INVESTIGATION OF THE INHIBITIVE OF ACTION OF NATURAL

SURFACTANT (ACACIA CONCINNA) ON CORROSION OF MILD

STEEL

1
 1.INTRODUCTION

1.1 DEFINITION OF CORROSION

Corrosion is the process of disintegration of a metal by its surrounding chemicals

by a chemical reaction on the surface of the metal. Corrosion is an oxidation process and
it causes damage of metal. Formation of rust on the surface of iron and formation of
green film on the surface of copper are considered as best examples for corrosion
process. Corrosion is a costly and natural course of destruction like to rnados,
earthquakes, floods and volcanic eruptions with one major difference. Corrosion of
metals can be prevented or at least controlled.
There are several definitions for corrosion have been given as follows:
Corrosion can also be defined as the degradation of a material as a result of a
reaction with its environment. Degradation denotes deterioration of physical properties of
the material.
Corrosion of metals is well defined as the spontaneous destruction of metals in the
course of their bio chemical, chemical and electro chemical interactions with the
environment [1], [2].Hence, it is accurately there verse of extraction of metal from ores.
In most of the environments the metals are not stable, but tend to revert to compounds
which are more stable, a process which is known as corrosion. The same amount of
energy needed to extract metals from their minerals is emitted during the chemical
reactions that produce corrosion [3]. Corrosion is derived from the Latin word “corrosus”
which is known as gnawed away.
Corrosion is there action of a solid with its environment [4]. Now a days it is
required to give more importance to corrosion because of the huge use of metals in all
fields of technology.
Corrosion is mainly the result of interaction between materials and their environment.
The term corrosion was restricted only to metals and their alloys and it did not
incorporate ceramics, polymers, composites and semiconductors in its regime. The term
corrosion now covers all types of natural and man-made materials including biomaterials
and nanomaterials and it is not limited to metals and alloys alone.

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1.2 TYPES OF CORROSION

1.2.1.GENERAL ATTACK CORROSION:

General attack corrosion is also known as uniform attack. corrosion. This is the most
common type of corrosion and is caused by a chemical or electrochemical reaction that
results in the deterioration of the entire exposed surface of a metal. Ultimately, the metal
deteriorates to the point of failure.

General attack corrosion accounts for the greatest amount of metal destruction by
corrosion but is considered as a safe form of corrosion, due to the fact that it is
predictable, manageable and often preventable.

1.2.2 LOCALIZED CORROSION

Localized corrosion specifically targets one area of the metal structure. Localized
corrosion is classified as one of three types:

 PITTING: Pitting results when a small hole, or cavity, forms in the metal, usually
as a result of de-passivation of a small area. This area becomes anodic, while part
of the remaining metal becomes cathodic producing a localized galvanic reaction.
The deterioration of this small area penetrates the metal and can lead to failure.
This form of corrosion is often difficult to detect due to the fact that it is usually
relatively small and may be covered and hidden by corrosion-produced
compounds
 CREVICE CORROSION: Similar to pitting, crevice corrosion occurs at a
specific location. This type of corrosion is often associated with a stagnant micro-
environment, like those found under gaskets and washers and clamps. Acidic
conditions or a depletion of oxygen in a crevice can lead to crevice corrosion.

 FILIFORM CORROSION: Occurring under painted or plated surfaces when

water breaches the coating, filiform corrosion begins at small defects in the
coating and spreads to cause structural weakness.

1.2.3 GALVANIC CORROSION

Galvanic corrosion or dissimilar metal corrosion occurs when two different metals
are located together in a corrosive electrolyte. A galvanic couple forms between the two
metals where one metal becomes the anode and the other the cathode. The anode or
sacrificial metal corrodes and deteriorates faster than it would alone while the cathode
deteriorates more slowly than it would otherwise.

Three conditions must exist for galvanic corrosion to occur they are

 Electrochemically dissimilar metals must be present

 The metals must be in electrical contact, and

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  The metals must be exposed to an electrolyte

1.2.4 ENVIRONMENTAL CRACKING:

Environmental cracking is a corrosion process that can result from a combination

of environmental conditions affecting the metal. Chemical, temperature and stress related
conditions can result in the following types of environmental corrosion:

 Stress Corrosion Cracking (SCC)

 Corrosion fatigue
 Hydrogen-induced cracking
 Liquid metal embrittlement

1.2.5 FLOW-ASSISTED CORROSION (FAC)

Flow-assisted corrosion, or flow-accelerated corrosion, results when a protective

layer of oxide on a metal surface is dissolved or removed by wind or water, exposing the
underlying metal to further corroding and deteriorate.

 Erosion-assisted corrosion
 Impingement
 Cavitation

1.2.6 INTERGRANULAR CORROSION

Intergranular corrosion is a chemical or electrochemical attack on the grain

boundaries of a metal. It often occurs due to impurities in the metal, which tend to be
present in higher contents near grain boundaries. These boundaries can be more
vulnerable to corrosion than the bulk of the metal.

1.2.7 DE-ALLOYING

De-alloying or selective leaching, is the selective corrosion of a specific element in

an alloy. The most common type of de-alloying is dezincification of unstabilized brass
The result of corrosion in such cases is a deteriorated and porous copper.

1.2.8 FRETTING CORROSION

Fretting corrosion occurs as a result of repeated wearing, weight and vibration on an

uneven, rough surface. Corrosion resulting in pits and grooves occurs on the surface.
Fretting corrosion is often found in rotation and impact machinery, bolted assemblies and
bearings, as well as to surfaces exposed to vibration during transportation.

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1.2.9 HIGH-TEMPERATURE CORROSION
Fuels used in gas turbines, diesel engines and other machinery, which contain
vanadium or sulfates can during combustion form compounds with a low melting point.
These compounds are very corrosive towards metal alloys normally resistant to high
temperatures and corrosion including stainless steel. High-temperature corrosion can also
be caused by high-temperature oxidization, sulfidation and carbonization.

1.3 CORROSION INHIBITORS

Corrosion inhibitors can reduce, control or prevent reactions between a metal and
its surroundings when added to the medium in small quantities. For economy purpose,
inhibitors should be in effect at low concentrations.
In industries like oil and gas production and exploration, iron and steel industries,
petroleum refining, chemical manufacturing units [5] corrosion data base is important.
Corrosion is a main damaging process that results in destructive effects. Corrosion
produces gaping hole or cracks in aircraft, automobiles, gutters screens, boats, plumbing
and many other things prepared by metals. Corrosion is an unproductive phenomenon that
should be reduced. The major concern is the stability of materials and structures, many
studies have been carried out to improve an efficient means of corrosion control to extend
service life of existing structures and reduce corrosion damage in new structures [6].
Though corrosion inhibitors are considered as the most effective and flexible means of
corrosion control. it is very complicated to select an appropriate inhibitor for a particular
system because of the specificity of inhibitors and great variety of corrosion related
applications. Corrosion in metallic surfaces causes much concern with respect to material
loss, particularly in technological activities. The size, shape, orientation and electric
charge on the molecule decide the degree of adsorption and hence the effectiveness of the
inhibitor [7], [8], [9], [10].

1.4 GREEN CORROSION INHIBITOR : ACACIA CONCINNA

Many powerful techniques were used to measure corrosion inhibition such as
anodic or cathodic protection, oxidizing or phosphatizing treatment, coating layer on the
metal, the application of inhibitors, etc. have been used to reduce the corrosion of metal
[11], [12], [13], [14], [15].
As a contribution to the growing interest in environmental friendly
green corrosion inhibitors, this present study seeks to investigate the inhibiting effect of
shikakai extracts of Acacia Concinna (Shikakai Extract) on the corrosion of mild steel
in bore well water medium.

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1.4.1 ACACIA CONCINNA : CHEMICAL STRUCTURE

Figure 1: Structure of acaciac acid in the saponin of pods of Acacia concinna

1.4.2 CHEMICAL COMPOSITION

In commercial extract, when the plant is hydrolyzed it yields liperol, spinasterol,
aacacic acid, lactone, and the natural sugars glucose, arabinose and rhamnose. It also
contains hexacosanol, spinasterone, oxalic acid, tartaric acid, citric acid, succinic acid,
ascorbic acid, and the alkaloids calyctomine and nicotine.
Molecular formul : C30H50O2
Chemical Name : Acacia Concinna
FamilyName : Fabaceae
Common Name : Shikakai, Soap Pod

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 2. AIM AND SCOPE
2.1 AIM
 To investigate the effectiveness of inhibitor by weight loss method in the absence
and presence of Zinc sulphate
 To analyse the protective film by UV-Visible and Fluorescence spectroscopy.
 To suggest a possible mechanism for the corrosion inhibition pro

2.2 SCOPE OF THE PRESENT WORK

Corrosion is considered as the destructive disintegration of a metal by
electrochemical means in which a metal is damaged by a chemical reaction. General
pitting ultimately produce structural weakness and disintegration of the metal. Many
inhibitors are used to protect different materials especially metals against corrosion. The
inhibitors, which retard corrosion on metallic materials, are mixed material inhibitors,
surfactant inhibitors, inorganic inhibitors and organic inhibitors.

Natural products have been used to be effective corrosion inhibitors as they are
cost effective. They are inherently stable and non-toxic and show greater corrosion
inhibition properties comparing with simple organic molecules. Natural products as
corrosion inhibitors have many advantages such as high inhibition efficiency, low
toxicity, low price and easy production. The functional groups present in the Acacia
Concinna adsorbed on the metal surface and forming a protective film on the metal
surface and hence prevents corrosion of the metal.

The present study deals with the corrosion inhibition of mild steel in bore well
water by Acacia Concinna . The inhibitive action of Acacia Concinna combination with
zinc sulphate on the corrosion of carbon steel in bore well water has been studied by
weight loss and UV visible absorption and Flourescence spectroscopy. The results
suggest that acacia concinna can actually be used as a green corrosion inhibitor.

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 3. MATERIALS AND METHODS

3.1 PREPARATION OF THE MILD STEEL SPECIMENS

The mild steel specimens were chosen from the same sheet of the following
composition:

Elements C Mn P Si S Cr Ni Mo Fe
Composition 0.1 0.4 0.06 0.022 0.026 0.0020 0.018 0.012 Rest

Mild steel specimens of the dimensions 1.0 cm x 4.0 cm x 0.2 cm were polished to
mirror finish, washed with double distilled water, degreased with trichloroethylene, dried
and were used for the weight loss and surface examination studies. The mild steel
specimens were stored in a desiccators and used for all investigations.

3.2 CHEMICALS USED

AnalaR Samples of acacia concinna, , Zinc sulphate, were used for the
experimental investigations.

3.3 PREPARATION OF STOCK SOLUTIONS

3.3.1 ACACIA CONCINNA EXTRACT

1g of acacia concinna was dissolved in double distilled water and then made
up to 100 ml in a standard measuring flask.

3.3.2 ZINC SULPHATE SOLUTION

1.1 g of zinc sulphate was dissolved in double distilled water and made up to
250ml.

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3.4 PREPARATION OF ENVIRONMENTS

The various concentrations of inhibitors are prepared such as 20, 40, 60 and
80 ppm and the concentrations of Zinc sulphate ion are maintained as 50 ppm.

3.5 WEIGHT LOSS METHOD

3.5.1 DETERMINATION OF SURFACE OF THE MILD STEEL

SPECIMENS

The length, breadth and thickness of mild steel specimens, the radius of the
hole was determined with the help of vernier calipers of high precision and the surface
areas of the specimens were calculated.

3.5.2 WEIGHING THE SPECIMENS BEFORE AND AFTER

CORROSION

Weighing of the mild steel specimens before and after corrosion were carried
out using a digital balance.

3.5.3.DETERMINATION Of CORROSION RATE

The weighed specimens in triplicate were suspended by means of plastic

hooks in 100 ml beakers containing 100 ml of bore well water containing various
concentrations of the inhibitor in the absence and presence of Zinc sulphate for one day.
After one day immersion, the specimens were taken out, washed with distilled water,
running water, dried and weighed. From the change in weight of the specimens, corrosion
rates were calculated using the following equation 1.

Loss in weight (mg)

Corrosion rate = ----------------------------------------------------------------- (1)

Surface area of the specimen (dm2) x Period of immersion (days)

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The corrosion rate is expressed in mdd units [mdd = mgm/(dm2) (day)]

Corrosion inhibition efficiency (IE) was then calculated using the equation 2

IE = 100 [1-(W2 / W1)] % .............................. ( 2 )

Where,

W1 = Corrosion rate in the absence of inhibitor

W2 = Corrosion rate in the presence of inhibitor

3.5.4 SURFACE EXAMINATION STUDIES

The environments chosen for surface examination studies are given in Table
3.1. Among the several inhibitor combinations, the one which offered the highest IE
selected as the environment.

Table 3.1 PREPARATION OF THE VARIOUS ENVIRONMENTS

FOR SURFACE EXAMINATIONSTUDIES

Environment chosen
Inhibition
Acacia Concinna a)Bore well water
b)Acacia concinna (60ppm)
+ Zn2+ (50ppm) + Bore well water

3.5 UV-VISIBLE ABSORPTION SPECTRA OF SOLUTIONS

UV-visible absorption spectra are used to confirm the formation of Zn-

inhibitor complex and Fe2+-inhibitor complex. The spectrum is recorded using Cary
Eclipse Varian (Model U-3400) spectrophotometer.

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3.6 SURFACE ANALYSIS BY FLUORESCENCE SPECTROSCOPY

Fluorescence spectroscopy is a fast, simple and inexpensive technique which

interprets the fluorescence from a sample. The principle involved is using a beam of light,
generally ultraviolet light, that excites the electrons in molecules of certain compounds
and causes them to emit light. This spectroscopy measures the intensity of photons
emitted from a sample after it has absorbed photons. Fluorescence spectra of solutions
were recorded on a Hitachi F-4500 fluorescence spectrophotometer.

11
 4. RESULT AND DICSCUSSION

SYNERGISTIC EFFECT OF ACACIA CONCINNA AND ZINC

SULPHATE

4.1 ANALYSIS OFTHE RESULTS OF WEIGHT LOSS METHOD

Corrosion rates (CR) of mild steel surface [16] [17] [18] immersed in Bore well
water in the absence and presence of inhibitor (Acacia Concinna) are given in Tables 4.1
to 4.2. The inhibition efficiencies (IE) are also given in these Tables. The inhibition
efficiencies of the Acacia Concinna-zinc sulphate systems as a function of concentrations
of Acacia Concinna are shown in Figure 4.1.

It is observed from Table 4.1 that Acacia Cocinna shows some inhibition
efficiencies that is 60ppm of Acacia Concinna has 57% inhibition efficiency. As the
concentration of Acacia Concinna increases, the inhibition efficiency increases. This
is due to the fact that as the concentration of Acacia Concinna increases, the
2+
protective film (probably Fe -Acacia Concinna complex) formed on the metal
surface. At concentrations ≥80ppm of Acacia Concinna, the protection efficiency
decreases. It may be due to the fact that these molecules aggregate together to form
micelles. They are not uniformly adsorbed on the metal surface. Hence corrosion
inhibition efficiency decreases.

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Table 4.1 Corrosion rates (CR) in milligram per decimeter per day (mdd) of mild
steel immersed in bore well water in the presence and absence of Acacia Concinna-
2+
Zn system at various concentrations and the inhibition efficiencies (IE) obtained
by weight loss method

2+
Inhibitor system: Acacia Concinna-Zn (0 ppm)
Immersion period: One day

Acacia concinna ( ml) Zn2+(ppm) CR (mdd) IE%

0 0 127.27 -

20 0 68.18 47%

40 0 68.72 51%

60 0 54.54 57%

80 0 61.81 53%

2+
4.1.1 INFLUENCE OF ZN ON THE INHIBITION EFFICIENCIES
OF ACACIA CONCINNA
2+
The influence of Zn on the inhibition efficiencies of Acacia Concinna is given in
Table 4.1 and Table 4.2. It is observed that as the concentration of Acacia Concinna
increases the IE increases. Similarly for a given concentration of Acacia Concinna, IE
2+
increases as the concentration of Zn increases. At concentrations ≥80ppm of Acacia
Concinna ,the inhibition efficiency decreases .It may be due to the fact that these
molecules aggregate together to form micelles. They are not uniformly adsorbed on the
metal surface. Hence corrosion inhibition efficiently decreases. It is also observed that a
2+ 2+
synergistic effect exists between Acacia Concinna and Zn .For example, 50ppm of Zn
has 42% IE; 60ppm of Acacia Concinna has 57% IE. Interestingly their combination has
a high IE, namely 99%.
2+
In the presence of Zn more amount of Acacia Concinna is transported towards the
2+
metal surface. On the metal surface Fe -Acacia Concinna complex is formed on the
anodic sites of the metal surface. Thus the anodic reaction is controlled. The cathodic
-
reaction is the generation of OH ,which is controlled by the formation of Zn(OH)2 on the

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cathodic sites of the metal surface. Thus the anodic and cathodic reactions are controlled
2+
effectively. This accounts for the synergistic effect existing between Zn and Acacia
Concinna.

2+ -
Fe→Fe +2e (Anodic reaction)
2+ 2+ 2+
Fe + Zn -
Acacia Concinna complex →Fe -

2+
Acacia Concinna complex +Zn
- -
O2 + 2H2O + 4e → 4OH (Cathodic reaction)

2+ -
Zn + 2OH →Zn (OH) 2↓

Table 4.2 Corrosion rates (CR) in milligram per decimeter per day (mdd) of
mild steel immersed in bore well water in the presence and absence of Acacia
2+
Concinna -Zn system at various concentrations and the inhibition efficiencies
(IE) obtained by weight loss method

2+
Inhibitor system: Acacia Concinna -Zn (50 ppm)
Immersion period: One day

Acacia Concinna Zn2+ CR(mdd) IE%

(ppm)

0 0 1227.27 -

0 50 72.72 42%

20 50 8.18 93%

40 50 7.27 94%

60 50 0.90 99%

50
80 3.63 97%

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4.2 Analysis of the UV –Visible absorption spectra

UV-Visible spectroscopy is the direct and most sensitive

spectrophotometric method which is used to identify the formation of Fe2+- inhibitor

complex on the metal surface [19] [20]. The formation of complex between two
species in solution is recognized by the change in position of the absorption maximum
and change in the value of absorbance.

The UV-Visible absorption spectrum of an aqueous solution of Acacia

Concinna is shown in Figure 3.2 (a). A peak appeared at 466.4 nm. When freshly

prepared Fe2+ ion (FeSO4.7H2O) is introduced in to the solution the peak shifts to
502.4nm Figure 3.2(b). This is considered as Blue shift (shorter wave length).
Another peak appeared at 440 nm.
+
This suggests that a complex formed between Fe and Acacia Concinna.

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 466.4 nm

502.4 nm

Figure 4.2 UV-Visible spectrum of

(a)Aqueous solution of Acacia Concinna

2+
-
(b)Fe Acacia Concinna

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4.3 ANALYSIS OF THE FLUORESCENCE SPECTRA
2+
Fluorescence spectra have been used to determine the presence of Fe -Acacia
Concinna complex formed on the surface of the metal [24]. The fluorescence spectrum
2+
(λex=300nm) of the aqueous solution of Acacia Concinna combined with Fe ion is
shown in Figure 4.2 (a). The solution was emitted at 300nm. A peak appeared at 511.5
nm. The increase in wavelength of the emitted light indicates that the energy of the
absorbed light is higher than that of the emitted light. As a result of this the molecules go
to the excited state where they collide with the other molecules and lose their energy.
Then they return to the lowest energy level in the excited state. Then they return to the
ground state and emit a phot on emitting light at a longer wavelength of 511.5 nm. The
energy loss is due to the molecular collision in the excited state.
The fluorescence spectrum (λex=300nm) of the film formed on the metal surface
after immersion in the solution containing 60 ppm of Acacia Concinna is shown in Figure
2+
3(b). A peak appeared at 508nm .This peak matches with the peak of Fe -Acacia
2+
Concinna complex. Therefore it is concluded that Fe -Acacia Concinna complex is
formed on the metal surface. This film is responsible for the protective nature of the
2+
inhibitor system. Decrease in the intensity of the peak indicating that the Fe - Acacia
Concinna complex formed on the metal surface is in solid state. From the figure it is
observed that there is only a single peak is obtained which indicates that the complex
formed on the metal surface is homogeneous in nature.

Figure 4.3 Fluorescence spectra λex= 300 nm

2+
(a) Fe + aqueous solution of Acacia Concinna

(b) Film formed on metal surface after immersion in the solution containing 60 ppm
2+
of Acacia Concinna and 50ppm of Zn

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4.4 MECHANISM OF CORROSION INHIBITION
The corrosion resistance of mild steel in bore well water has been evaluated by
weight loss method. The formulation consisting of 200 ppm of Acacia Concinna and 50
2+
ppm of Zn shows 99% inhibition efficiency (IE) in controlling corrosion of mild steel
for one day immersion period. A synergistic effect exists between Acacia Concinna and
2+
Zn .UV-visible, Fluorescent spectral data indicate the possibility of formation of
protective layer on the metal surface.

The following corrosion inhibition mechanism was derived from the above results.
2+
• When the solution containing well water, 50 ppm Zn and 200 ppm of
2+
-
Acacia Concinna is prepared, there is formulation of Zn Acacia Concinna complex in
solution.
2+
• When mild steel is immersed in this solution, the Zn -
Acacia Concinna
complex diffuses from the bulk of the solution towards metal surface.
2+
• Zn -
Acacia Concinna complex diffuses from the bulk solution to the surface
2+
-
of the metal and is converted into a Fe Acacia Concinna complex, which is more stable
2+
-
than Zn Acacia Concinna.
2+ 2+
• On the metal surface Zn -
Acacia Concinna complex is converted into Fe -
2+
Acacia Concinna on the anodic sites, Zn is released.
2+ 2+ 2+
- →
Zn Acacia Concinna + Fe Fe2+ Acacia Concinna+ Zn
2+ -
• The released Zn combines with OH to form Zn (OH) 2 on the cathodic sites.
2+
Zn + 2OH-→ Zn (OH) 2↓
2+
• Thus the protective film consists of Fe -
Acacia Concinna complex
and Zn(OH).

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 5. SUMMARY AND CONCLUSION

2+
5.1 ACACIA CONCINNA – ZN SYSTEM

Corrosion is a naturally occurring phenomenon which deteriorates a metallic

material by are action with its environment. Corrosion never stops but its severity can be
lessened by using corrosion inhibitors. Surfactants can be used as inhibitors due to their
surface adsorption nature.
The corrosion inhibition efficiency for the natural surfactant Aacia Concinna
were studied for various concentrations.
2+
The synergistic effect of Acacia concinna with Zn on the inhibition of
corrosion of mild steel in well water has been evaluated.

The mechanistic aspects of corrosion inhibition are based on the results

obtained from the weight-loss method and UV-Visible absorption spectroscopy.

The corrosion resistance of mild steel in well water has been evaluated by
weight loss method. The formulation consisting of 60ppm of Acacia concinna and 50ppm
2+
of Zn shows 99% inhibition efficiency (IE) in controlling corrosion of mild steel for
one day immersion period.
2+
.
A synergistic effect exists between Acacia concinna and Zn UV-visible,
Fluorescent spectral data indicate the possibility of formation of protective layer on the
metal surface.
5.2 SUMMARY AND CONCLUSION
The present study leads to the following conclusions:

The corrosion inhibition efficiency of the inhibitor Acacia concinna at various

2+
concentrations in the presence of Zn were studied.
UV-Visible and Fluorescence data confirm the formation of protective film
on mild steel surface.

Based on the weight loss, UV-visible and Fluorescence studies and

spectroscopic techniques, a suitable mechanism has been proposed for the inhibitor and
2+
Zn system.

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5.3 SCOPE FOR FURTHER STUDY

• The present inhibitor formulations can be studied in other natural

surfactant.
• The present inhibitor combination scan be studied in neutral and basic
medias.
• Electrochemical studies like AC impedance, Polarisation and Cyclic
voltammetry can be studied for the present inhibitor combinations.
 Surface examination studies like IR, SEM, EDAX, AFM and Contact angle
measurements can be studied for the present inhibitor combinations
 The present inhibitor formulation scan be studied under different
immersion periods.
• The present inhibitor formulation scan be studied using other metals like
Copper, Aluminium etc.
• Inhibition efficiency (IE) of the selected inhibitors may be evaluated in
2+ 2+ 2+
, , ,
combination with Mg Mn Ba etc.,
• The effect of temperature and pH on the inhibition efficiency (IE) of these
inhibitors can be studied.
• The stability of the protective film formed on the metal surface could be
analysed

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