the use of inhibitors that get adsorb as protective films
on the metal to prevent its corrosion. At the same time, inhibitor injection, especially
nitrogen-containing compounds with a diphilic structure (Example: colloidal cationic
surfactants such as amine, imidazoline and their salts) seem to be one of the most
appropriate and most cost-effective methods to solve this problem. However, most
inhibitor’s evaluations are generally based on the test results under stagnant or low flow
rate (<1 m s-1) conditions [5].
Fig. 1.6: Corrosion in boilers.
There are five good reasons to study corrosion.

a) Materials are precious resources of a country. Our material resources of iron,
aluminum, copper, chromium, manganese, titanium, etc., are dwindling fast. In
some days we are going to face acute shortage of these materials. An impending
metal crisis does not seem anywhere to be a remote possibility but it will be a
reality. There is bound to be metal crisis and we are getting the signals. To
preserve these valuable resources, we need to understand how these resources are
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destroyed by corrosion and how they must be preserved by applying corrosion

protection technology.
b) Engineering knowledge is incomplete without understanding the corrosion. Aero
planes, ships, automobiles and other transport carriers cannot be designed without
any recourse to the corrosion prevention mechanism used in these structures.
c) Several engineering disasters such as crashing of civil and military aircraft, naval
and passenger ships, explosion of oil pipelines and oil storage tanks, collapse of
bridges and decks and failure of drilling plat forms and tanker trucks have been
witnessed in recent years. Corrosion has played a very important role in these
disasters. Applying the knowledge of corrosion prevention can minimize such
disasters.
d) Designing the artificial implants for the human body requires a complete
knowledge of the corrosion science and engineering. Surgical implants must be
by corrosion products and become unfit for consumption. Corrosion prevention is
integral part of the system to stop contamination of air, water and soil.
1.1.2. Theories and mechanism of corrosion
1.1.2.1. Local cell theory
According to De la Rive [6] corrosion occurs because of the creation of a large

number of micro electrochemical cells or local cells (Fig. 1.7) at heterogeneities
(impurities, defects, different phases, non-uniform stress distribution etc.,) on the metal
surface. Corrosion is an electrochemical process in which a difference in electrical
potential develops between two metals or between different parts of a single metal. This
voltage difference can be measured when a metal is electrically connected to a standard
electrode.
The electrical potential of a metal may be either more or less than the standard in
which case the voltage is expressed as either positive or negative. The difference in this
potential makes the current to pass through the metal causing reaction at anodic and
cathodic sites. Every metal surface is covered with numerically small anodes and
cathodes. These sites are usually developed due to the following reasons [7]:
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 Stress from welding or other works.
 Compositional differences at the metal surface.
 Surface irregularities from forming, extruding and other metal working operations.
Ionic conductor
Cathodic site Anodic site
Fig.1.7: Model for local cell theory of corrosion.
1.1.2.2. Wagner and Trauds’ theory
Wagner and Traud [8] have proposed a theory for the corrosion of pure metals.
According to this theory, impurities and other surface heterogeneities are not essential
for corrosion to occur. The necessary condition for corrosion (metal dissolution) to
occur is that, some cathodic reaction should proceed simultaneously on the surface. The
impurities might have formed when the metal is molten and these impurities are passed
onto the surface during rolling, forming or shaping operations.
Although corrosion is a complicated process, it can be most easily comprehended

as an electrochemical reaction involving the following three steps (Fig. 1.8):
a) Loss occurs from that part of the metal called the cathodic area because of the
lower potential at this site. In this case iron is lost to the water solution (oxidized
from Fe0 to Fe2+ state) and becomes oxidized to Fe2+ ion.
b) As a result of the formation of Fe2+, two electrons are released to flow through the
steel to the cathodic area.
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c) Oxygen in aqueous solution moves to the cathode and completes the electric
circuit by using the electrons that flow to the cathode to form OH- at the surface of
the metal.
Fig. 1.8: Reaction occurring during the corrosion of steel.
The reaction takes place as follows:
Anodic reaction: Fe o  Fe 2   2 e  (1.1)

Cathodic reaction: 1 / 2O2  H 2 O  2e   2OH  : pH  4.0 (1.2)
In the absence of oxygen, H+ participates in the reaction at the cathode instead of

oxygen and completes the electrical circuit as follows:
2H   2e  H2  (1.3)
Hydroxyl ions will combine with the Fe2+ produced by dissolution of the metal as
follows:
Fe 2   2OH   FeOH 2  (1.4)

The ferrous hydroxide produced has a very low solubility and quickly precipitates as a
white flock at the metal – water interface. The floc is then rapidly oxidized to ferric
hydroxide.
4 FeOH 2  O2  2 H 2 O  4 FeOH 3 (1.5)

Dehydrolysis of this product leads to the formation of the corrosion products normally
seen on the metal surface (Eqs. 1.6 and 1.7).
2 FeOH 3  Fe2O3  3H 2O (1.6)
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FeOH 3  FeO (OH )   H 2 O (1.7)
As solid corrosion products are precipitated at the anode, they may cause the
precipitation of other ions of water. Thus, a corrosion film may show traces of hardness
salts or such suspended matter as mud, sand, silt, clay or microbiological slime. If a
porous film forms over the metal, corrosion can continue because metal ions can
penetrate it and reach the solution interface, but when a tight adherent film is formed,
ionic diffusion is prevented and the metal will no longer dissolve.
1.1.3. Classification of corrosion
There is no universally accepted classification for corrosion, but the following

classification is adapted [9-11]:
1.1.3.1. Uniform or general corrosion

Uniform or general corrosion, as the name implies, results in a fairly uniform
penetration (or thinning) over the entire exposed metal surface. The general attack
results from local corrosion cell action, that is, multiple anodes and cathodes are
operating on the metal surface at any given time. The location of the anodic and
cathodic areas continues to move about on the surface, resulting in uniform corrosion.
In this case the exposed metal/alloy surface area is entirely corroded in an environment
such as a liquid electrolyte (chemical solution, liquid -metal), gaseous electrolyte (air,
CO2, SO2 etc.,) or a hybrid electrolyte (solid, water, biological organisms, etc.).
Some types of general corrosion and their description are given below,
 Atmospheric corrosion on steel tanks, steel containers, Zn parts, Al plates, etc.,
 High-temperature corrosion on carburized steels that forms a porous scale of
several iron oxide phases.
 Liquid-metal corrosion on stainless steel exposed to sodium chloride environment.
 Molten-salt corrosion on stainless steel due to molten fluorides (LiF, BeF2, etc.,).
 Biological corrosion on steel, Cu– alloys, and Zn– alloys in seawater.
 Stray-current corrosion on pipelines near railroad.
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1.1.3.2. Galvanic corrosion
Galvanic corrosion is an electrochemical action of two dissimilar metals in the

presence of an electrolyte and an electron conductive path (Fig. 1.9). It occurs when
dissimilar metals are electrically coupled in a common solution, the more negative
(more active) metal will be the anode of the galvanic corrosion cell and its corrosion
rate will increase. The more positive (more noble) metal will be the cathode and its
corrosion rate will decrease and it is detectable by the presence of a buildup of corrosion
at the joint between the dissimilar metals. For example when aluminum alloys or
magnesium alloys are in contact with steel (carbon steel or stainless steel), galvanic
corrosion can occur and accelerate the corrosion of the aluminum or magnesium.
Fig. 1.9: Galvanic corrosion of mild steel pipe connected to copper connector.
1.1.3.3. Localized corrosion
This term implies that, specific parts of an exposed surface area corrode in a
suitable electrolyte. This form of corrosion is more difficult to control than general
corrosion. Localized corrosion can be classified as,
 Crevice corrosion: It is similar to pitting corrosion in a stagnant electrolyte after its

initiation. This form of corrosion initiates due to changes in local chemistry such as
depletion of oxygen in the crevice, increase in pH with increasing hydrogen ion
concentration and increase of chloride ions. Oxygen depletion implies that, cathodic
reaction for oxygen reduction cannot be sustained within the crevice area and
consequently metal dissolution occurs. Crevice corrosion may take place on any metal
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and in any corrosive environment. However, metals like aluminum and stainless steel
that depend on their surface oxide film for corrosion resistance are particularly prone to
crevice corrosion, especially in environments such as seawater that contain chloride
ions. The material responsible for forming the crevice corrosion need not be metallic.
Wood, plastic, rubber, glass, concrete, asbestos, wax and living organisms have been
reported to cause crevice corrosion. It is frequently more intense in chloride
environments. The mechanism of crevice corrosion is electrochemical in nature and it is
illustrated in Fig. 1.10. It requires a prolong time to start the metal oxidation process,
but it may get accelerated afterwards.
Fig. 1.10: Crevice corrosion of mild steel connectors.
 Filiform corrosion: It is basically a special type of crevice corrosion, sometimes

termed as “under film” corrosion. This type of corrosion occurs under painted or plated
surfaces when moisture permeates the coating. Lacquers and "quick-dry" paints are
most susceptible to the problem. Their use should be avoided unless absence of an
adverse effect has been proven by field experience.
 Pitting corrosion: Pitting Corrosion is "self-nucleating" crevice corrosion, starting

at occluded cells (Fig. 1.11). Corrosion products often cover the pits, and may form
"chimneys". Pitting is considered to be more dangerous than uniform corrosion damage
because it is more difficult to detect, predict and prevent. A small, narrow pit with
minimal overall metal loss can lead to the failure of an entire engineering system. Once
initiated, both crevice and pitting corrosion can be explained by differential
concentration cells, cathodic reactions, i.e., oxygen reduction or hydrogen evolution
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may start in the crevice or the pits. Large surface areas will become cathodic and pits or
crevices will become anodic and corrode. Metal dissolution will thus be concentrated in
small areas and will proceed at much higher rates than with uniform corrosion. Large
crevices are less likely to corrode because water movement causes mixing and
replenishes oxygen, hydrogen ions, bicarbonate or hydrogen sulfide.
Fig. 1.11: Pitting corrosion in mild steel pipes.
 Intergranular corrosion: Intergranular corrosion is a localized form of corrosion.

It is a preferential attack on the grain boundary phases or the zones immediately
adjacent to them. Little or no attack is observed on the main body of the grain. This
results in the loss of strength and ductility. The attack is often rapid, penetrating deeply
into the metal and causing failure.
1.1.3.4. Stress corrosion cracking (SCC)

Structural parts subjected to a combination of a tensile stress and a corrosive
environment may prematurely fail at a stress below the yield strength (Fig. 1.12). This
phenomenon is known as environmentally induced cracking (EIC) which is divided into
the following categories:
 Stress-corrosion cracking (SCC)
 Hydrogen-induced cracking (HIC) and
 Corrosion-fatigue cracking (CFC).
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Fig. 1.12: Stress corrosion cracking of mild steel.
1.1.3.5. Erosion corrosion
The term “erosion” applies to deterioration due to mechanical force. When the
factors contributing to erosion accelerate the rate of corrosion of a metal, the attack is
called “erosion corrosion”. It is the result of a combination of an aggressive chemical
environment and high fluid surface velocities. This can be the result of fast fluid flow
past a stationary object, such as the case with the oilfield check valve, or it can result
from the quick motion of an object in a stationary fluid, such as when a ship's propeller
churns the ocean. Surfaces which have undergone erosion corrosion are generally fairly
clean, unlike the surfaces from many other forms of corrosion.
1.1.4. Rate of corrosion
As previously mentioned (Wagner and Trauds’ theory), three basic steps are
necessary for corrosion to proceed. If any step is prevented from occurring, then
corrosion stops. The slowest step among these determines the rate of the overall
corrosion process. The cathodic reaction (Eq. 1.3) is the slowest of the three steps
involved in the corrosion of steel and this reaction determines the rate. A large cathodic
surface area relative to the anodic area allows more oxygen, water and electrons to react
which increase the flow of electrons from the anode leading to increase of corrosion
rate. Conversely, as the cathodic area becomes smaller relative to the anodic area, the
corrosion rate decreases. This ratio affects the corrosion rate and plays a significant role
in the selection of effective inhibitors to control corrosion [12].
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1.1.5. Factors influencing the corrosion rate

Primary factors influencing the corrosion rate are the conditions of the metal
surface and the secondary factors are the nature of the environment [13].
Primary factors
1.1.5.1. Nature of the metal
The tendency of the metal to undergo corrosion is mainly dependent on the nature
of the metal. In general the metal with lower electrode potential has more reactive and is
more susceptible for corrosion and metal with high electrode potential is less reactive
and less susceptible for corrosion. For example, metals like K, Na, Mg, Zn etc., have
low electrode potential and undergo corrosion very easily where as noble metals like
Ag, Au, and Pt have higher electrode potential, their corrosion rates are negligible. But
there are few exceptions for this general trend as some metals show the property of
passivity like Al, Cr, Ti, Ta, etc., According to electrochemical series, metal with more
positive potential are relatively stable and those with more negative potential are
unstable [14]. If we know the electrode potentials of metals in some electrolyte, we may
predict whether the metal would corrode or not. The electromotive force, E is the
difference between electric potentials of cathodic and anodic reactions,
E = Ecathodic − Eanodic (1.8)
This value is related to Gibbs free energy which is represented by the equation,
ΔG = -nFE (1.9)
where, ΔG is the change of Gibbs free energy of corrosion reaction, n is the number of
electrons taking part in the corrosion reaction and F is Faraday’s constant.
In corrosion processes where hydrogen evolution is the cathodic reaction,

hydrogen over potential (resistance to hydrogen evolution) is another important factor
effecting the corrosion. Each metal in a given environment has characteristic hydrogen
overpotential. Thus a metal with low hydrogen overpotential in a given environment
undergoes facile corrosion. In the case of alloys, other entities added in micro-quantities
will alter the hydrogen overpotential and thereby affect the corrosion process.
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1.1.5.2. Surface state of the metal
The corrosion product is usually the oxide of the metal, and the nature of the
product determines the rate of further corrosion process. If the oxide layer formed on
the surface is stoichiometric, highly insoluble and non-porous in nature with low ionic
and electronic conductivity, then that type of layer effectively prevents further corrosion
which acts as a protective film. For example, Al, Cr and Ti develop such a layer on their
surface and become passive to corrosion, and some metals like Ta, Zn and Mo not only
form such protective layers but are capable of self repairing oxide films when it is
damaged. Hence these are extremely passive metals. If the oxide layer formed on the
metal surface is non-stoichiometric, soluble, unstable and porous in nature and has an
appreciable conductivity, it cannot control corrosion on metal surface (For Ex: oxide
layer formed on metals like Zn, Fe, Mg, etc,). Highly polished and smooth surface
resists corrosion while a rough surface containing various types of imperfections such
as clearage steps, dislocations, point defects etc., is liable to severe attack.
1.1.5.3. Protective film
Certain metals like Al have a tendency to form a protective film on the surface
which acts as physical barrier (passivation) between the metal and the medium, thereby
curtailing the corrosion [15].
Secondary factors
1.1.5.4. pH of the medium
In general, rate of corrosion is higher in acid pH than in neutral and alkaline

pH. In case of iron, at very high pH, protective coating of iron oxide is formed which
prevents corrosion where as low pH serve corrosion takes place. But for metals like Al,
corrosion rate is high even at high pH. For metals like zinc, iron, magnesium etc.,
hydrogen evolution is thermodynamically favored cathodic reaction. Corrosion of each
metal in acidic medium is therefore highly pH dependent. Decrease in pH facilitates the
rate of hydrogen evolution and hence increases the corrosion rate of metals. In case
where a protective film is formed on the metal surface, change in solution pH may
affect the solubility of the film and therefore affect the corrosion process. Thus under
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varying pH conditions of the medium, a corroding surface may exhibit activity,

immunity or passivity [14].
1.1.5.5. Temperature of the medium
Corrosion is an activation-controlled chemical reaction, the rate of which is

greatly affected by temperature. Usually, corrosion rate increases significantly as
temperature increases. A rule of thumb is that, when corrosion is controlled by
diffusion of oxygen, the corrosion rate at given oxygen concentration approximately
doubles for every 10 °C rise in temperature. In an open vessel, allowing dissolved
oxygen to escape, corrosion rate increases with increase in temperature to about 80 °C
and then falls to a very low value at the boiling point. The lower corrosion rate above 80
°C is related to a marked decrease of oxygen solubility in water as the temperature is
raised and this effect eventually overshadows the accelerating effect of temperature
alone. In a closed system, on the other hand, oxygen cannot escape, and the corrosion
rate continues to increase with temperature until all the oxygen is consumed. When
corrosion is accompanied by hydrogen evolution, the corrosion rate is more than double
for every 10 °C rise in temperature [16]. In general, as temperature rises, diffusion
increases, and both viscosity and over-voltage decrease causing depolarization by
hydrogen evolution. Increased diffusion enables more dissolved oxygen to react with
cathodic surface, thereby depolarizing the corrosion cell. A decrease in viscosity aids
depolarization mechanism, and it favors the solution having atmospheric oxygen and
enhances hydrogen evolution. In a domestic water system, an increase in temperature
from 25 oC to 75 oC (Fig. 1.13) may increase the corrosion as much as 400 percent. An
increase in temperature is normally expected to speed up a chemical reaction according
to thermodynamic considerations [17].
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At constant O2
concentration
Fig. 1.13: Effect of temperature on the corrosion rate of low carbon steel in tap water.
1.1.5.6. Effect of dissolved oxygen
Dissolved oxygen plays a very important and complicated role in the corrosion
of metals. Oxygen takes part in cathodic processes on the metal surface in neutral,
alkaline, and acidic media. If dissolved oxygen is absent in water, and then corrosion
diminishes near to zero in neutral and alkaline solutions. If the concentration of
dissolved oxygen increases, corrosion accelerates as a result of oxygen participation in
the cathodic processes. In the presence of oxygen, depolarization of the cathodic
products takes place according to Eqs. (1.1) and (1.2). In most situations, depolarization
by oxygen tends to control the rate at which the iron corrodes. However, Eq. (1.2) is
generally so rapid that oxygen concentration at the cathodic surface approaches zero.
Therefore, rate of oxygen depolarization depends on the rate of diffusion of oxygen
through the resistant film at the surface of the metal. Ferrous ion is converted to the
ferric state by further oxidation and most of the common rust is comprises of hydrated
ferric oxide. Frequently, a black layer of magnetic hydrous ferrous ferrite (Fe3O4. nH2O)
forms between Fe2O3 and FeO. Hence, the rust film normally consists of three layers of
iron oxide in different states of oxidation. Although increase in oxygen concentration
initially accelerates the corrosion of iron, but, beyond a critical concentration, the
corrosion rate drops down again to a low value. If we inject more and more oxygen into
water, under some specific conditions (in water of high purity) and at high temperature
that may result in the formation of a passive protective dense film composed of metal
oxides on the metal surface, and corrosion would decrease [18]. The injection of oxygen
into water is one of the corrosion control methods at power stations.
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Cohen [19] reported that the corrosion rate in the presence of oxygen is 65 times
higher the rate in the absence of oxygen. Whitman [20] stated that the corrosion rate
increased at higher velocity due to increase in oxygen diffusion and breaking down of
the protective films on the metal surfaces. Frese [21] showed that, iron tends to become
passive with high oxygen. Fig. 1.14 shows the effect of oxygen concentration on the
corrosion of low carbon steel in tap water at different temperatures.
Fig. 1.14: Effect of oxygen concentration on the corrosion of low carbon steel in tap
water at different temperatures.
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SECTION - II: CORROSION INHIBITORS
1.2.1. Introduction
An inhibitor is a chemical substance or combination of substances which when

added in very low concentrations in a corrosive environment effectively prevents or
reduces corrosion without significant reaction with the components of the environment.
Concentrations of corrosion inhibitors can vary from 1 to 15,000 ppm (0.0001 to 1.5 wt
%). Corrosion inhibitors can be solids, liquids and gases, and can be used in solid, liquid
and gaseous media. Solid media can be concrete, coal slurries or organic coatings
(paints). Liquids may be water, aqueous solutions or organic solvents. A gaseous
medium is an atmosphere or water vapor. Corrosion inhibitors are selected on the basis
of solubility or dispersibility in fluids which are to be inhibited. For instance, in a
hydrocarbon system, a corrosion inhibitor soluble in hydrocarbon is used. Two phase
system composed of both hydrocarbons and water is utilized as oil soluble water-
dispersible inhibitor.
Corrosion inhibitors have been found to be effective and flexible means of

corrosion mitigation. The use of chemical inhibitors to decrease the rate of corrosion
processes is quite variable. Corrosion inhibitors are used in oil and gas exploration and
production, petroleum refineries, chemical manufacturing, heavy manufacturing, water
treatment and product additive industries [22]. In the oil extraction, processing and
chemical industries, corrosion inhibitors have always been considered to be the first line
of defense. A great number of scientific studies have been devoted to the subject of
corrosion inhibitors [23-36].
Inhibitors find major use in closed environmental systems that have good
circulation so that an adequate and controlled concentration of inhibitor is ensured. Such
conditions can be met, for instance in cooling water recirculation systems, oil
production, oil refining, and acid pickling of steel components. One of the more
recognizable applications for inhibitors is in antifreeze for automobile radiators. The
application of inhibitors must be viewed with caution by the user because inhibitors
may afford excellent protection for one metal in a specific system but can aggravate
corrosion for other metals in the same system. Inhibitors can be organic or inorganic
compounds and they are usually dissolved in aqueous environments. Some of the most
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effective inorganic inhibitors are chromates, nitrites, silicates, carbonates, phosphates

and arsenates. The organic inhibitors include amines, heterocyclic nitrogen compounds,
sulfur compounds such as thioethers, thioalcohols, thioamides, thiourea and hydrazine.
Chromates and zinc salts are used increasingly less due to their toxicity and are
nowadays largely replaced by organic inhibitors. Thus practical criteria for the selection
of corrosion inhibitors from the great variety of inorganic and organic substances with
inhibiting properties are not only their inhibition efficiency but also safety of use,
economic constraints and compatibility with other chemicals in the system, and
environmental concerns [27].
In order to avoid or reduce the corrosion of metallic materials, inhibitors used in

cooling system must satisfy the following criteria [28]:
a) It must give good corrosion protection at a very low concentration of inhibitor.

b) It must protect all exposed materials from the attack of corrosion.
c) It must remain efficient in extreme operating conditions (higher temperature and
velocity).
d) In case of an under or over dosage of inhibitor, corrosion rate should not increase
drastically.
e) The inhibitor or reaction products of the inhibitor should not form any deposits on
the metal surface particularly at locations where heat transfer takes place.
f) It should suppress both uniform and localized corrosion.
g) It should have long range effectiveness.
h) It should not cause toxicity and pollution problems.
1.2.2. Mechanism of corrosion inhibition
Many corrosion inhibitors form protective films on the metal surface and
diminish possible contact with aggressive components. In order to protect metals from
corrosion, inhibitors must reach the surface of metals and react with the products of
electrochemical reactions or be adsorbed. The protective mechanisms of anodic,
cathodic and adsorbing inhibitors are different. The protective mechanism of anodic
inhibitors (phosphates, carbonates, molybdates and nitrites) is based on the reaction
with the metal surface and the formation of passive layers of oxides, hydroxides or salts.
These inhibitors significantly influence the corrosion potentials of the protected metals.
21
The protective mechanism of cathodic inhibitors is generally based on the reaction with
the products of a cathodic electrochemical reaction (OH−) [29 - 31]. For example, Zn2+
react with OH− with the formation of insoluble Zn(OH)2 at cathodic sites of metallic
surfaces. Organic inhibitors are adsorbed on the metal surface and the presence of polar
groups such as CN, CS, CO and CP in organic molecules of inhibitors with free
electrons on N, S, O and P atoms promote their adsorption on metallic surfaces. The
mechanism of adsorption may be physical or chemical. When weak Coulomb forces are
formed between atoms of inhibitors and metallic atoms, then the adsorption is physical.
If strong chemical bonds are formed between atoms of inhibitors and metallic atoms,
the chemisorption occurs. Organic inhibitors are sometimes called non-passivating
types. They nearly have no influence on the corrosion potential of metals.
Organic compounds containing multiple bonds, preferably triple bonds are

effective inhibitors. The choice of effective inhibitors is based on their mechanism of
action and their electron donating capability. The inhibiting ability of the inhibitor is
supported by molecular structure of the adsorption active sites with lone pair and/or p -
orbitals such as heterocyclic rings containing sulphur, oxygen, phosphorus and/or
nitrogen atoms [32-34]. They have an ability to accept or donate electrons in order to be
adsorbed on metallic surfaces by electrostatic interaction between the unshared electron
pair of corrosion inhibitor and metal. These inhibitors are usually adsorbed on the metal
surface by the formation of a coordinate covalent bond (chemical adsorption) or the
electrostatic interaction between the metal and inhibitor (physical adsorption). The
action of inhibitors in acid solutions depends on adsorption onto the metal surface in
oxide-free solutions. The adsorbed inhibitors then acts to retard the cathodic and/or
anodic electrochemical corrosion processes. Inhibitors in acid solutions can interact
with metals and affect the corrosion reaction in a number of ways, some of which may
occur simultaneously. It is very difficult to assign a single general mechanism of action
to an inhibitor because the mechanism may change with experimental conditions. Thus,
the action of an inhibitor depends on its concentration, the pH of the acid, the nature of
the anion of the acid, the presence of other species in the solution, the extent of reaction
to form secondary inhibitors and the nature of the metal. The mechanism of action of
inhibitors with the same functional group may additionally differ with factors such as
the effect of the molecular structure and the electron density. Inhibition usually results
from one or more of the following mechanisms [35, 36]:
22
 Adsorption of corrosion inhibitors onto metals: The inhibitive performance is

usually depends on the fraction of the surface covered, θ with adsorbed inhibitor.
But, at low surface coverage (θ < 0.1), the effectiveness of adsorbed inhibitor
species in retarding the corrosion reactions may be greater than at high surface
coverage.
 Presence of surface charge on the metal: Adsorption of inhibitor on the metal
surface may be due to electrostatic force of attraction between ionic charges or
dipoles of the adsorbed species and the electric charge on the metal at the
metal/solution interface.
 Effect of functional group and structure of the inhibitor: Inhibitors can also
bond to metal surfaces by electron transfer to the metal to form a coordinate type of
bond. Usually, the above process is favored when the metal contains vacant
electron orbitals of low energy such as transition metals. Electron transfer from the
adsorbed species is favored by the presence of relatively loosely bound electrons.
Example: Anions and neutral organic molecules containing lone pair of electrons or
electron systems associated with multiple bonds especially triple bonds or aromatic
rings. The electron density at the functional group is directly proportional to the
inhibitive efficiency in a series of related compounds.
 Interaction between inhibitor and water molecules: Adsorption of inhibitor
molecules is a displacement reaction involving removal of adsorbed water
molecules from the metal surface. During the adsorption of an inhibitor molecule,
the change in interaction energy with water molecules in passing from the dissolved
to the adsorbed state forms an important part of the free energy change on
adsorption. This increases the solvation energy of the inhibitor species, which in
turn is related with size of the hydrocarbon portion of an inhibitor molecule. Thus
increasing size leads to decreasing solubility and increasing adsorption ability. This
is consistent with the increasing inhibitive efficiency observed at constant
concentrations with increasing molecular size in a series of related compounds.
 Interaction of adsorbed inhibitor species: Lateral interactions between adsorbed
inhibitor species may become significant as the surface coverage and hence the
proximity of the adsorbed species increases. These lateral interactions may be either
attractive or repulsive. Attractive interactions occur between molecules containing
large hydrocarbon components (e.g., n-alkyl chains). As the chain length increases,
23
the increasing Van der Waals attractive force between the adjacent molecules leads
to stronger adsorption at high coverage.
 Reaction of adsorbed inhibitors: In some inhibitors, the adsorbed corrosion
inhibitor may react usually by electrochemical reduction to form a product that may
also exhibit inhibitive action. Inhibition due to the added substance is called
primary inhibition and that due to the reaction product is secondary inhibition. In
these cases, the inhibitive efficiency may increase or decrease with time, it depends
to what extent the secondary inhibition is effective than the primary inhibition. For
example, sulfoxides can be reduced to sulfides which are more efficient inhibitors.
 Formation of a diffusion barrier: The absorbed inhibitor may form a surface film
that acts as a physical barrier to limit the diffusion of ions or molecules to or from
the metal surface, and hence retard the rate of corrosion reactions. Generally, this
effect occurs when the inhibitor species are large molecules (e.g., proteins such as
gelatin or agar-agar, polysaccharides such as dextrin or compounds containing long
hydrocarbon chains). A surface film of these types of inhibitors affects both anodic
and cathodic reactions.
 Blocking of reaction sites: The blocking decreases the number of metal atoms at
which corrosion reactions can occur. During this, mechanisms of the reactions are
not affected, and the Tafel slopes of the polarization curves remain unaffected.
 Participation in the electrode reactions: Sometimes corrosion reactions involve
the formation of adsorbed intermediate species with surface metal atoms (e.g.,
adsorbed hydrogen atoms in the hydrogen evolution reaction and adsorbed Fe(OH)2
in the anodic dissolution of iron). The adsorbed inhibitors will hinder the formation
of these adsorbed intermediates, but the electrode processes may then proceed by
alternative paths through intermediates containing the inhibitors. In these processes,
the inhibitor species act like catalyst and remain unchanged. Such action of
inhibitor is generally characterized by an increase in the Tafel slope of the anodic
dissolution of the metal. Inhibitors may also retard the rate of hydrogen evolution
on the metals by affecting the mechanism of the reaction by increasing the Tafel
slopes of cathodic polarization curves. This effect has been observed on iron in the
presence of inhibitors such as phenylthiourea, acetylenic hydrocarbons, aniline
derivatives, benzaldehyde derivatives and pyridinium salts.
24
 Alteration of the electrical double layer: The adsorption of ions or species that
can form ions on metal surfaces will change the electrical double layer at the
metal/solution interface, and this will affect the rates of the electrochemical
reactions. The adsorption of cations such as quaternary ammonium ions and
protonated amines makes the potential more positive in the plane of the closest
approach to the metal ions from the solution. This positive potential shift hinders
the discharge of the positively charged hydrogen ions. On the other hand, the
adsorption of anions makes the potential more negative on the metal side of the
electrical double layer, and this will tend to accelerate the rate of discharge of
hydrogen ions. This effect has been observed with sulfosalicylate ions and the
benzoate ions.
1.2.3. Classification of corrosion inhibitors
A common classification of inhibitors is based on their effects on the

electrochemical reactions involved in the corrosion process [37-42].
1.2.3.1. Passivating inhibitors
Passivating inhibitors cause a large anodic shift of the corrosion potential forcing
the metallic surface into the passivation range. There are two types of passivating
inhibitors.
a) The oxidizing anions such as chromates, nitrites and nitrates that can passivate steel
in the absence of oxygen.
b) The non-oxidizing ions such as phosphates, tungstates and molybdates that require
the presence of oxygen to passivate steel.
In general, passivation inhibitors can actually cause pitting and accelerate

corrosion when concentrations fall below minimum limits. For this reason, it is essential
to monitor the inhibitor concentration.
1.2.3.2. Volatile inhibitors
Volatile corrosion inhibitors (VCIs) also called vapor phase inhibitors (VPIs) are
compounds transferred in a closed environment to the site of corrosion by volatilization
from a source. In boilers, volatile basic compounds such as morpholine or hydrazine are
25
transported with steam to prevent corrosion in condenser tubes by neutralizing the

acidic carbon dioxide or by shifting the surface pH towards less acidic. If the corrosion
product is volatile, it volatilizes as soon as it is formed, thereby leaving the underlying
metal surface exposed for further attack. This causes rapid and continuous corrosion
leading to excessive corrosion. For example, molybdenum oxide (MoO3), the oxidation
corrosion product of molybdenum is volatile. In closed vapor process (shipping
containers), volatile solids such as salts of dicyclohexylamine, cyclohexylamine and
hexamethylene amine are used as volatile corrosion inhibitors.
1.2.3.3. Cathodic inhibitors
Cathodic inhibitors reduce corrosion by slowing the reduction reaction rate of the
electrochemical corrosion cell. This is done by blocking the cathodic sites by
precipitation. For example, calcium, magnesium and zinc ions will precipitate as
hydroxides on cathodic sites as the local environment becomes more alkaline due to the
reduction reaction at these sites. Cathodic inhibitors are effective when they slow down
the cathodic reaction rate. Arsenic, bismuth and antimony which are referred to as
cathodic poisons reduce the hydrogen reduction reaction rate and thus lower the overall
corrosion rate. Other cathodic inhibitors remove reducible species from the
environment. Removal of oxygen from the corrosive environment will significantly
decrease the corrosion rate. This can be done through (a) the use of oxygen scavengers
such as sodium sulfite and hydrazine which react with the oxygen and remove it from
the solution (b) vacuum de-aeration or (c) boiling to lower the dissolved oxygen
concentrations.
1.2.3.4. Anodic inhibitors
Anodic inhibitors such as chromates, phosphates, tungstates and other ions of

transition elements with high oxygen content are those that stifle the corrosion reaction
occurring at the anode by forming a sparingly soluble compound with a newly produced
metal ion. They are adsorbed on the metal surface forming a protective film or barrier,
thereby reducing the corrosion rate. Anodic inhibitors build a thin protective film along
the anode and increasing their potential and thus slow down the corrosion reaction.
Chromates, nitrates, tungstate and molybdates are some examples of anodic inhibitors.
26
Although, this type of control is affected, yet it may be dangerous since severe local
attack can occur, if certain areas are left unprotected by depletion of the inhibitors.
1.2.3.5. Mixed inhibitors
Some substances inhibit corrosion by reducing simultaneously the rate of anodic

and cathodic reactions involved in the corrosion process and are therefore called mixed
inhibitors. They are typically film forming compounds that cause the formation of
precipitates on the surface blocking both anodic and cathodic sites indirectly. Anodic
inhibitors are, for the most part, dangerous inhibitors, especially if their concentrations
are too less. But cathodic inhibitors are generally safe. Mixed inhibitors are less
dangerous than pure anodic inhibitors, and in number of cases they may not increase the
corrosion intensity. The most common inhibitors of this category are the silicates and
the phosphates.
1.2.3.6. Synergistic inhibitors
It is very rare that a single inhibitor is used in systems such as cooling water
systems. More often, a combination of inhibitors (anodic and cathodic) is used to obtain
better corrosion protection properties. The blends which are produced by mixing of
multi-inhibitors are called synergistic blends. Examples include chromate-phosphates,
polyphosphate-silicate, zinc-tannins, and zinc-phosphates.
1.2.3.7. Precipitation inhibitors
Precipitation inhibitors are compounds that cause the formation of precipitates on

the surface of the metal, thereby providing a protective film. Hard water that is high in
calcium and magnesium is less corrosive than soft water because of the tendency of the
salts in the hard water to precipitate on the surface of the metal and form a protective
film. The most common inhibitors of this category are the silicates and the phosphates.
Sodium silicate, for example, is used in many domestic water softeners to prevent the
occurrence of rust. In aerated hot water systems, sodium silicate protects steel, copper
and brass.
27
1.2.3.8. Green corrosion inhibitors
There is no clear and accepted definition of “environmentally friendly” or

“green” corrosion inhibitors. In practice, corrosion inhibition studies have become
oriented towards human health and safety considerations. For this purpose recently, the
researchers have been focused on the use of eco-friendly compounds such as plant
extracts which contain many organic compounds. Amino acids, alkaloids, pigments and
tannins are used as green alternatives for the toxic and hazardous compounds. Due to
biodegradability, eco-friendliness, low cost and easy availability the extracts of some
common plants and plant products have been studied as corrosion inhibitors for various
metals and alloys under different environmental conditions [43].
1.2.4. Adsorption
Adsorption is a surface phenomenon exhibited by solids which consists of

adhesion in an extremely thin layer of the molecules of gases, liquids and dissolved
substances with which they are in contact. The adsorption of ions or neutral molecules
on bare metal surfaces immersed in solution is determined by the mutual interactions of
all species present at the phase boundary. These include electrostatic and chemical
interactions of the adsorbate with the surface, adsorbate–adsorbent and adsorbate–
solvent interactions. There are two types of adsorptions depending on the nature of
forces involved [41, 44]. (a) Chemisorption: In this type of adsorption, a single layer of
molecules, atoms or ions is attached to the surface by chemical bonds and is essentially
irreversible. (b) Physical adsorption: In this type, the attachment is by the weaker van
der Waal’s forces, whose energy levels approximate to those of condensation. The
factors that influence the adsorption of inhibitor ions on metal surfaces are [45]:
a) Surface charge on the metal: Adsorption may occur due to the electrostatic
attractive forces between the ionic charges or dipoles on the adsorbed inhibitor and
the electric charge on the metal at the metal-solution interface.
b) The functional groups and structure of inhibitor: Inhibitors can bind to the
metal surface by electron transfer and form a coordinate type of linkage leading to
strong binding and effective inhibition. Species containing relatively loosely bound
electrons in anions, neutral molecules, lone pair of electrons, π – electron systems
associated with triple bonds or organic ring systems and the functional groups
28
containing elements of group V or VI of the periodic table favour facile electron

transfer and stronger bond formation and hence effective inhibition. The tendency
to form stronger coordinate bond increases with decreasing electronegativity and
follow the order, O < N < S < P.
c) The interaction between adsorbed inhibitor species (synergism and
antagonism): Adsorbed species may enter into various interactions on the surface
of an electrode that may significantly influence their inhibitive properties and the
mechanism of their action.
d) Reaction of adsorbed inhibitors: The adsorbed inhibitor species may react usually
by electrochemical reduction to form a product which is also inhibitive. Inhibition
due to the added substance is termed as primary inhibition and that due to reaction
products as secondary inhibition.
Adsorption is usually described through isotherms, i.e., the amount of adsorbate

on the adsorbent as a function of its pressure (if gases) or concentration (if liquids) at
constant temperature. The first mathematical fit to an isotherm was published by
Freundlich and Kuster. It is a purely empirical formula for gaseous adsorbates. Irving
Langmuir published a new isotherm model for gases adsorbed on solids which retained
his name. It is a semi-empirical isotherm derived from a proposed kinetic mechanism. It
is based on four assumptions:
1. The surface of the adsorbent is uniform.

2. Adsorbed molecules do not interact.
3. All adsorptions occur through the same mechanism.
4. At the maximum adsorption, only a monolayer is formed.
These assumptions are seldom true. There are always imperfections on the
surface, and the adsorbed molecules are not necessarily inert. The mechanism is not
clearly same for the very first molecule to adsorb as for the last. The fourth assumption
is the most troublesome as frequently more molecules will adsorb on the monolayer.
This problem is addressed by the BET isotherm for relatively flat (non-microporous)
surfaces. Nevertheless, the Langmuir isotherm is the first choice for most models of
adsorption and has many applications in surface kinetics (usually called Langmuir-
Hinshelwood kinetics) and thermodynamics.
29
Different adsorption isotherms were found to describe the adsorption of inhibitors

on metal surface such as Langmuir [46 – 48], Temkin [49–51], Frumkin [52 – 54],
Flory– Huggins [55 – 57], Dhar–Flory–Huggins and Bockris–Swinkels [58], and
Freundlich [58, 59].
1.2.5. Polarization
Polarization [44] is defined as the departure of the electrode potential from their
equilibrium values that is from open circuit potential (OCP) causing a decrease in the
current density. Corrosion process on a metal surface or when two metals are in contact
is due to the current flowing from anodic area to cathodic area. The open circuit
potential difference between the anodic and cathodic areas determines the direction of
current flow. However, the magnitude of the current is controlled by polarization
characteristics of the electrodes. An important factor that controls the polarization is the
concentration of the corrosive species. When the corrosion reaction progresses, the
concentration of the electrolyte species changes (gets depleted at the cathode and
accumulated at the anode) in the vicinity of each electrode. The greater the polarization
of the electrodes (cathodic or anodic), the smaller the corrosion current despite the open
circuit potential difference being high. If the anode alone undergoes polarization, the
rate of corrosion is controlled by anodic polarization as shown in Fig. 1.15a, where the
corrosion current is largely determined by the anode [59]. Fig.1.15b shows the cathodic
polarization where the cathode alone undergoes polarization. Here the cathodic
polarization curve is much steeper and the corrosion current is under cathodic control. If
both electrodes undergo polarization, it is said to be under mixed control as shown in
Fig.1.15c.
Ec Ec Ec
Ecor
Ecor
Ecor
Ea
Ea Ea
Icor Icor Icor
(a) (b) (c)
Fig. 1.15: Evans polarization diagrams: (a) anodic control (b) cathodic control (c) mixed
control.
30
1.2.6. Electrochemical impedance
Electrochemical methods based on alternating currents can be used to obtain

insights into corrosion mechanisms and to establish the effectiveness of corrosion
control methods such as inhibition and coatings. In an alternating current circuit,
impedance determines the amplitude of current for a given voltage. Impedance is the
proportionality factor between voltage and current. In electrochemical impedance
spectroscopy (EIS), the response of an electrode to alternating potential signals of
varying frequency is interpreted on the basis of circuit models of the
electrode/electrolyte interface [44]. The simplest model for characterizing the metal –
solution interface includes the three essential parameters, Rs (the solution resistance),
Cdl (the capacitance of the double layer) and Rp (the polarization resistance). When
direct current measurements are carried out (i.e., frequency is zero), the impedance of
the capacitor approaches infinity. In parallel electrical circuits, the circuit with the
smallest impedance dominates, with the result that, under these conditions, the sum of
Rs and Rp is measured. When compared to other techniques for corrosion evaluation,
EIS has several advantages:
 It gives kinetic information on the corrosion processes. The use of AC signals

allows the separation between the resistances of charge transfer resistance of the
coating itself and of the solution.
 It gives mechanistic information. This is based on the use of ‘‘equivalent circuits’’
which are electronic circuits whose response is identical to that of the cell under
study.
 It provides information on the properties of the coating itself, namely its
resistance and capacitance. The changes in these properties have been associated
with the loss of protective properties.
1.2.7. Quantum chemical calculations
Quantum chemical methods are very useful in determining the molecular structure
as well as elucidating the electronic structure and reactivity [60]. The selection of an
effective and appropriate inhibitor for the corrosion of metals has been widely carried
out based on empirical approach [61-62]. Recently, quantum chemical calculations have
been performed enormously to complement the experimental evidence. Quantum
31
chemical methods and molecular modeling techniques enable the definition of a large
number of molecular quantities characterizing the reactivity, shape and binding
properties of a complete molecule as well as of molecular fragments and substituents.
The quantum chemical calculations have been applied widely to compute electronic
properties possibly relevant to the inhibition action. Knowing the orientation of the
molecule, favorable configurations, atomic charges, steric and electronic effects would
be useful for better understanding of the inhibitor performance. It has been stated that
the experimental data can be correlated well with quantum chemical parameters such as
electron density, ionization potential, total energy, dipole moment, charge density,
highest occupied molecular orbital (HOMO) and lowest unoccupied molecular orbital
(LUMO) energies and the gap between them.
32
SECTION - III: ANTIOXIDANT ACTIVITY AND CORROSION

INHIBITION
An antioxidant is a molecule capable of slowing or preventing the oxidation of

other molecules. Oxidation is a chemical reaction that involves transfer of electrons
from a substance to an oxidizing agent. The term antioxidant was used to refer
specifically to a chemical that prevents the consumption of oxygen. In the late 19th and
early 20th century extensive study was devoted to the uses of antioxidants in important
industrial processes such as prevention of metal corrosion. It was found that these
antioxidants can act as good corrosion inhibitors and their efficiencies depend
principally on the substituted functional groups. Organic molecules of this type can get
adsorbed on the metal surface and form a bond between their N-electron pair and/or π-
electron cloud and the metal surface, thereby reducing the corrosion in different
aggressive solutions. Antioxidants (free radical scavengers) are widely applied in the
coating industry to prevent thermal and photochemical degradation of organic coatings
by inactivating the free radicals generated by these processes. Consequently, this study
will address the application of free radical scavengers in relation to cathodic
delamination of organic coatings (primers) and the steel surface [63].
Antioxidants from different origins have high bioavailability, and therefore high
protective efficiency against free radicals [64]. Free radicals and singlet oxygen
scavengers (antioxidants) have metal and alloy corrosion inhibition character, which
depends to a greater extent on the structural feature of the antioxidant added and to its
accepting - donating hydrogen or electron behaviors [65]. Greater antioxidant activity
and corrosion inhibition behaviour of molecules is linked to the electron donating effect
of the different groups attached to aromatic ring, which increases the electron density on
the benzene ring. The increasing delocalization of electron density in the molecule
makes more reactive towards scavenging reactive oxygen as well as inhibiting corrosion
process. The adsorption of inhibitor molecules is further stabilized by participation of π-
electrons of benzene ring. Electronegative oxygen, sulfur and nitrogen atoms present in
compounds facilitate more efficient adsorption of the molecules on mild steel surface.
Reduction of oxygen availability in the corroding system and the presence of a barrier
between the electrode surface and oxygen in the medium retard the rate of metal
corrosion [66].
33
Synthetic and natural antioxidants are free radical scavengers containing some
N- heterocyclic compounds and their derivatives possess compact structures and high
thermal stabilities. They have been widely used as lubricating additives because they
possess excellent antioxidant and anticorrosion properties. The experimental results
demonstrate that antioxidants (free radical scavengers) containing hetero atoms, not
only accept the electron to terminate the oxygen radical reaction, but also donate
electron to form a stable chemical adsorption film on metal surface in order to prevent
the corrosion of metals. A series of N-containing compounds and their derivatives such
as benzotriazole derivatives, 1, 3, 4-thiadiazole derivatives, thiazole derivatives,
oxazoline, thiazoline and imidazoline derivatives were reported as excellent
multifunctional lubricating additives [67]. Christ Tamborski et al. [68] studied
antioxidant and anticorrosion properties of new aromatic phosphine compounds. The
antioxidant and anticorrosion properties of the some natural products have been
investigated by Shanab and coworkers [69].
34
SECTION - IV: CORROSION INHIBITION STUDIES ON MILD STEEL:

A REVIEW
The corrosion inhibition of mild steel by organic compounds has been widely
studied using different organic moieties. The use of organic inhibitors for preventing
corrosion is a promising alternative solution. Organic compounds containing functional
electronegative groups, pi-electron in triple or conjugated double bonds and presence of
aromatic rings in their structure are the major adsorption centers and usually are good
inhibitors [72]. The adsorption characteristics of organic molecules are also affected by
sizes, electron density at the donor atoms and orbital character of donating electrons
[70, 71]. The choice of effective inhibitors is based on their mechanism of action and
their electron donating capability. The inhibiting ability of an inhibitor depends upon
the molecular structure of the adsorption active sites and/or p-orbitals such as
heterocyclic rings containing sulphur, oxygen, phosphorus and/or nitrogen atoms. They
have the ability to accept or donate electrons in order to get adsorbed on metallic
surfaces by electrostatic interaction between the unshared electron pair of corrosion
inhibitor and metal.
Abboud et al. [76] synthesized and studied the inhibition of mild steel corrosion in
1 M HCl by 2, 2'-bis(benzimidazole) using various corrosion monitoring techniques and
found that the inhibition efficiency value increases with the inhibitor concentration and
reaches a maximum of 97.8 % at 10-4 M. The effect of N, N'-bis (salicylaldehyde)-1,3-
diaminopropane and its corresponding cobalt complex on the corrosion behaviour of
steel in 1 M sulphuric acid solution was investigated by Abdel-Gaber et al [77].
Thermodynamic characterization of metal dissolution and inhibitor adsorption processes
on mild steel using 2, 5-bis (n-thienyl)-1,3,4-thiadiazoles in hydrochloric acid system
was investigated by Bentiss et al. [78] and they discussed about thermodynamic
functions of dissolution and adsorption processes from experimental polarisation. The
effect of 4-(2'-amino-5'-methylphenylazo) antipyrine (AMPA) on the corrosion of mild
steel in a 2 M HCl solution was studied by Abd El Rehima et al [79]. All the data
revealed that AMPA acts as inhibitor in acidic environment. Furthermore, polarization
data showed that the compound behaves as a mixed-type inhibitor. Aminopyrimidine
derivatives as inhibitors for corrosion of 1018 carbon steel in nitric acid solution was
reported by Abdallah et al [80]. It was found that the aminopyrimidine derivatives
35
provide a good protection to steel against pitting corrosion in chloride containing

solutions.
Ganesha Achary et al. [81] reported that, two quinoline derivatives namely 8-
hydroxy quinoline (HQ) and 3-formyl 8-hydroxy quinoline (FQ) are good corrosion
inhibitors on mild steel in hydrochloric acid solution. The results indicated that the
corrosion inhibition efficiency and extent of surface coverage were increased with
increase in inhibitor concentration and decreased with increase in temperature and acid
concentration. Bouklah et al [82] studied corrosion inhibition behavior and
thermodynamic properties of 2, 5-bis (4-methoxyphenyl)-1,3,4-oxadiazole as a
corrosion inhibitor for mild steel in normal sulfuric acid medium. Results obtained
revealed that 4-MOX showed excellent performance as corrosion inhibitor for mild steel
in sulfuric acid media and its efficiency attains 96.19 % for 8 × 10−4 M at 333 K. The
role of some new thiosemicarbazide derivatives namely, 1-ethyl-4(2,4-dinitrophenyl)
thiosemicarbazide (I), 1,4-diphenylthiosemicarbazide (II), 1-ethyl-4-
phenylthiosemicarbazide (III) as corrosion inhibitors for carbon steel in 2 M HCl was
investigated by Badr et al [83]. Results obtained revealed that the inhibition efficiency
(% IE) follows the sequence: I > II > III.
Yuanyuan et al. [84] reported that 5, 10, 15, 20-tetraphenylporphyrin and 5, 10,
15, 20-tetra-(4-chlorophenyl) porphyrin are good inhibitors for iron corrosion in H2SO4
solutions. The maximum protection efficiency for the porphyrin-covered iron electrodes
is more than 80 %. The new isoxazolidines were synthesized and their influence on
corrosion inhibition of mild steel in 1M and 5 M HCl at 50–70 °C has been studied by
Ali et al [85]. All compounds have shown very good corrosion inhibition efficiency (IE
%) in acidic solution in the range of 100 – 400 ppm. Abboud et al. [86] studied 2, 3-
quinoxalinedione as novel corrosion inhibitor for mild steel in 1M HCl, and found good
inhibiting properties for steel corrosion in acidic bath with efficiencies of around 88 %.
A series of new thiazole derivatives have been synthesized and investigated as corrosion
inhibitors for carbon steel in 2 M HCl solutions by Al-Sarawya et al [87]. The results
showed that the inhibition efficiency of the investigated compounds depend on
concentration and the nature of the inhibitor. The presence of substituted donating group
(–OCH3) plays an important role in the inhibition efficiency of these investigated
compounds. The inhibition action of N-(furfuryl)-N′-phenyl thiourea on the corrosion of
36
mild steel in hydrochloric acid medium was reported by Divakara Shetty et al [88].
Good inhibition efficiency (> 93%) has been evidenced at 28 °C and 50 °C and
inhibition is governed by chemisorption mechanism.
Amin et al. [89] evaluated the inhibiting effects of the newly synthesized (GlyD1),
2-(4-(dimethylamino)benzylamino)acetic acid hydrochloride on mild steel corrosion in
4.0 M H2SO4 solutions at different temperatures (278–338 K). The inhibition
performance of GlyD1 was much better than those of N, N-bis (2-aminoethyl)glycine
(GlyD2) and Gly itself. Results obtained from the different corrosion evaluation
techniques were in good agreement with each other. New macrocyclic polyether
compounds containing a 1, 3, 4-thiadiazole moiety have been prepared to study the
corrosion inhibitive effect of mild steel in normal hydrochloric acid solutions [90]. The
results of these investigations have shown enhancement in inhibition efficiencies with
the extent of the polyethylene glycol unit that forms a cavity. Molecular modeling has
been conducted in an attempt to correlate the corrosion inhibition properties with the
calculated quantum chemical parameters. Shassi-Sorkhabi et al. suggested that, the
newly synthesized compound namely 3H-phenothiazin-3-one -7-dimethylamin acts as
corrosion inhibitor on mild steel in 1 M HCl solution [91]. It was found that this
compound acts as a good inhibitor for mild steel in 1 M HCl even at very low
concentration (1 ppm).
The effect of formation of covalent bonds between carbon and iron atoms on the
adsorption of p-toluene and p-hydroxymethylbenzene on iron for its protection was
studied by Shimura et al [92]. The inhibitive effect of indole-3-acetic acid on the
corrosion of mild steel in 0.5 M HCl medium was reported by Avci et al [93].
According to the obtained results from all measurements, inhibition efficiency was
about 77 % with 1.7 ×10-3 M inhibitor present and increased to about 93 % at the 1 ×10-
2
M inhibitor concentration. A new corrosion inhibitor namely N-(piperidinomethyl)-3-
[(pyridylidene)amino]isatin (PPI) has been synthesized and its influence on corrosion
inhibition of low carbon steel in 1N hydrochloric acid solution was studied by Quraishi
et al [94]. The PPI showed more than 94 % inhibition efficiency at an optimum
concentration of 300 ppm. The inhibition efficiency of inhibitor was found to vary with
inhibitor concentration, solution temperature, immersion time and acid concentration.
Experimental and theoretical investigations of three newly synthesized organic
compounds on mild steel corrosion in sulfuric acid medium was reported by Bahrami
37
and co-workers [95]. It was found that the investigated compounds exhibit a good
inhibition effect especially at 8–10 ppm range concentration, which makes them
commercially important.
Bhrara et al. [96] evaluated the inhibiting effects of butyl triphenyl

phosphonium bromide (BuTPPB) on the corrosion of medium carbon steel in 0.5 M
sulphuric acid solution. At 298 K, inhibition efficiency was found to be 94.5 % for
10−7 M BuTPPB which increased to about 99 % for 10−2 M concentration. The use of
electrochemical and theoretical methods on the corrosion inhibition mechanism of mild
steel by three Schiff bases, 2-{[(2-sulfanylphenyl)imino]methyl}]phenol (A), 2-{[(2)-1-
(4-methylphenyl)methylidene]amino}-1-benznethiol (B) and 2-[(2-sulfanylphen-
yl)ethanimidoyl)]phenol (C) on the corrosion of mild steel in 15 % hydrochloric acid
solution has been reported by Behpour and co-workers [97]. The results of the
investigation showed that the compounds A and B with mean efficiency of 99 % at
200 mg/L concentration for mild steel corrosion in hydrochloric acid, and they act as
mixed inhibitors.
The corrosion inhibition properties of tris(benzimidazole-2-ylmethyl)amine

(TBMA) by different techniques were analyzed and the data showed that, this
compound can retard anodic reaction [98]. DFT results clearly showed that TBMA
posses corrosion inhibition properties by having a delocalization region in the
benzimidazole ring that gives up their π-electrons through its HOMO orbital to the
metal LUMO orbital to form a adsorption layer over the metallic surface. Yuce et al.
evaluated the adsorption and corrosion inhibition effect of 2-thiohydantoin (2-THD) on
mild steel in 0.1 M HCl solution [99]. The results showed that 2-THD acts as a mixed
type inhibitor by suppressing simultaneously the cathodic and anodic processes via
physical adsorption on the MS surface followed by Langmuir adsorption isotherm. New
long alkyl side chain acetamide, isoxazolidine and isoxazoline derivatives were
synthesized and their corrosion inhibitive property was studied by Yildirım and Cetin
[100]. The best inhibition was generally obtained at 50 ppm inhibitor concentration in
the acidic medium. All the tested inhibitors except two showed promising inhibition
efficiencies in oil medium also. Kinetics of mild steel corrosion in aqueous acetic acid
solutions has been studied by Singh and Mukherjee [101]. The results obtained by
weight loss method and polarization technique are in good agreement with each other.
The surface studies support the conclusions drawn from the weight loss method.
38
Kenya and co-workers studied gallic acid (GA) as corrosion inhibitor for carbon
steel (CS) in chemical decontamination formulation at 4.25 mM concentration. [102]. A
formulation containing Citric acid (CA) (1.4 mM), EDTA/NTA (1.4 mM), Ascorbic
acid (AA) (1.0–2.0 mM) and GA (4.25 mM) was found to be more efficient in
dissolving hematite and providing 31% corrosion inhibition (passivation) to the CS.
Doner et al. reported the corrosion inhibitive behaviour of 2-amino-5-mercapto-1,3,4-
thiadiazole (2A5MT) and 2-mercaptothiazoline (2MT) on mild steel using experimental
and theoretical studies [103]. It was shown that both 2A5MT and 2MT act as good
corrosion inhibitors for mild steel protection. The effect of the presence of extra NH2
group and N atom in 2A5MT on the ability to act as corrosion inhibitor was investigated
by theoretical calculations. Xianghong et al. [104] studied the inhibition effect of
Tween-20 as a nonionic surfactant on the corrosion of cold rolled steel in 1.0 – 8.0 M
hydrochloric acid. The results showed that Tween-20 is a good inhibitor in 1.0 M HCl,
and the inhibition efficiency increases with the inhibitor concentration, while decreases
with increasing the hydrochloric acid concentration and temperature.
The corrosion inhibition effect of 3-[(2-hydroxy-benzylidene)-amino]-2-thioxo-

thiazolidin-4-one (HBTT) on mild steel in the 0.5 M H2SO4 medium has been
investigated by Ali Doner and co-workers [105] using the conventional
potentiodynamic polarization studies, linear polarization studies (LPR), electrochemical
impedance spectroscopy studies (EIS). SEM was used for surface characterization. The
results showed that HBTT posses excellent inhibition effect towards MS corrosion. The
corrosion inhibition of iron in HCl, HClO4, H2SO4 and H3PO4 solutions (1M for each)
by cefatrexyl has been studied by Morad [106]. The results obtained at 30 °C revealed
that cefatrexyl acts as a weak inhibitor in HCl solution but shows excellent inhibition
performance in the remaining acids. The corrosion inhibition mechanism of some amino
acids namely cysteine (CYS), serine (SER), amino butyric acid (ABU) alanine (ALA)
and valine (VAL), threonine (THR), phenylalanine (PHE), tryptophan (TRP) and
tyrosine (TYR) were studied on the mild steel using experimentally and theoretically by
Eddy [107]. From this study, the expected trends for the variation of the inhibition
efficiencies of the amino acids is CYS > SER > ABU, THR > ALA >VAL and TRP >
TYR > PHE, respectively.
Khaled [108] synthesized N-(5,6-diphenyl-4,5-dihydro-[1,2,4]triazin- 3-yl)-

guanidine (NTG) and studied its inhibitive performance towards the corrosion of mild
39
steel in 1 M hydrochloric acid and 0.5 M sulphuric acid. These studies have shown that
NTG is a very good inhibitor in acid media and the inhibition efficiency goes up to 99
% and 96 % in 1M HCl and 0.5M H2SO4, respectively. Adsorption of 2-amino-5-
mercapto-1,3,4-thiadiazole (2A5MT) on mild steel (MS) surface in 0.5 M HCl solution
and its corrosion inhibition effect was studied by Solmaz and co-workers [109] in both
short and long immersion times (over 120 h). The obtained results indicate that the
stability of 2A5MT is good in the typical temperature range of working conditions of
pickling. Fouda et al. suggested that, some furfural hydrazone derivatives act as
corrosion inhibitors on C-steel in H3PO4 solution [110]. These hydrazone derivatives
are fairly efficient inhibitors for C-steel dissolution in 3M H3PO4. The oxo-triazole
derivative (DTP) was synthesized and its inhibitory action on the corrosion of mild steel
in sulphuric acid was investigated by Zhihua Tao et al. [111] using weight loss,
potentiodynamic polarization, EIS and SEM. The results revealed that DTP is an
excellent inhibitor and the inhibition efficiencies obtained from weight loss and
electrochemical experiment were in good agreement. Shuwei et al [112] used
molecular dynamics and density functional theory to study the relationship between
structure and inhibitory behaviour of imidazoline derivatives like 3-ethylamino-2-
undecyl imidazoline (EUI) and chloride-3-ethylamino-3-(2,3-two hydroxyl) propyl-2-
undecyl imidazoline sodium phosphate(CEPIP) for Q235 steel in CO2 saturated solution
at 298 K, and calculated by weight loss and electrochemical techniques. The results
indicated that the two imidazoline derivatives could both adsorb on the Fe surface
firmly through the imidazoline ring and heteroatoms, and hence the two inhibitors both
have excellent corrosion inhibition performance.
Corrosion monitoring of mild steel in sulphuric acid solutions in the presence of

some thiazole derivatives like 2-amino-4-(p-tolyl)thiazole (APT), 2-methoxy-1,3-
thiazole (MTT) and thiazole-4-carboxaldehyde (TCA) at iron (110) surface dissolved in
aqueous solution were studied via molecular dynamics (MD) simulations by Khaled and
Amin [113]. Chemical and electrochemical measurements are agreeing with
computational study and APT is the most effective inhibitor among the tested thiazoles.
EIS and polarization studies to evaluate the inhibitors effect of 3H-phenothiazin-3-one,
7-dimethylamin on mild steel corrosion in 1 M HCl solution was reported by Sorkhabi
et al [114]. It was found that it acts as a strong inhibitor for mild steel in 1 M HCl even
at very low concentration (1 ppm). Tris-hydroxymethyl-(2-hydroxybenzylidenamino)-
40
methane (THHM) was synthesized and its anticorrosive property for cold rolled steel in
hydrochloric acid has been studied by Qing et al [115]. Ali et al. [116] studied the bis-
isoxazolidines obtained by the cycloaddition reaction of 1-pyrroline 1-oxide with 2,7-
di(10-undecenyloxy)naphthalene and 1,4-di(10-undecenyloxy)benzene as new class of
corrosion inhibitors for mild steel in acidic media. All the three inhibitors molecules at
60 °C and 400 ppm concentration achieved inhibition efficiencies in the ranges 97–98
% and 92–96 % as determined by gravimetric method for corrosion of mild steel in 1 M
HCl and 0.5 M H2SO4, respectively.
The effect of two triazole derivatives namely 1-[2-(4-nitro-phenyl)-

5[1,2,4]triazol-1-ylmethyl-[1,3,4]oxadiazol-3-yl]-enthanone (NTOE) and 1-(4-methoxy-
phenyl)-2-(5-[1,2,4]triazol-1-ylmethyl-4H[1,2,4]triazol-3-ylsulfanyl)-ethanone (MTTE)
against the corrosion of mild steel in 1 M hydrochloric acid was studied by Zhanga et al
[117]. The inhibition ability of the two follows the order NOTE > MTTE, and the
inhibition deficiencies determined by polarization, EIS, and weight loss methods are in
good agreement with each other. Gokhan Gece [118] reported the application of
quantum chemical methods in corrosion inhibitor studies. It begins with a concise
summary of the most used quantum chemical parameters and methods and then
summarizes the results of research articles in corrosion science over the past 20 years.
Quantum chemical study of the inhibition of the corrosion of mild steel in H 2SO4 by
some antibiotics was studied by Nabuk et al [119]. Some Schiff base compounds
containing disulfide bond were analyzed as corrosion inhibitors for mild steel in HCl
[120] by Behpour et al. Quantum chemical calculations were further applied to reveal
the adsorption structure and explain the experimental results. The effect of organic
compounds on the electrochemical behaviour of steel in acidic media, a review has been
reported by Abd El–Maksoud [121]. Natural product as corrosion inhibitor for metals in
corrosive media - a review was reported by Raja and Sethuraman [122].
The relationship between the quantum chemical parameters for three triazole
compounds and their inhibition ability was studied using electrochemical measurements
(potentiodynamic polarization and EIS), molecular dynamic method and quantum
chemical calculations were done by Musa et al [123]. The quantum chemical
calculations showed that the triazole ring is the active site in these inhibitors and they
can adsorb on Fe surface by donating electrons to d-orbitals of Fe. Adsorption isotherms
and corrosion inhibitive property of some oxadiazol-triazole (TOMP) derivatives in
41
acidic solution was analyzed by Zhihua et al [124]. Results obtained revealed that
TOMP is an effective corrosion inhibitor for mild steel in sulphuric acid and its
efficiency attains more than 97.6% at 298 K. Solmaz [125] studied the inhibition effect
of a Schiff base 5-((E)-4-phenylbuta-1,3-dienylideneamino)-1,3,4-thiadiazole-2-thiol
(PDTT) on mild steel corrosion in 0.5 M HCl for both short and long immersion time.
The Schiff base has shown remarkable inhibition on the corrosion of mild steel in 0.5 M
HCl solution. The high inhibition efficiency was attributed to the blocking of active
sites by adsorption of inhibitor molecules on the steel surface.
Four Gemini surfactants were synthesized and evaluated as corrosion inhibitors

for carbon steel in 0.5 M HCl solution by Negm et al [126]. The results showed that
inhibition efficiencies increased on increasing the inhibitor doses, hydrophobic chain
length and reached a maximum at 500 ppm by weight for stearyl derivative. Corrosion
inhibition of mild steel in 0.5 M H2SO4 and 1.0 M HCl by 2-amino-5-phenyl-1,3,4-
thiadiazole (APT) has been studied using potentiodynamic polarization and
electrochemical impedance spectroscopy (EIS) measurements by Yongming Tang et al.
[127]. The results showed that inhibition efficiency increases with the increase of APT
concentration in both acids, and higher inhibition efficiency is obtained in 0.5 M H2SO4.
Obot et al. [128] evaluated ketoconazole (KCZ) as corrosion inhibitor for mild steel in
aerated 0.1 M H2SO4 by gravimetric method. Quantum chemical approach was further
used to calculate some electronic properties of the molecule in order to ascertain
correlation between the inhibitive effect and molecular structure of ketoconazole.
The behavior of Schiff base, N, N′-bis(salicylidene)-1,2-ethylenediamine (salen),

its reduced form (N, N′-bis(2-hydroxybenzyl)-1,2-ethylenediamine) and a mixture of its
preceding molecules, ethylenediamine and salicylaldehyde as corrosion inhibitors on
carbon steel in 1 mol L−1 HCl solution was studied by da Silva et al [129]. Experimental
results showed that the reduced salen showed highest efficiency among the inhibitors
studied. The results obtained in the presence of salen were similar to those obtained in
the presence of the salicylaldehyde and ethylenediamine mixture, showing that in acid
medium salen molecule undergoes hydrolysis, regenerating its precursor molecules.
Potentiodynamic polarization, electrochemical impedance spectroscopy (EIS),

weight loss measurements and atomic force microscopy techniques were used to
investigate the inhibitory effect of diethylcarbamazine (DECM) on the corrosion of mild
42
steel in HCl solution was studied by Singh et al [130]. The inhibitor showed >90 %
inhibition efficiency at 5.01 × 10−4 M. Three compounds of N-alkyl-sodium
phthalamates were synthesized and tested as corrosion inhibitors for carbon steel in
0.5 M aqueous hydrochloric acid by Flores et al [131]. Tests showed that inhibition
efficiencies were related to aliphatic chain length and dependent on concentration. N-1-
n-tetradecyl-sodium phthalamate displayed moderate efficiency against uniform
corrosion, which is 42–86% at 25 °C and 25–60 % at 40 °C. Some 4-phenylthiazole
derivatives were tested as corrosion inhibitors for 304L stainless steel in 3 M HCl using
weight loss and galvanostatic techniques by Fouda et al [132]. The results showed that
inhibition efficiency increases with increasing concentration of 4-phenylthiazole
derivatives.
Four 1,3-diketone malonates compounds were synthesized and tested as corrosion

inhibitor by Fragoza-Mar et al. [133] on mild steel in 1 M aqueous hydrochloric acid.
Both tautomers displayed high corrosion inhibition efficiency (75–96 %) at 100 mg L−1,
which increased with temperature (25–55 °C) and dependent on diketo population.
Goulart et al. [134] studied the inhibition ability of four thiosemicarbazones and two
semicarbazones towards carbon steel corrosion in 1 M HCl. Results were evaluated by
molecular modeling, potentiodynamic polarization and electrochemical impedance
spectroscopy (EIS) at different inhibitor concentrations. Both experimental and
theoretical data showed that thiosemicarbazones are better corrosion inhibitors than the
semicarbazones. A comparative study of 5-amino-1,2,4-triazole (5-ATA), 5-amino-3-
mercapto-1,2,4-triazole (5-AMT), 5-amino-3-methylthio-1,2,4-triazole (5-AMeTT) and
1-amino-3-methylthio-1,2,4-triazole (1-AMeTT) as inhibitors for mild steel corrosion in
0.1 M HCl solution at 20 ºC was carried out by Hassan et al [135]. The studies have
shown that 5-AMT was the most efficient inhibitor reaching the values of inhibition
efficiency up to 96 % at the concentration of 10-3 M.
The effect of 1-methyl-3-pyridin-2-yl-thiourea on the corrosion resistance of mild

steel in H2SO4 solution was investigated by Hosseini et al [136]. The results showed
that inhibition efficiency increases with the increase of inhibitor concentration. Jawich
et al. [137] for the first time, compared the corrosion inhibition properties of
diethylenetetramine-derived imidazoline (I), tetraethylenepentamine-derived
imidazoline (II) and bis-imidazoline (III), all having heptadecyl pendants as
hydrophobes. At the concentration of 100 ppm at 40 °C, imidazolines I, II, and III
43
imparted inhibition efficiencies of 84 %, 95 % and 96 % respectively. Imidazolines

cover most of the steel surface before their critical molar concentrations are reached.
The corrosion inhibition of mild steel in 1M HCl solution by a Schiff base compound
named 2-[(4-phenoxy-phenylimino)methyl]-phenol (APS) was investigated by Keles
[138] at different temperatures (25–55 °C) using electrochemical measurements. Time
dependency of mild steel in 1 M HCl solution in the absence and presence of APS was
also studied. N-Phenyl oxalic dihydrazide (PODH) and oxalic N-phenylhydrazide N′-
phenylthiosemicarbazide (OPHPT) were synthesized and tested as inhibitors for the
corrosion of mild steel in 1M HCl by Larabi et al [139]. Inhibition efficiencies up to 92
% for OPHPT and 79 % for PODH were obtained.
Sodium diethyldithiocarbamate (DDTC) as corrosion inhibitor for cold rolled steel

(CRS) in 0.5 M HCl solution was investigated by Lei Li et al. [140] using Tafel
polarization and electrochemical impedance spectroscopy (EIS). All the data indicate
that DDTC can inhibit the corrosion of CRS in HCl solution. Polarization data showed
that DDTC acts as a good inhibitor though it can accelerate the anodic reaction to some
extent. 2-((Dehydroabietylamine) methyl)-6-methoxyphenol (DMP) was investigated by
as a corrosion inhibitor for mild steel in synthetic seawater medium by weight loss
measurements, electrochemical tests, SEM, XPS, quantum chemical calculations and
molecular dynamics Liu et al [141] (MD). The results showed that DMP inhibits the
corrosion of mild steel in synthetic seawater, and inhibition efficiency increases with the
increase in concentration of the inhibitor. The inhibitory effect of tryptamine on the
corrosion of mild steel in 0.5 M hydrochloric acid at 30 °C was investigated by
Lowmunkhong et al. [142] using linear polarization, potentiodynamic polarization and
electrochemical impedance spectroscopy (EIS) techniques. When the concentration of
tryptamine is 500 ppm the inhibition efficiency calculated by these techniques is around
97 %. The inhibition effect of 3-amino-1,2,4-triazole-5-thiol (3ATA5T) was
investigated in 0.5 M HCl on carbon steel (CS) by Mert et al. [143] at various
concentrations and temperatures. The results showed the correlation between
experimental (inhibition efficiencies, ΔGads, Ea) and quantum chemical parameters
(dipole moment, EHOMO, ELUMO). The high inhibition efficiency was described in terms
of strong adsorption of protonated inhibitor molecules on the metal surface which forms
a protective film.
44
Safarizadeh and Khosravan [144] investigated the interaction energies of

benzimidazole, aniline and nine of their derivatives on the surface of iron in
hydrochloric acid medium through cluster model using quantum chemical calculations
at DFT level. The interaction energy is then used as a descriptor in QSIR method for
corrosion behavior modeling of the inhibitors in solutions at different concentrations.
The findings are indicative of the effectiveness of the new descriptor. The corrosion
protection of mild steel in 2.5 M H2SO4 solution by 4,4-dimethyloxazolidine-2-thione
(DMT) was studied by Musa et al. [145] at different temperatures by measuring
changes in open circuit potential (OCP), potentiodynamic polarization and
electrochemical impedance spectroscopy (EIS). Results showed that DMT inhibited
mild steel corrosion in 2.5 M H2SO4 solution and inhibition efficiencies increased with
the concentration of the inhibitor, but decreased proportionally with temperature.
The corrosion inhibition of mild steel in 2.5 M H2SO4 solution by 4-amino-5-

phenyl-4H-1, 2, 4-trizole-3-thiol (APTT) was studied at different temperatures, utilising
open circuit potential, potentiodynamic and impedance measurements by Musa et al
[146]. The results indicate that APTT performed as an excellent mixed-type inhibitor
for mild steel corrosion in 2.5 M H2SO4 solution. The corrosion inhibition properties of
a new class of oxadiazole derivatives, namely 3,5-bis(n-pyridyl)1,2,4-oxadiazoles (n-
DPOX) for C38 carbon steel corrosion in 1 M HCl medium were analysed by Outirite et
al [147]. An adequate structural model of the interface was used and values of the
corresponding parameters were calculated and discussed. The inhibition efficiency,
increase with the increase in inhibitor concentration and attained a maximum value of
97 % at 12 ×10-4 M of 3-DPOX. At all concentrations, IE(%) follows the ranking order:
3-DPOX > 2DPOX> 4-DPOX. Popova et al. [148] investigated eight diazoles as
corrosion inhibitors for mild steel in 1 M hydrochloric acid using gravimetric and
polarization techniques. It was found that the inhibition efficiency increased with the
increase of organic substrate concentration and the adsorption followed the Frumkin
isotherm.
The inhibitory properties of four azoles (indole, benzimidazole, benzotriazole,

benzothiazole) were investigated in case of mild steel corrosion in 1 M HCl by Popova
[149], the effect of temperature was followed. Impedance spectroscopy, polarization
resistance, gravimetric and polarization curves methods were applied. The corrosion
inhibition effect of 4-{[(1Z)-(2-chloroquinolin-3-yl)methylene]amino} phenol (CAP),
45
N-[(1Z)-(2-chloroquinolin-yl)methylene]-N-(4-methoxyphenyl)amine (CMPA) and N-

[(1E)-(2-chloroquinolin-3-yl)methylene]-N-(4-nitrophenyl)amine (CNPA) on mild steel
in 1 M HCl has been investigated by Prabhu et al. [150] using mass loss, polarization
and electrochemical impedance techniques at 300 K.
Inhibition of mild steel corrosion in de-aerated 0.5 M sulfuric acid solutions

containing various concentrations of indole-5-carboxylic acid was studied in the
temperature range of 25 - 55ºC using weight loss, potentiodynamic polarization and
spectrophotometric tests has been carried out by Quartarone and co-workers [151].
Selected triazole derivatives have been synthesized and evaluated as corrosion inhibitors
for mild steel in natural aqueous environment by weight loss, potentiodynamic
polarization and ac impedance methods by Ramesh and Rajeswari [152]. All the
condensed products showed good inhibition efficiency. The effect of changing
functional groups of some triazole derivatives on their inhibition efficiency was also
reported using weight loss and potentiodynamic techniques. 3-Salicylalidene amino-
1,2,4-triazole phosphonate (SATP) was found to be the best corrosion inhibitor compare
to the other compounds. Sathiyanarayanan et al. [153] attempted to study the inhibitive
effect of triethylene tetramine (TETA) and hexamethylene tetramine (HMTA) for mild
steel in 1 M hydrochloric acid in the concentration range of 10−6 to 10−2 M by weight
loss, DC polarization and AC impedance spectroscopy methods. Results indicate that
the addition of tetramines to the acid reduce the rate of metal attack.
The inhibitory effect of 2-((5-mercapto-1,3,4-thiadiazol-2-

ylimino)methyl)phenol Schiff base (MTMP) on mild steel corrosion in 0.5 M HCl
solution was studied by Solmaz et al [154]. It was shown that, the MTMP Schiff base
has remarkable inhibition efficiency on the corrosion of mild steel in 0.5 M HCl
solution. The inhibition efficiency depends on the concentration of inhibitor and reaches
97 % at 1 mM MTMP. Jacob and Parameswaran [155] investigated heterocyclic Schiff
base furoin thiosemicarbazone for its corrosion inhibition towards mild steel in 1 M HCl
solution using weight loss, Tafel polarization and electrochemical impedance
spectroscopy techniques. Furoin thiosemicarbazone revealed good corrosion inhibition
efficiency even at low concentrations towards mild steel in HCl medium. Chemical
methods were used to assess the inhibitive and adsorption behaviour of carboxymethyl
cellulose (CMC) by Solomon et al. [156] for mild steel in H2SO4 solution at 30–60 °C.
Results obtained show that CMC acts as inhibitor for mild steel in H2SO4.
46
Two thiadiazole derivatives namely 2-amino-5-(3-pyridyl)-1,3,4-thiadiazole (3-

APTD) and 2-amino-5-(4-pyridyl)-1,3,4-thiadiazole (4-APTD) were investigated as
steel corrosion inhibitors in 0.5 M H2SO4 by Tang et al. [157] using polarization and
electrochemical impedance spectroscopy. The experimental results showed that the
inhibition efficiency of 4-APTD is higher than that of 3-APTD, and the molecular
dynamics (MD) simulations showed that the adsorption of 4-APTD on iron surface has
the higher binding energy than that of 3-APTD. Tuken et al. [158] studied the inhibition
efficiency of 1-ethyl-3-methylimidazolium dicyanamide (EMID) against mild steel
corrosion in acidic environment. Surface analysis showed that the assembled inhibitor
film could protect the metal successfully during 120 h exposure in 0.1 M H2SO4. The
inhibitor was fixed successfully within polypyrrole film and applied to steel surface as
highly protective coating.
Zhang et al. [159] investigated the corrosion inhibition performance of 2-(4-

pyridyl)-benzimidazole (PBI) against corrosion of mild steel in 1 M HCl using weight
loss and electrochemical measurements. The theoretical results from DFT and MD
simulations revealed that adsorption of PBI depends on the formation of coordinative
bonds between PBI molecule and iron surface, and the binding energy between PBI
molecule and iron surface is the highest among the three studied compounds. Five new
tetrathiafulvalene (TTF) derivatives bearing two or four thiazole groups were prepared
by Zhao et al [160]. The derivatives were characterized by 1H NMR, IR, MS spectra,
elemental analyses and X-ray analysis. The preliminary electrochemical properties of
the derivatives were investigated by cyclic voltammetry (CV) and two one-electron
quasi-reversible waves with redox potentials were observed. The synergistic inhibition
effect of rare earth cerium(IV) ion and 3,4-dihydroxybenzaldehye (DHBA) on the
corrosion of cold rolled steel (CRS) in H2SO4 solution was first investigated by Li et al.
[161] using weight loss and potentiodynamic polarization methods. The effect of
inhibitor concentration, temperature, immersion time and acid concentration on
synergism were discussed in detail. The results revealed that DHBA has moderate
inhibitive effect and its adsorption obeys Temkin adsorption isotherm. The corrosion
inhibition of mild steel in 1 M HCl solution by streptomycin has been studied by Shukla
et al. [162] using Tafel polarization, electrochemical impedance spectroscopy (EIS) and
weight loss measurements. The inhibitor showed 88.5 % inhibition efficiency at
optimum concentration of 500 ppm.
47
Sodium tungstate (Na2WO4) has been investigated as corrosion inhibitor of cold

rolled steel (CRS) in per acetic acid (PAA) solution by weight loss, potentiodynamic
polarization and electrochemical impedance spectroscopy (EIS) by Qu et al [163]. All
the data obtained from the experiments indicate that Na2WO4 is capable of inhibiting
the corrosion of CRS in PAA solution. Ostovari et al. [164] investigated the corrosion
inhibitory action of henna extract (Lawsonia inermis) and its main constituents
(lawsone, gallic acid, α-d-Glucose and tannic acid) on corrosion of mild steel in 1 M
HCl solution through electrochemical techniques and surface analysis. Maximum
inhibition efficiency (92.06 %) was obtained at 1.2 g/l henna extract. Inhibition
efficiency increases in the order: lawsone > henna extract > gallic acid > α-d-
Glucose > tannic acid. The corrosion inhibition of 2-hydrazino-4,7-
dimethylbenzothiazole on low carbon steel in industrial water has been investigated by
Badiea and Mohana [165] at different temperatures and fluid velocities at different
concentrations of the inhibitor using mass loss, potentiodynamic polarization and
electrochemical impedance spectroscopy measurements.
Different electrochemical methods have been employed by da Trindade and

Gonçalves [166] in order to confirm the ability of caffeine (1,3,7-trimethylxanthine) to
adsorb to low-carbon steel in ethanol solutions and thereby inhibit the corrosion
process. The presence of the adsorbed organic compound on low-carbon steel electrode
surface was confirmed by comparing the voltammograms, Tafel plots and EIS curves of
the electrode in the absence and presence of caffeine. The inhibition performance of
3,5-bis(4-methoxyphenyl)-4-amino-1,2,4-triazole (4-MAT) on mild steel in normal
hydrochloric acid medium at 30 °C was tested by Bentiss et al. [167] using weight loss,
potentiodynamic polarization and electrochemical impedance spectroscopy (EIS)
techniques. 4-MAT inhibits the acidic corrosion even at very low concentration,
reaching a value of inhibition efficiency up to 98 % at the concentration of 3 × 10−4 M.
Influence of hydrodynamic conditions on the corrosion of St52-3 type steel rotating disc
electrode (RDE) in 3.5 % NaCl and its corrosion inhibition using K2HPO4 have been
studied by Ashassi-Sorkhabi and E. Asghari [168].
The corrosion inhibition behavior of benzotriazole (BTZ), Na3PO4 (SP) and their
mixture on carbon steel in 20 wt.% (0.628 mol l−1) tetra-n-butylammonium bromide
aerated aqueous solution was investigated by Liu et al. [169] using weight-loss test,
potentiodynamic polarization measurement, electrochemical impedance spectroscopy
48
and scanning electron microscope/energy dispersive X-ray techniques. The results

revealed that inhibitor mixtures have shown synergistic effects at lower concentration of
inhibitors. At 2 g l−1 BTA and SP showed optimum enhanced inhibition compared with
their individual effects. Shukla [170] and co-workers studied the corrosion inhibition of
mild steel in 1 M HCl solution by cefotaxime sodium by Tafel polarization,
electrochemical impedance spectroscopy (EIS) and weight loss measurements. The
inhibitor showed 95.8 % inhibition efficiency at the optimum concentration of 300 ppm.
Mahdavian and Attar [171] studied the corrosion inhibition of some metal
acetylacetonate complexes including Co(acac)2, Cu(acac)2, Mn(acac)2 and Zn(acac)2
using electrochemical impedance spectroscopy (EIS) in 3.5 % NaCl for mild steel. The
results were compared to zinc potassium chromate (ZPC) solution in 3.5 % NaCl.
Corrosion inhibition of these metal complexes followed the order:
ZPC > Co(acac)2 > Zn(acac)2 > Mn(acac)2 while Cu(acac)2 displayed corrosion catalytic
activity. Liua et al. [172] studied the inhibitory behaviour of 2-undecyl-1-aminoethyl
imidazoline (AEI-11) and 2-undecyl-1-aminoethyl-1-hydroxyethyl quaternary
imidazoline (AQI-11) on CO2 corrosion of N80 mild steel in single liquid phase and
liquid/particle two-phase flow using weight loss, linear polarization, potentiodynamic
polarization, EIS methods and SEM observations. In both phases, AQI-11 exhibited
better inhibition ability than AEI-11 due to the polycentric adsorption sites on its
structure.
Zhang and Hua [173] investigated the acid corrosion inhibition process of mild
steel in 1 M HCl by 1-butyl-3-methylimidazolium chloride (BMIC) and 1-butyl-3-
methylimidazolium hydrogen sulfate ([BMIM]HSO4) using electrochemical impedance,
potentiodynamic polarization and weight loss measurements. For both inhibitors, the
inhibition efficiency increased with increase in the concentration of inhibitor, and
effectiveness of the two inhibitors are in the order [BMIM]HSO4 > BMIC. The
inhibition behaviour of 2-undecyl-1-ethylamino-1-methylbenzyl quaternary imidazoline
(2UMQI) and KI on mild steel in 1 M H2SO4 solutions was investigated by Okafor and
Zheng [174] at 25 °C using electrochemical methods. Inhibition efficiency of 2UMQI
was enhanced by the addition of iodide ions. In the presence of KI, the potential of
unpolarization, was observed to increase with KI concentration. The synergistic effect
of iodide ions and benzisothiozole-3-piperizine hydrochloride (BITP) on the corrosion
inhibition of mild steel in 0.5 M H2SO4 solution has been studied by Pavithra et al.
49
[175] using both chemical and electrochemical methods. The BITP showed maximum
inhibition efficiency of 93 % in HCl media whereas its inhibition efficiency in sulphuric
acid is about 85 %. Hegazy et al. [176] synthesized, characterized and tested novel
cationic gemini surfactants namely: bis(p-(N,N,N-octyldimethylammonium
bromide)benzylidene)benzene-1,4-diamine (I), bis(p-(N,N,N-decyldimethylammonium
bromide)benzylidene)benzene-1,4-diamine (II), and bis(p-(N,N,N-
dodecyldimethylammonium bromide)benzylidene)benzene-1,4-diamine (III) as
corrosion inhibitors for carbon steel in 1 M HCl solution. The obtained results showed
that, the synthesized inhibitors are excellent inhibitors for carbon steel in 1 M HCl
solution.
Two series of cationic Schiff base surfactants namely: 2-(benzylideneamino)-3-

(2-oxo-2-alkoxyethyl)-1,3-benzothiazol-3-ium bromide and 2-[(4-
methoxybenzylidene)amino]-3-(2-oxo-2-alkoxyethyl)-1,3-benzothiazol-3-ium bromide
were prepared by Negm et al. [177] and their structures were confirmed using elemental
analyses, FTIR, and 1H NMR spectra. The surface activity of the synthesized Schiff
bases showed their tendency towards adsorption at the interfaces. Nam and Kim [178]
examined the effect of niobium (Nb) addition on the electrochemical properties of low
alloy steel using electrochemical techniques in 10 wt.% sulfuric acid solution as well as
surface analysis techniques. These results suggest that the interaction of elements
improves the corrosion resistance of low alloy steel by the formation of Nb, C, S, P, and
Fe products on the surface. Ionic liquids with chemical 1,3-dioctadecylimidazolium
bromide and N-octadecylpyridinium bromide were synthesized by Likhanova et al.
[179] using conventional and microwave-assisted reactions, respectively. Ionic liquids
were tested as corrosion inhibitors and polarization curves displayed corrosion
protection efficiency between 82 % & 88 % at 100 ppm for mild steel in 1 M aqueous
solution of sulfuric acid.
Adsorption of four derivatives of piperidinylmethylindoline-2-one on mild steel

surface in 1 M HCl solution and its corrosion inhibition properties have been studied by
Ahamad et al. [180] using a series of techniques such as polarization, electrochemical
impedance spectroscopy (EIS), weight loss and quantum chemical calculation methods.
Soltani et al. [181] studied the inhibition effect of four double Schiff bases on the
corrosion of mild steel in 2 M HCl by polarization, electrochemical impedance
spectroscopy (EIS) and weight loss measurements. Quantum chemical calculations have
50
been performed. Several quantum chemical indices were calculated and correlated the
corresponding inhibition efficiencies. A cationic gemini-surfactant, namely 1,4-bis (1-
chlorobenzyl-benzimidazolyl)-butane (CBB) was synthesized and its inhibitory effect
on the corrosion of mild steel in 0.5 M HCl solution was investigated by Wang et al.
[182] using weight loss and electrochemical techniques. The results showed that CBB
acts as an excellent corrosion inhibitor in 0.5 M HCl by suppressing simultaneously
cathodic and anodic processes via chemical adsorption on the surface of steel, which
followed the Langmuir adsorption isotherm. Obot et al. [183] synthesized 2,3-
diphenylbenzoquinoxaline (2,3DPQ) and assessed its inhibitory action on the corrosion
of mild steel in 0.5 M H2SO4 by weight loss method at 30 °C. The results of the
investigation showed that this compound has excellent inhibitory properties for steel
corrosion in sulphuric acid. Quantum chemical calculations were employed to give
further insight into the mechanism of inhibition action of 2,3-DPQ. Singh and Quraishi
[184] studied the adsorption and inhibition effect of cefazolin on mild steel in 1 M HCl
between 308 & 338 K using weight loss, EIS, potentiodynamic polarization and atomic
force microscopy techniques. The results showed that inhibition efficiency increases
with increase in inhibitor concentration.
The corrosion inhibition efficiencies of two crown type polyethers, namely

dibenzo-bis-imino crown ether (C-1) and dibenzo-diaza crown ether (C-2) which are
macrocyclic Schiff base and its reduced form (macrocyclic amine), respectively, for the
steel in 1 M H2SO4 have been investigated by Hasanov et al. [185] using Tafel
extrapolation and linear polarization methods. The obtained results of these calculations
for the compounds were found to be consistent with the experimental findings. Obot et
al. [186] tested acenaphtho [1,2-b] quinoxaline (AQ) as a novel corrosion inhibitor for
mild steel in 0.5 M H2SO4 solution using chemical technique at 30 °C. AQ acts as an
effective inhibitor for mild steel in acidic medium. Inhibition efficiency increased with
increasing concentration of AQ. A zero-order kinetics relationship with respect to mild
steel was obtained with and without AQ from the kinetic treatment of the data. DFT
study gave further insight into the mechanism of inhibition action of AQ. The inhibitory
effect of novel nonionic surfactants on the corrosion of carbon steel (CS) in 1 M HCl
was studied by Hegazy and Zaky [187] at different temperatures (20–60 °C) by weight
loss, electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization
methods. The CS surface morphology was investigated by SEM. The obtained results
51
showed that the prepared non-ionic surfactants are excellent inhibitors in 1 M HCl, and
the inhibition efficiency increases with the increase in inhibitor concentration and
temperature.
The inhibition ability of 4,4-dimethyloxazolidine-2-thione (DMT) for mild steel

corrosion in 1 M HCl solution at 30 °C was studied by Musa et al. [188] using
potentiodynamic polarization, electrochemical impedance spectroscopy (EIS) technique,
and scanning electron microscopy (SEM). Results showed that DMT performed good
inhibiting effect for the corrosion of mild steel in 1 M HCl solution and inhibition
efficiency is higher than 82 % at 4 × 10−3 M of DMT. Acetyl thiourea chitosan polymer
(ATUCS) has been synthesized and evaluated as corrosion inhibitor by Fekry and
Mohamed [189]. The electrochemical behavior of mild steel in naturally aerated 0.5 M
H2SO4 acid containing different concentrations of ATUCS has been studied by
potentiodynamic polarization, electrochemical impedance spectroscopy (EIS)
measurements and surface examination via scanning electron microscope (SEM)
technique. Electrochemical impedance spectroscopy measurements under open-circuit
conditions confirmed well polarization results. ATUCS has shown very good inhibition
efficiency in 0.5 M sulphuric acid solution and reaches to 94.5 % efficiency for
0.76 mM concentration. Negm et al. [190] examined the effects of two biodegradable
corrosion inhibitors derived from vanillin and aminophenol (Meta: VPAP and Para:
VOAP) on the corrosion of carbon steel in 1 M HCl solution. The geometry of the
inhibitors showed that VPAP has slightly higher corrosion inhibition efficiency than
VOAP. The inhibitors showed good biodegradability in the environment that is within
28 days they were completely degraded.
Nataraja et al. [191] investigated the inhibition potential of ziprasidone for the
corrosion of steel in 1 M HCl and 0.5 M H2SO4 using weight loss, polarization,
electrochemical impedance spectroscopy and quantum chemical methods. Ziprasidone
is composed of benzisothiozole-3-piperizine (BITP) and an indole moiety. The results
showed that nearly 10 times lower concentration of ziprasidone showed the same
efficiency that was rendered by BITP. This is related to the planarity of ziprasidone
molecule, potential adsorption sites and extensive distribution of LUMO orbitals on
indole moiety which cause larger back donation. Inhibitive performance of some
synthesized thiophenol derivatives on the corrosion behavior of mild steel in 0.1 M HCl
solution was investigated by Kosari et al. [192] using electrochemical techniques,
52
quantum chemical calculations and optical microscopy. Inhibitor molecules directly get
adsorbed at surface on the basis of donor–acceptor interactions between π-electrons of
benzene, sulfur and nitrogen atoms and the vacant d-orbitals of iron atoms. The
inhibitive effect of a newly synthesized imidazoline phosphate against Q235 steel and
its adsorption behavior were investigated by Zhang et al. [193] in 1 M HCl solution
using weight-loss, potentiodynamic polarization and electrochemical impedance
spectroscopy (EIS) techniques. The quantum chemistry calculations exhibited that the
imidazoline ring and heteroatoms (N, O, and P) were the active sites of inhibitor.
The inhibition effect of three pyrazine derivatives such as 2-methylpyrazine

(MP), 2-aminopyrazine (AP) and 2-amino-5-bromopyrazine (ABP) on the corrosion of
cold rolled steel (CRS) in 1 M H2SO4 solution was studied by Li et al. [194] using
weight loss, potentiodynamic polarization and electrochemical impedance spectroscopy
(EIS) methods. The results showed that all pyrazine compounds are good inhibitors, and
the inhibition efficiency follows the order: ABP > AP > MP. The corrosion inhibition
effect of 2-[4-(methylthio) phenyl] acetohydrazide (HYD), 2-{[4-(methylthio) phenyl]
acetyl} hydrazinecarbothioamide (TAD) and 5-[4-(methylthio) benzyl]-4H-1,2,4-
triazole-3-thiol (TRD) on steel in 1 M HCl was investigated by Nataraja et al. [195]
using mass loss and electrochemical methods. The efficiency stands in the order
TRD > TAD > HYD, and is confirmed by the Quantum chemical studies. Singh et al.
[196] studied the inhibitory effect of two Schiff bases on the corrosion of the mild steel
in 1 M HCl using electrochemical impedance spectroscopy and Tafel polarization
measurements. It is suggested that the effects of Schiff bases depend on concentrations
and the molecular structures. Popova [197] and co-worker investigated seven
quaternary ammonium bromides of different heterocyclic compounds as corrosion
inhibitors of mild steel in 1 M HCl using gravimetric and polarization techniques. For
comparison, gravimetric experiments were carried out in 1 M H2SO4 as well. The
inhibition efficiency was found to depend on both concentration and molecular structure
of the inhibitor.
The influences of a benzimidazole derivative, namely 1,8-bis (1-chlorobenzyl-

benzimidazolyl)-octane (CBO) on the corrosion behaviour of mild steel in different
concentrations HCl solutions were studied by Wang et al. [198] using weight loss,
potentiodynamic polarization, electrochemical impedance spectroscopy (EIS)
measurements and SEM observations. The results showed that CBO acted as an
53
excellent and a mixed-type inhibitor via strongly chemical adsorption onto mild steel
surface to suppress simultaneously both anodic and cathodic processes according to the
Langmuir adsorption isotherm. The inhibition effect of triazolyl blue tetrazolium
bromide (TBTB) on the corrosion of cold rolled steel (CRS) in 1 M HCl and 0.5 M
H2SO4 solution was investigated for the first time by Li et al. [199] using weight loss,
potentiodynamic polarization and electrochemical impedance spectroscopy methods.
The results showed that TBTB is a very good inhibitor, and is more efficient in 1 M
HCl than in 0.5 M H2SO4. Obot et al. [200] studied the anti-corrosive effect of xanthone
(XAN) on the corrosion of mild steel in 0.5 M H2SO4 by gravimetric and UV–visible
spectrophotometric methods between 303 & 333 K. Results obtained revealed that XAN
performed excellently as a corrosion inhibitor for mild steel in sulphuric acid. Quantum
chemical calculations have been performed using DFT, and several quantum chemical
indices were calculated and correlated with the inhibitory effect.
The corrosion inhibition properties of ceftadizime (CZD) on mild steel corrosion

in HCl solution were analyzed by Singh et al. [201] using electrochemical impedance
spectroscopy, potentiodynamic polarization and gravimetric methods. The experimental
data showed a frequency distribution and therefore a modeling element with frequency
dispersion behaviour and a constant phase element (CPE) have been used. 2-
Aminothiazole (AT) was polymerized by Solmaz [202] using electrochemical technique
on mild steel electrode from 0.01 M monomer containing 0.3 M ammonium oxalate
solution. The results obtained indicated that, the polymer film adherent to the steel
surface. The polymer film gives good corrosion protection against the attack of
corrosive environment. The inhibitory action of 2-mercapto benzimidazole (2MBI) on
mild steel in 1 M hydrochloric acid has been investigated by Benabdellah et al. [203] at
308 K using weight loss measurements and electrochemical techniques. Inhibition
efficiency increases with 2MBI concentration to attain 98 % at 10−3 M.
Palomar-Pardave et al. [204] investigated the corrosion inhibition efficiency of

2-amino 5-alkyl 1,3,4 thiadiazole compounds with different alkyl chain lengths, namely,
2 ethyl, 3 n propyl, 5 n penthyl, 7 hepthyl, 11 undecyl and 13 tridecyl in the system,
steel/1 M H2SO4. The results showed that the inhibition mechanism involves blockage
of steel surface by inhibitor molecules by Langmuir-type adsorption process and the
alkyl chain length plays an important role in the inhibition efficiency of the synthesized
inhibitors. The inhibitory effect of three novel nonionic surfactants, 2-((alkylimino)
54
methyl)phenyl bis(53- hydroxy-3,6,9,12,15,18,21,24,27,30,33,36,39,42,45,48,51

heptadecaoxatripentacontyl) phosphate (I–III), on the corrosion of carbon steel in
0.5 H2SO4 was studied by Hegazy et al. [205] using polarization, EIS and weight loss
measurements. It was found that all the inhibitors were effective and their inhibition
efficiency was significantly increased with increasing both concentration and
temperature. The adsorption behaviour of cefapirin (CFP) on mild steel in 1 M HCl
solution was studied by Singh et al. [206] using potentiodynamic polarization,
electrochemical impedance spectroscopy and weight loss techniques. The hydrophobic
character of MS increased with increasing concentration of CFP. The results showed
that CFP performed excellently as corrosion inhibitor for MS.
The inhibition performance of four benzylidine malononitriles (BMNs) on mild

steel in 1 M HCl was studied by Yadava et al. [207] using weight loss, potentiodynamic
polarization and electrochemical impedance spectroscopy techniques. The results of
quantum chemical calculations were correlated with experimental inhibition
efficiencies. The inhibition performance of cationic gemini-surfactant (CBB) and its co-
adsorption behavior with halides on mild steel in 0.25 M H2SO4 solution was studied by
Wang et al. [208] using weight loss and electrochemical techniques. Results showed
that the compound could effectively inhibit the mild steel corrosion and acted as a
mixed-type inhibitor by suppressing simultaneously anodic and cathodic reactions.
Mendes et al. [209] used quantum mechanical calculations based on the density
functional theory under periodic boundary conditions to construct a model for the
inhibition performance of imidazole on iron surface. It is shown that, at high coverage,
imidazole molecules form C–C intermolecular bonds creating a protective film, which
constitutes a hydrophobic medium and, consequently, prevents adsorption of water
molecules. 2-Thiohydantoin (2-THD) was investigated as a corrosion inhibitor of mild
steel in 0.1 M HCl solution by Yuce et al. [210] using potentiodynamic polarization,
electrochemical impedance spectroscopy, and linear polarization resistance
measurements. The results showed that 2-THD acts as a mixed type inhibitor in 0.1 M
HCl by suppressing simultaneously cathodic and anodic processes via physical
adsorption on the MS surface followed by the Langmuir adsorption isotherm.
Corrosion of carbon steel pipes and tanks by concentrated sulfuric acid: a review
was reported by Pimenta and Marques [211]. The inhibition effect of 3-(4-((Z)-indolin-
3-ylideneamino)phenylimino)indolin-2-one Schiff base (PDBI) on mild steel corrosion
55
in 1 M HCl solution was studied by Singh [212] using potentiodynamic polarization

curves, weight loss, electrochemical impedance spectroscopy and linear polarization
resistance. PDBI has remarkable inhibition efficiency on the corrosion of mild steel in 1
M HCl solution. John and Joseph [213] studied the interaction and corrosion properties
of three different 1,2,4-triazole precursors on mild steel in 1 M hydrochloric acid by
polarization, EIS, adsorption, surface studies and computational calculations at 300 K.
Electrochemical and theoretical studies agree fairly well with each other. The results
showed that 4-(4-(dimethylamino)benzylideneamino))-4H-1,2,4-triazole-3,5-
diyl)dimethanol (DBATD) is a better inhibitor than (4-(benzylideneamino)-4H-1,2,4-
triazole-3,5-diyl) dimethanol (BATD) and 4-amino-4H, 3,5-di(methoxy)-1,2,4,triazole
(ATD). Four environmentally friendly corrosion inhibitors were derived from vanillin
by Negm et al. [214] and evaluated gravimetrically and electrochemically as corrosion
inhibitors for carbon steel in 1 M HCl. The inhibition efficiencies of these inhibitors
depend on their concentration and the chemical structures. Corrosion inhibition of four
diquaternary amines such as N,N-pentane-2,4-diylidenedipyridin-4-amine (NDSI), N,N-
(3-benzylidenepentane-2,4-diylidene)dipyridin-4-amine (NBDSI), N,N-[3-(4-
methoxybenzylidene)pentane-2,4-diylidene]dipyridin-4-amine (NMDSI) and N,N-[3-
(4-chlorobenzylidene)pentane-2,4-diylidene]dipyridin-4-amine (NCDSI) on carbon
steel was investigated by Negm et al. [215] using gravimetric measurements,
polarization and electrochemical impedance spectroscopy (EIS).
Moretti et al. [216] tested the use of 2-butyl-hexahydropyrrolo[1,2-b ][1,2]

oxazole (BPOX) as corrosion inhibitor of mild steel with a polished or a pre-corroded
(for 2 h) surface in 0.5 M aerated hydrochloric acid in the 30–60 °C temperature range.
The inhibition effect of new heterocyclic compounds, namely 2-aryl-benzothiazin-3-one
(P1) and 3-aryl-benzothiazin-2-one (P2) on mild steel corrosion in 1 M HCl was
investigated by Ghailane et al. [217] using electrochemical measurements. It is also
found that the inhibition of P1 is greater than P2. The obtained results showed that the
experimental and theoretical studies agree well and confirm that P1 is the better
inhibitor. Corrosion inhibition of carbon steel in normal hydrochloric acid solution at
30 °C by new 4-amino-1,2,4-triazole derivative, namely 3,5-bis(2-thienylmethyl)-4-
amino-1,2,4-triazole (2-TMAT) has been studied by Tourabi et al. [218] using
electrochemical impedance spectroscopy (EIS) and polarization techniques.
56
Experimental results have shown that 2-TMAT showed good corrosion inhibition and
the inhibition efficiency increased with increase in inhibitor concentration.
The inhibition behavior of imidazole (IM) and 2-phenyl-2-imidazoline (2-PI) for

AA5052 was investigated by He et al. [219] using weight loss and electrochemical
method, contact angle measurements and scanning electron microscopy. The results
showed that IM and 2-PI can inhibit the corrosion of AA5052 and the inhibition
efficiency of 2-PI is higher. Cao et al. [220] studied the adsorption behavior and
inhibition mechanism of 2-aminomethyl benzimidazole (ABI), bis(2-
benzimidazolylmethyl) amine (BBIA) and tri-(2-benzimidazolylmethyl) amine (TBIA)
on the surface of mild steel by quantum chemical calculations and molecular dynamics
(MD) simulations. It was found that the three molecules showed similar ability to
donate electrons while the difference in inhibition performance should mainly be
attributed to the difference in accepting electrons. The application of 2-amino-4-methyl-
thiazole (2A4MT) as corrosion inhibitor for mild steel protection was investigated by
Yuce et al. [221] in 0.5 M HCl solution. Electrochemical impedance spectroscopy and
potentiodynamic measurements were used at various concentrations and temperatures.
The high corrosion inhibition efficiency of 2A4MT was associated with its strong
adsorption as a barrier film on the MS surface. Kosari et al. [222] examined the
inhibitive performance of two pyridine derivatives namely pyridine-2-thiol (P2T) and 2-
pyridyl disulfide (2PD) for mild steel corrosion under stagnant condition and
hydrodynamic flow in HCl solution at 25 °C. P2T and 2PD reveal 98 % efficiency in
200 mg/L concentration at stagnant condition.
57
SECTION - V: SCOPE OF THE PRESENT WORK
Corrosion is a destructive phenomenon which affects almost all metals.

Although iron was not the first metal used by man, it is certainly the most used and
must have been one of the first in which serious corrosion problems were encountered.
From the literature survey it is clear that there is great need for more research in the
field of corrosion of metals in general and mild carbon steel in particular due to its
practical importance. Mild steel is widely used in many industries because of its
economically cost-effectiveness and easy fabrication. However, it is subject to corrosion
under aggressive environmental conditions especially during acid cleaning or pickling.
Therefore in the present study greater attention was bestowed on mild carbon steel.
Addition of corrosion inhibitors is one of the requirements to protect metals

and alloys against attack of corrosion in many industrial environments. Hence,
development of new corrosion inhibitors based on organic/inorganic compounds
containing nitrogen, oxygen, sulphur and phosphorous atoms is of growing interest in
the field of chemical industries to solve the corrosion problems and to reduce the
economic cost of equipments. The thesis aims at the application of different organic
compounds as corrosion inhibitors. The present work was designed to understand the
inhibition mechanism of corrosion inhibitors on mild steel in acid medium. The
behavior of mild steel in the presence of inhibitive formulation was investigated by
steady-state electrochemical measurements. The mechanism of metal corrosion is the
prime priority of the research which will be achieved by evaluating the adsorption
thermodynamic parameters.
The present work involves the investigation of corrosion and corrosion inhibition
of mild steel in acid medium using some of the inhibitors such as 2-methyl-2-{4-[5-(6-
methyl pyridin-2-yl)-[1,3,4]oxadiazol-2-yl]-phenyl}-propionitrile (6-MMOPP), 2-
methyl-6-(5-pyridin-4-yl-[1,3,4]oxadiazol-2-yl)-pyridine (5-MPOP), 2-[5-(4-bromo-
phenyl) [1,3,4]oxadiazol-2-yl]-6-methyl-pyridine (4-BPOMP), 6-methyl-4-morpholin-
4-yl-2-oxo-1,2,3,4-tetrahydro-pyrimidine-5-carboxylic acid ethyl ester (P1), 6-methyl-
4-morpholin-4-yl-2-thioxo-1,2,3,4-tetrahydro-pyrimidine-5-carboxylic acid ethyl ester
(P2), 6-methyl-4-morpholin-4-yl-2-oxo-1,2,3,4-tetrahydro-pyrimidine-5-carboxylic acid
hydrazide (P3), 6-methyl-4-morpholin-4-yl-2-thioxo-1,2,3,4-tetrahydro-pyrimidine-5-
carboxylic acid hydrazide (P4), 6-bromo-2-(4-fluoro-phenyl)-1H-benzoimidazole
58
(BFB), 2-[3-(6-bromo-1H-benzoimidazol-2-yl)-phenyl]-2-methyl-propionitrile (BPMP),

6-bromo-2-(3,4-dimethoxy-phenyl)-1H-benzoimidazole (BDB), 8-bromo-5-
morpholino-3-(4-propylphenyl)-[1,2,4]triazolo[4,3-c]pyrimidine (5a), 8-bromo-3-(2-
fluoro-3-methoxyphenyl)-5-morpholino-[1,2,4]triazolo[4,3 c]pyrimidine (5b), 8-bromo-
3-(2-fluoro-4,5-dimethoxy-phenyl)-5-morpholin-4-yl-[1,2,4]triazolo[4,3-c]pyrimidine
(5c), (3-methoxy-phenoxy)-acetic acid hydrazide (3-MAH), 4-amino-5-(3-methoxy-
phenoxymethyl)-4H-[1,2,4]triazole-3-thiol (4-AMTT) and 3-(3-methoxy-
phenoxymethyl)-6-phenyl-7H-[1,2,4]triazolo[3,4-b][1,3,4]thiadiazine (3-MPTT). The
behavior and mechanisms of the inhibitors have been investigated in the temperature
range of 303-333 K at different concentrations of inhibitors using mass loss,
potentiodynamic polarization and electrochemical impedance spectroscopy (EIS)
techniques. Scanning Electron Microscopy (SEM) EDAX and FT-IR spectral studies
were also used to analyze the surface adsorbed film.
The frame work of the investigation is based on the following objectives:

1. Proposed to synthesize novel nitrogen containing heterocyclic compounds.
2. Proposed to characterize newly synthesized compounds using spectroscopic
methods such as elemental analysis, FT-IR, 1H-NMR, 13C-NMR and LC-MS.
3. Proposed to carry out the antioxidant assay for newly synthesized compounds.
4. Proposed to establish the synthesized compounds as corrosion inhibitors for
carbon steel in acid medium.
5. Proposed to find the optimum conditions of temperature of the environment and
concentration of inhibitors.
6. Proposed to evaluate the adsorption thermodynamic parameters.
7. Proposed to establish the behavior of corrosion inhibitors on carbon steel.
8. Proposed to identify the protective layer that formed on the metal surface.
59
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Corrosion Inhibitors

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Chapter I Introduction to corrosion and corrosion inhibitors

INTRODUCTION TO CORROSION AND CORROSION INHIBITORS

Fig. 1.1: Oil pipeline corrosion.

Fig. 1.2: Gas pipeline corrosion.

Fig. 1.3: Inner view of corroded pipeline.

Pickling is a metal surface treatment used to remove impurities such as stains,

Fig. 1.4: Stainless steel sheet before and after pickling.

Fig. 1.5: Microbial corrosion in pipeline.

In oil production industries, economic losses and ecological damage caused by

Fig. 1.6: Corrosion in boilers.

There are five good reasons to study corrosion.

destroyed by corrosion and how they must be preserved by applying corrosion

1.1.2. Theories and mechanism of corrosion

1.1.2.1. Local cell theory

According to De la Rive [6] corrosion occurs because of the creation of a large

 Stress from welding or other works.

 Compositional differences at the metal surface.

Cathodic site Anodic site

Fig.1.7: Model for local cell theory of corrosion.

1.1.2.2. Wagner and Trauds’ theory

Although corrosion is a complicated process, it can be most easily comprehended

Fig. 1.8: Reaction occurring during the corrosion of steel.

The reaction takes place as follows:

Anodic reaction: Fe o  Fe 2   2 e  (1.1)

In the absence of oxygen, H+ participates in the reaction at the cathode instead of

Fe 2   2OH   FeOH 2  (1.4)

4 FeOH 2  O2  2 H 2 O  4 FeOH 3 (1.5)

2 FeOH 3  Fe2O3  3H 2O (1.6)

FeOH 3  FeO (OH )   H 2 O (1.7)

1.1.3. Classification of corrosion

There is no universally accepted classification for corrosion, but the following

1.1.3.1. Uniform or general corrosion

1.1.3.2. Galvanic corrosion

Galvanic corrosion is an electrochemical action of two dissimilar metals in the

1.1.3.3. Localized corrosion

 Crevice corrosion: It is similar to pitting corrosion in a stagnant electrolyte after its

Fig. 1.10: Crevice corrosion of mild steel connectors.

 Filiform corrosion: It is basically a special type of crevice corrosion, sometimes

 Pitting corrosion: Pitting Corrosion is "self-nucleating" crevice corrosion, starting

Fig. 1.11: Pitting corrosion in mild steel pipes.

 Intergranular corrosion: Intergranular corrosion is a localized form of corrosion.

1.1.3.4. Stress corrosion cracking (SCC)

Fig. 1.12: Stress corrosion cracking of mild steel.

1.1.3.5. Erosion corrosion

1.1.4. Rate of corrosion

1.1.5. Factors influencing the corrosion rate

1.1.5.1. Nature of the metal

E = Ecathodic − Eanodic (1.8)

In corrosion processes where hydrogen evolution is the cathodic reaction,

1.1.5.2. Surface state of the metal

1.1.5.3. Protective film

1.1.5.4. pH of the medium

In general, rate of corrosion is higher in acid pH than in neutral and alkaline

varying pH conditions of the medium, a corroding surface may exhibit activity,

1.1.5.5. Temperature of the medium

Corrosion is an activation-controlled chemical reaction, the rate of which is

1.1.5.6. Effect of dissolved oxygen

SECTION - II: CORROSION INHIBITORS

An inhibitor is a chemical substance or combination of substances which when

Corrosion inhibitors have been found to be effective and flexible means of

effective inorganic inhibitors are chromates, nitrites, silicates, carbonates, phosphates

In order to avoid or reduce the corrosion of metallic materials, inhibitors used in

a) It must give good corrosion protection at a very low concentration of inhibitor.

1.2.2. Mechanism of corrosion inhibition