SYNERGISTIC EFFECT OF SODIUM BENZOATE - Zn2+

SYSTEM IN CONTROLING THE CORROSION STEEL IN GROUND WATER

Dissertation Submitted to the
Holy Cross College (Autonomous), Tiruchirappalli
Affiliated to Bharathidasan University In partial fulfillment of the requirements
For the award of the Degree of
MASTER OF SCIENCE IN CHEMISTRY
Submitted

by

VIJINA. N.P.
Register Number: 09PG124
Under the guidance of
Mrs.H.BENITA SHERINE, M.Sc., M.phil, PGDBI.

DEPARTMENT OF CHEMISTRY
HOLY CROSS COLLEGE (AUTONOMOUS)
National Re-accredited with A Grade by National Assessment and
Accreditation Council (NAAC),
(Affiliated to Bharathidasan University)
THIRUCHIRAPPLLI - 620 002
APRIL-2010

Mrs. H. Benita Sherine, M.Sc, M.phil. PGDBI.

Lecturer, department of chemistry,
Holy Cross College,
Trichy-2

CERTIFICATE
This is to certify that the dissertation entitled SYNERGISTIC EFFECT OF SODIUM
BENZOATE ZN2+ SYSTEM

IN

CONTROLING

THE CORROSION STEEL IN

GROUND WATER submitted to holy cross college (Autonomous) affiliated to

Bharathidasan university in partial fulfillment for the award of the degree of

MASTER OF SCIENCE IN CHEMISTRY is a bonafide record of the work
carried out by Miss.VIJINA. N. P. under my guidance for the academic period
2010-2011.

SIGNATURE OF HEAD

SIGNATURE OF

THE DEPARTMENT

OF THE GUIDE

SIGNATURE OF THE EXAMINER

ACKNOWLEDGEMENT
I am sincerely thankful to God, our Almighty father, for all the blessings he has
showered up on me during this work.
I express my gratitude to Rev.Gr. Sr. Sarguna Mary, Principal and Sr. Christina
Bridget, In charge of evening session , Holy Cross College (Autonomous) for giving me
permission to do this project in the college itself.
I wish to express my deep sense of gratitude and the most sincere thanks to
Dr.Mrs.Beatrice cherian, Head of the department, department of chemistry for her kind help
and advice during the project work.
I sincerely thank my guide Mrs. H. Benita Sherine, M.Sc, M.phil. PGDBI. For her
constant encouragement and unfailing support and guidance throughout the period of my
Endeavour.
I find immense pleasure in forwarding my gratitude to my family members especially
my parents and my beloved friends, for their prayers which helped me to complete this work
successfully.

VIJINA. N. P

DEDICATED TO GOD
AND
MY FAMILY

CONTENTS
CHAPTER

TITLE

INTRODUCTION

II

REVIEW OF LITERATURE
NEED, OBJECTIVE AND SCOPE
OF THE PRESENT STUDY

III

MATERIALS AND METHODS

IV

RESULTS AND DISCUSSION

CONCLUSION

VI

BIBLIOGRAPHY

PAGE
NO

CHAPTER-I

INTRODUCTION

CHAPTER - 1
INTRODUCTION

The present civilization depends up on machines and structures, which utilize metal
parts. But metals in contact with moist oxygen containing atmosphere are fundamentally
unstable with the expectations of noble metals, all metals display a thermodynamic
tendency to revert to the oxides from which most other came. This reversion would occur
by their chemical reaction with oxygen or water.
Many metals are attacked rapidly, and losses due to corrosion sustained by all
branches of the national economy are enormous. 5-20% of ferrous metals produced
annually are destroyed by corrosion. However, the great direct loss due to corrosion
cannot give an accurate idea of the actual damage cost by this process. Even a slight
deterioration of a chemical apparatus by corrosion may put it out of service, upset and
interrupt the technological process, wastage of time and materials etc.The associated
expenses are much higher than the cost of replacement material.
The instability of the surfaces arises from an electrodic mechanism, an
electronation reaction, and teams up with the metal dissolution, reaction to keep
numerous micro corrosion cells running.
Definition of corrosion
Corrosion is defined as the destruction of metals (or) deterioration of metals as a
consequence of chemical (or) electrochemical reaction with the environment.

Loss of corrosion
The economics loses due to corrosion are divided in to two .
(1) Direct loss
(2) Indirect loss
Direct loss includes the cost of replacement of corroded equipments and
machineries such as condensers, pipelines etc.inclusive of labour. The direct loss also take
in to account the extra cost of using corrosion resistant alloys, instead of carbon steel sand
also take into account the cost of galvanizing or plating and adding inhibitors to water.
Indirect losses includes shut down, loss of product, loss of efficiency,
contamination of product and cost due to over design.
HUMAN LIFE AND SAFETY
Corrosion takes an even more on human life and safety corrosion is scarcely
reported as the cause of many fatal accidents, but few examples can be cited readily. The
spectacular airline accidents in Hawaii was in all probability due to the combined effect
of cyclic mechanical stress and atmospheric corrosion in a semitropical environment .
The well known bridge collapse present at western Virginia, killed 46 people in
1967. Selective corrosion of a welded liquid gasoline in Minnesota in 1986 resulted in
massive fire damage to the entire town and also in the loss of two lives.

Again in 1986, a steam pipe suffered from the combined effect of corrosion, burst at a
nuclear plant in Virginia severely burnt eight workers, four of whom died later. These are
only a few examples of many such fatal accidents caused by corrosion.
FACTORS INFLUENCING CORROSION
The nature and extent of corrosion depends largely on metal and the environment.
Thus factors like structural features of the metal, nature of the environment and the type
of the reaction that occur at metal environment interface, must be considered for the
understanding of corrosion phenomenon.
The important factors which may influence the corrosion process are,

Nature of the metal

Nature of the environment

Electrode potential

Temperature

Solution concentration

Aeration

Agitation

pH of the solution

Nature of the corrosion products

Hydrogen over potential

Generally high temperatures produce more intense corrosion.

CORROSION FATIGUE
It occurs due to the combined action of corrosion and cyclic stresses such as
rapidly alternating tensile and compressive stresses, while in purely mechanical fatigue,
failure takes place above a critical value of cyclic stress known as the fatigue limit.
Corrosion fatigue can occur at lower stresses and the corrosion fatigue crack
propagation experiments were conducted on low alloy steels in elevated temperature in
aqueous environment.
EROSION CORROSION
Erosion corrosion is the increase in the rate of attack of a metal because of
relative movement between a corrosive medium and the metal surface. Generally this
movement is rapid and the mechanical wear is involved. Metal is removed from the
surface either in the form of dissolved ions or in the form of solid corrosion products,
which are mechanically swept from the metal surface. This type of attack is characterized
by the appearance of the grooves, rounded holes etc.
Erosion corrosion is observed in piping systems such as bend, elbows, valves,
grinders etc. Some of the factors involved in corrosion are the nature of the surface film
formed on the metal surface, the velocity off the moving fluid, turbulence in the liquid

impingement, the galvanic effect. Chemical composition, hardness. Corrosion resistance

and the metallurgical history of the metals and alloys.

CAVITATION DAMAGE
It is a special form of erosion corrosion caused by the formation and collapse of
vapour bubbles in a liquid near metal surface. cavitation damage occurs in hydraulic
turbines, pump impellers and other surface where high velocity liquid flows and pressure
changes are experienced.
CLASSIFICATION OF CORROSION PROCESS
A distinction is made between chemical, biochemical, and electrochemical
corrosion of metals.
(1) Chemical corrosion
It is a spontaneous destruction governed by the loss of ordinary heterogeneous
chemical reaction. The destruction of metals caused at high temperature by aggressive
gases which prevent condensation of moisture on the metal surface and the dissolution of
metals in contact with non conducting organic media belonging to the corrosion process.
(2) Bio chemical corrosion
It is caused by the vital activity of various microorganisms using a metal as a
culture medium and evolving products which attack the metals. The corrosion usually

accompanies other types of corrosion. Soil of definite composition, stagnant waters and
certain organic products greatly favour the progress of biochemical corrosion.
(3) Electrochemical corrosion
It is encounted more frequently than other types of corrosive destruction and it is
most dangerous to metals. It may occur in a gaseous atmosphere, when moisture
condenses on the metal surface in soils, and in solution. These corrosion is governed by
the kinetics of electrochemical reactions.
A special type of electrochemical corrosion is electro corrosion i.e., corrosion
caused by an external electric current.
(i) Hydrogen evolution type electrochemical corrosion
In this type of corrosion , displacement of hydrogen ions from acidic solution are
considered. All metals placed above hydrogen in the electrochemical series have a
tendency to displace hydrogen by dissolving themselves in acidic solution.
(ii)Absorption of oxygen type electrochemical corrosion
The neutral medium involves the corrosion of the parts which gets oxidized.
(iii) Galvanic type of electrochemical corrosion
When two dissimilar metals are electrically connected and exposed to an
electrolyte, the metal higher in the electrochemical series undergoes corrosion.

(iv) Concentration cell type of electrochemical corrosion

This corrosion is differential oxygenation corrosion, difference in

oxygen

concentration set up corrosion current. In the solution, the immersed parts of the metal act
as anode and get corroded, where as the exposed part which act as a cathode is not
corroded due to differential oxygenation corrosion.
THEORIES OF CORROSION
The rate of corrosion can be determined with the aid of kinetic theory of
corrosion. In this case, cathodic and anodic polarization curves are traced directly on the
metal whose corrosion is studied. The overall rate of corrosion can be express in terms of
current referred to unit area of the entire metal surface without separating it in to anodic
and cathodic areas. The possibility of a dissolution of metal indicates that under given
conditions the rate of ionization is higher than that of discharge of ions. In the absence of
externally applied current and with the potential remaining unchanged, this ratio of the
rate is possible. If the rate discharge of the hydrogen ion exceeds the rate of reverse
process by the same amount. The corrosion rate is defined as the difference between the
rate of discharge of ions and that ionization of hydrogen molecules.
(A) Electrochemical theory of corrosion
According to this theory, the corrosion rate depends not only on the
electrochemical properties of the electrodes of the voltaic couples but also on the ohmic
resistance of the medium in which the corrosion process occurs and which separate the
anode from the cathode. It was originally assumed that the cathodic and anodic processes
are spatially separated and each of these reaction proceeds only on the definite part of the

corroding metal surface. It was concluded on the basis that ideally pure metals with the
highly homogeneous surfaces are not subject to corrosion.
(B) Homogenious theory of corrosion (wagner-traud mechanism
It emphasizes that, irrespective of the presence or absence of impurities, metals
become unstable because of different electrodic charge transfer reactions occurring
simultaneously and the opposite direction to the surface.
METHODES OF CONTROL OF CORROSION
Methods of control of corrosion are divided in to four types.
(1) Electrical methods
This method is based on modifying the electrochemical properties of a metal
under the influence of polarizing current. The protection of metal against corrosion by
imposing a cathodic polarization is most widely used. When the potential of the metal is
moved to more electronegative values, the rate of cathodic values increases, that of
anodic values falls. The decrease in the rate of anodic reaction up on cathodic polarization
is equivalent to the decrease of corrosion rate. An auxiliary metal which is made to
dissolve (corrode) in place of the metal to be protected is often called sacrificial
anodes.
(2) Methods based on changing the properties of corroding metals.
This is achieved by special treatment of the surface or by alloying . The treatment
of the surface of a metal to decrease its corrosion is carried out by any one of the
following methods.

(i)

Coating of the metal surface with passivating films of its sparingly soluble
compounds.

(ii)

Covering the metal surface with protective coats of oils greases, bitumens and
paints.

(iii)

Applying coating of the other metals which are more stable under given condition

than the metal to be protected

(3)

Methods based on changing the properties of corrosion medium.

The corrosion rate can also be decreased by alterating the properties of the metal

medium. This is achieved either by special treatment of the medium with a view to
depress its aggressiveness or by introducing into it the small amounts of special substance
called corrosion inhibitors.
(4) Combination methods.
The mechanical means of corrosion protection are used in combination with
cathodic or anodic protection, which prevents the metal from corrosion at spots
unprotected by the insulating layer.
Paints used to prevent metals from corrosion contained a corrosion inhibitor. Thus
mechanical protection is combined with electrochemical protection.

INHIBITORS
A corrosion inhibitor may be defined as a substance which when added in small
quantities to the aqueous corrosive environment, effectively decreases the corrosion rate
of the metal or allots significantly. Inhibitors are organic or inorganic substances that
dissolves in the dissolving medium, but are capable of forming a protective layer of some
kind at either anodic or cathodic areas.
CLASSIFICATION OF COROSION INHIBITORS
Putilova et al, classified corrosion inhibitors in to 3 types.
Type 1 : Those which forms a protective film on the metal surfaces
Type 2: Those which reduce the aggressiveness of the corrosive media.
Type 3:

Those which functions by forming a protective film and at the same

time reducing the aggressiveness of the corrosive agent.

Another classification is anodic inhibitors, cathodic inhibitors and mixed
inhibitors. This classification is based on polarization data.
Anodic inhibition results in greater shifts in anodic Tafel slope and cathodic
inhibition results in greater shifts in cathodic Tafel slopes. In the case of mixed inhibition
both cathodic and anodic slopes are shifted in an equal extent or there is not much change
in a Tafel slopes.

Examples of anodic inhibitors are chromate, nitrite, molybdate, tungstate,

orthophosphate, silicate and benzoate. Examples of cathodic inhibitors are ZnSO4,
Cr2(SO4)3, NiSO4, polyphosphate, As3+,Sb3+, Hg. Examples of mixed inhibitors are
organic inhibitors, containing nitrogen and sulphur, Eg: amines, triazols, thiazols,
inorganic inhibitors .Eg:Arsenate, arsenite and selenate.
SYNERGISTIC EFFECT AND CORROSION INHIBITION
Mixtures of inhibitors provide better inhibition than either of the individual
components; i.e, the mixtures are sinergestic. This was recognized by Speller in midthirties who reported that the compound films formed by phosphate chromate mixtures
are more effective than individual components.

Phosphonate based cooling water

inhibitors offer protection by forming three- dimensional layers on the metal surface.
THEORIES OF CORROSION INHIBITION
Several theories have been put forward to account for the inhibition corrosion .
(1)Adsorption theory
Macho put forwarded the adsorption theory and effect molecular structure.
According to this theory, the passivity can be achieved through the retardation of metaldissolution reaction caused by adsorbed oxygen atoms. Oxygen atoms may appear on the
metal surface from the discharge of hydroxyl ions (or water molecules) at potentials
lower than those at which oxygen is evolved or oxides are formed. The adsorbed oxygen
atoms passivate the metal either by forming a continuous monomolecular layer on its

surface or by blocking the most active centers or else by changing the potential difference
across the metal- solution interface.
Machu predicts the formation of a porous layer of the inhibitive substance with
high electrical resistivity, which is an essential characteristic of corrosion inhibition.
Uhlig considered that inhibitors get adsorbed at the metal surface, thus blocking
the active sites and affecting the potential of the metal by virtue of their net charge.
Riggs proposed that in the case organic inhibitors, adsorption depends on
chemical nature of metal surface and the electrochemical potential of the metal or
solution interface.
(2) Film formation theory
In this theory (kistyakovaky) which owes its origin to faraday, it is assumed that
passivation of a metal is caused by the formation of a thin, usually oxide film, on the
surface of the metal, which ceases to interact with the surrounding medium and is thus
protected from dissolving. These oxide film has the thickness of several molecular layer
and it may be regarded as a phase oxide. The more perfect the structure of oxide film and
less the number of cracks and defects, the more complete is the passivation and lower the
rate of metal dissolution.
In order to explain the action of inhibitors in neutral and alkaline media, Evans
proposed the film formation theory. He used the specially selected solutions attacking
only the metal and not the oxide film on its surface, succeeded in separating the film by
carefully dissolving the underlying metal. Naturally, the continuity of the film had to be

disturbed to a certain extent because otherwise the metal would not be dissolved. The
data of electron diffraction and the optical investigations all confirms the existence of a
film on the surface of passive metal and, in a number of cases; permit one to identify its
composition and structure.
According to putilova et. al., in acid solution the inhibition is due to the formation
of a layer of insoluble or slightly soluble corrosion product on the metal surface.
(3) Hydrogen over potential theory
The action of acid inhibitors was explained by hydrogen over potential theory. It
was believed that inhibitors increased hydrogen over potential, and thus, increased the
cathodic polarization; Hacker man and Sudbery pointed out those amines are adsorbed on
the cathodic and anodic regions of metal surface. Hoar and Holliday pointed out the shift
in the initial potential of the metal in the presence of organic inhibitors in the positive
direction indicate that they act on the anodic sites . This theory does not explain inhibitive
action of all types of systems.
(4) Electeochemical polarozation theory
Explaining the action of passivating inhibitors, Stern suggested that inhibitors like
chromate get reduced at the cathiodic sites and consequently, raise the electrode potential
to more noble value, bringing about passivation. Studies on passivating inhibitors reveal
that only a small amount of the total current could be associated with cathodic reduction
of inhibitors. Thus Sterns theory also cannot explain the behavior of all types of systems.

CHAPTER II
REVIEW OF LITERATURE
Wormwell and mercer [16] have investigated that sodium benzoate and other metal
benzoate as corrosion inhibitor of mild steel in distilled water, moderately hard mains - water and
in 0.03%of sodium chloride solutions. Electrode-potential measurements and film-stripping
experiments provide evidence for the view that anodic inhibition produces and maintains
continuous film. Electron-diffraction examination of the stripped film has yielded definite
evidence of Fe3O4.
Ann et al [17] investigated the corrosion inhibition effect, compatibility and corrosion
rate of calcium nitrate in aqueous condition using polarization method and its influence on the
chloride transport, comprehensive strength and setting time of concrete. It was observed that
concrete specimens containing the corrosion inhibitor produced the higher total charge passed in
a rapid test for chloride ion permeability. An increase in the dosage of corrosion inhibitor
resulted in a decrease in the concrete setting time.
Amin et al [18] investigated the inhibitive properties of sodium benzoate for AISI-1018
steel controlling corrosion in sea water environment at atmospheric condition .Highest corrosion
rate was observed for the alloy without inhibitor in sea water condition. The corrosion rate
decreases as the corrosion of sodium benzoate being increased. Result demonstrated that the
higher concentration of sodium benzoate in sea water condition, exhibiting protection of AISI1081 steel in sea water environment.
Worm well et al [19] investigated the efficiency of the sodium benzoate and sodium
nitrite corrosion inhibitor in working vehicles .The test have shown that the addition of 1.5% of

sodium benzoate with 1% of sodium nitrite to 20% or 331/3%solutions of ethylene glycol will
effectively prevent corrosion of the cast iron of the cylindrical block.
Blustein et al [20] investigated the lab synthesized iron benzoate as a novel steel
corrosion inhibitor pigment to formulate anti-corrosive paint films. The iron benzoate antiproperties were studied by electrochemical and spectroscopic essays employing pigment
suspensions. Experimental results shown that ferric benzoate was adequate to formulate anticorrosive paint films with improved anti-corrosive assessed.
Huseyin saricimen [21] has evaluated the inhibition of carbon steel corrosion under
wet/dry condition using electrochemical techniques. Sodium dihydrogen ortho phosphate
dicyclohexylamine nitrite and sodium benzoate were used as inhibitors in the investigation. The
corrosion rates of the specimens were determined by electrochemical methods at several
intervals during corrosion. This study showed the beneficial effect of inhibitors in slowing down
the corrosion of steel. Furthermore, wet/dry cycling of steel samples in the laboratory produced
corrosion rates were comparable to those measured under actual outdoor conditions.
Blustein et al [22] investigated the inhibitive properties of benzoate anion in anti
corrosive paints. The anti corrosive properties of zinc benzoate were assessed by electrochemical
techniques, salt spray, humidity tests and electrochemical impedance spectroscopy. The
morphology and the nature of the protective layer grown under the paint film in the salt spray
chamber was assessed by scanning electron microscopy (SCM)

UV -VISIBLE

diffuse

reflectance spectroscopy. Experimental results showed that basic zinc benzoate was adequate
were formulate epoxy anti-corrosive paints with improved anti-corrosive performance, especially
with the water borne binder.

Rosliza et al [23] investigated the corrosion inhibitor of aluminum and its alloy using
weight loss and electrochemical impendence spectroscopic (EIS) measurements on the corrosion
inhibition of AA6061 and AA6063 aluminum alloys in acidic solutions using sodium benzoate as
inhibitor. The results showed that the addition of sodium benzoate retards the rate of dissolution
and inhibits the corrosion of the aluminum alloy in acidic solutions. Electrochemical studies
showed that there was a significant increase in overall resistance after addition of sodium
benzoate when compared to the case without inhibitor.
Zhihua et al [24] investigated that benzoic triazole derivative 3,5 dimethyl benzoic acid
[1,2,4]triazol-1-ylmethyl ester (DBT) as a corrosion inhibitor of mild steel in 1M HCl solution
using weight loss measurements, potentiodynamic polarization, SEM and EIS methods. The
results revealed that DBT was an excellent inhibitor, and the inhibition efficiencies obtained
from weight loss method and electrochemical experiments were in good agreement. Using the
potentiodynamic polarization techniques, the inhibitor was proved to have a mixed type
character for mild steel suppressing both anodic and cathodic reactions on the metal surface.
Wormwell et al [25] investigated that sodium benzoate has been shown to be an effective
inhibitor of the corrosion of mild steel in distilled water, a moderately hard mains- water and
very dilute (0.03%) sodium chloride solutions. The concentration of benzoate required for
inhibition is greater (0.5%) for machined than for emeried surfaces (0.1% in favorable
conditions) and for mains water or chloride solutions (1 or 1.5%) as compared with distilled
water (0.5%). Comparisons with sodium chromate show that sodium benzoate is less efficient. it
is, a safe inhibitor since it does not lead to intense localized corrosion when the concentration is
just below the minimum for protection .the following benzoates have also been shown to possess
inhibitive properties, Li, Zn, and Mg. zinc is partly and copper and aluminum completely,

protected in 0.05% sodium benzoate solution at room temperature. Electrode- potential

measurements and film stripping experiments provide evidence for the view that anodic
inhibition produces and maintains a continuous film. Electron- diffraction examination of the
stripped film has so far yielded definite evidence e of ferric oxide only.
Jauhari et al [26] investigated the inhibition effect of imidazole derivative 4-methyl-2propyl-1H-benzimidazole-6-carboxylic acid(MPBI) against mild steel corrosion in 1N HCI
solutions was evaluated using conventional weight loss, potentiodynamic polarization, linear
polarization and electrochemical impedance spectroscopy. The weight loss result showed that
MPBI is an excellent corrosion inhibitor, electrochemical polarizations data revealed the mixed
mode inhibition and the result of electrochemical impedance spectroscopy have shown that the
change in the impedance parameters, charge transfer resistance and double layer capacitance,
with the change in concentration of the inhibitor is due to the adsorption of the molecule leading
to the formation of a protective layer on the surface f mild steel.
Kanojia et al [27] investigated the effect of nicotinic acid (pyridine 3- carboxylic acid) on
mild steel dissolution in H2SO4 by electrochemical methods: steady state galvanostatic and
potentiostatic polarization measurements. The dissolution parameters such as corrosion currents,
passive current, flade potential, open circuit potential, cathodic and anodic Tafel slopes and
inhibition efficiencies are determined. The adsorption and corrosion rates based on heat of
adsorption and activation energies are calculated from Langmuirs adsorption isotherm. The
inhibition efficiencies range of 94-99% is obtained for a concentration range of 10 -1 to 10-7 mol
l-1. Synergistic effect of I-1 has a strong impact on the performance of these additives. These
results are verified by the weight loss method.

Mumtaz ahamed quraishi [28] the protection of metals against corrosion by means of
volatile compounds is the most progressive method of fighting corrosion. These inhibitors are
used to protect metallic article and equipment during storage and transportation in view of this
six organic volatile corrosion inhibitors (VCIs) using lauric hydrazide with various acids such as
cinnamic acid, succinic acid, nitro benzoic acid, phthalic acid and maleric acid were evaluated
for their inhibiting action on corrosion of mild steel, copper, brass, zinc and aluminum by weight
loss and potentiodynamic polarization methods .All the investigated VCIs exhibited good
inhibition efficiency for all the metals.
Quraishi et al [29] investigated the influence of some substituted dianils on corrosion of
mild steel in 1N hydrochloric acid and 1N sulphuric acid using weight loss and electrochemical
techniques. Inhibition efficiency of these compounds has been found to vary with nature and
concentration of these compounds, solution temperature, immersion time and nature of acid
solutions. The potentiodynamic polarization studies were carried out at room temperature,
according to which all the compounds were found to be mixed type inhibitors and inhibited the
corrosion of mild steel by blocking the active sites of the metal

NEED,OBJECTIVE AND SCOPE OF THE

PRESENT STUDY
Need of present study
Corrosion is a great economic concern. Millions of dollars are lost each year
because of corrosion. Use of corrosion inhibitors is one of the oldest and popular methods
to prevent corrosion . In early days chromates and phosphate were used as inhibitors but
they release toxic materials to the environment. During 1990, carboxylates were used as
corrosion inhibitors. In this study sodium benzoate with zinc ions is used as mixed
inhibitor. Zinc alone does not give good inhibition efficiency. So it is coupled with
sodium benzoate.
Objective and scope of the present study.
The studies are confined to a single metal species namely , carbon steel of composion .
Sulphur

__

0 .026%

Phosphorous

__

0.06%

Manganese

__

0.4%

Carbon

__

0.1%

And the reminder iron.

 The present work is undertaken,

To evaluate the inhibition efficiency of sodium benzoate in controlling

corrosion of carbon steel immersed in aqueous environment.

To evaluate the synergistic effect of Zinc ions with sodium benzoate

inhibitor, by determining synergistic parameters.

To investigate whether the synergistic effect of the inhibitor system is

statistically significant or not by doing F-Test.

To evaluate the extent of controlling the metal dissolution (anodic

reaction) by doing potentiodynamic polarization study.

To analyse the nature of protective film by means of Bode plot, AC

impedance and FT-IR spectroscopy.

To propose a suitable mechanism of corrosion inhibition based on the

results from the above studies.

CHAPTER-III
MATERIALS AND METHODS
Preparation of the mild steel specimens
These mild steel specimens were choosen from the same sheet of the steel having
the following composition.
Sulphur

__

0.026%

Phosphorous

__

0.06%

Manganese

__

0.4%

Carbon

__

0.1%

And the rest iron .

Mild steel specimens of the dimensions 1.0 4.0 0.2 cm polished to mirror
finish and degreased with trichloroethylene, were used in the weight loss method and
surface examination studies.
ZnSO4 Solution
Weighed 1.1 gram of zinc sulphate and made up to 250 ml in a 250 ml standard
flask by using double distilled water

Sodium benzoate solution

Weighed 1 gram of sodium benzoate and made up to 100 ml in a 100 ml standard
flask by using double distilled water.

WEIGHET LOSS METHOD

Determination of surface area of the specimens
The length breadth and thickness of the mild steel specimens and the radius of
the hole were determined with the help of a vernier calipers of high precision and the
surface area of the specimens were calculated.
Weighing the specimens before and after corrosion
All the weighing of the mild steel specimens before and after the corrosion was
carried out using a digital balance.
Determination of corrosion rate
The weighed specimens in duplicate were suspended by means of glass hooks in
100 ml beakers containing 100 ml of various test solution of different concentrations.
After 5 days of immersion, the specimens were taken out, washed in running water, dried
and weighed. From the change weight of the specimens, corrosion rate was calculated
using the following relationship.

Loss in weight (mg)

Corrosion rate =

mdd
Surface area of the specimen(dm2) Period of Immersion (days)

mdd = milligram /dm2/days

mpy = mdd 5.473
mpy = mils per year
corrosion inhibition efficiencies (I.E) was then calculated by using the
equation
W1-W2
IE =

100%
W1

W1 = Corrosion rate in the absence of inhibitor.

W2 = Corrosion rate in the presence of inhibitor
Surface examination study.
The mild steel specimens were immersed in various test solutions for a period of 5 days
the specimen were taken out and dried. The nature of the film formed on the surface of the metal
specimens were analysed by FTIRs pectra.
Potentiodynamic polarization study.
Polarization study was carried out in H & CH electrochemical work station impedence.
Analyser model CH1 660A provided with IR compensation facility, using a three electrode cell
assembly. Carbon steel was used as a working electrode, platinum as counter electrode and

saturated calomel electrode (SCE) as reference electrode. After having done IT compensation,
polarization study was carried out at a sweep rate of .01 V/Sec. The corrosion parameters such as
linear polarization resistance (LPR) corrosion potential (Ecorr), corrosion current (Icorr) and tafel
slopes (bc and ba) were measured.
(b) Alternating Current Impedence Spectra.
AC impedence spectra were recorded in the same instrument used for polarization study,
using the same type of three electrode cell assembly. The real part (Z) and the imaginary part
(Z) of the cell impedance were measured in ohms for various frequencies .The charge transfer
resistance (Rt) and double layer capacitance(Cdl) values were calculated.
Rt = (Rs +Rt) - Rs
Where, Rs

= solution resistance.

Cdl =
Where, fmax =

1/2Rtfmax
maximum frequency.

(C) Analysis of synergistic Effect.

The synergistic effect existing between the inhibitors was verified by calculating the
synergistic parameters. The F-test (ANOVA) was done to find out whether the synergistic
parameters are statistically significany or not.
Synergistic parameter calculation
By using the following formula, the synergistic parameter of the mixed inhibitors is
determined.

SI = 1-I 1+2 / 1-I1+2.

Where, I 1+2

= (I1+I2) (I1I2)

I1

inhibition efficiency of inhibitor 1

I2

inhibitionefficiency of inhibitor2

I1+2

= combined inhibition efficiency of inhibitors 1 and 2 .

(d) F-T est:

It is the significant test and it is defined as the ratio of variance between the sample and
variance within the sample.
Variance between the sample
F =
Variance with in the sample

RESULT AND DISSCUSSION

WATER QUALITY PARAMETERS

S.No

Parameters

Value

1.

pH

7.30

2.

TDS mg/ 1

1236

3.

Color

Nil

4.

Chloride

232

5.

Sulphate

75

6.

Phenolic compound

Nil

7.

Fluoride

0.2

8.

Iron

Nil

9.

Nitrate

40

10.

Sodium

208

11.

Potassium

16

12.

Magnesium

39

13.

Manganese

Nil

14.

Total Hardness mg /1

416

15.

Conductivity

1792

16.

Odour

None

17.

Phosphate

0.05

TABLE:IV-1

Corrosion rates of carbon steel in ground water containing 0 ppm of

Zn2+andtheinhibition
Inhibitor

efficiencies

(IE)

obtained

by

Zn2+

SB

CR

IE

ppm

ppm

mpy

43.8

50

33

25

100

33

25

150

66

-50

200

15

66

250

70.7

-61

: SB + Zn2+

Immersion Period : 5 days

S.No

the

inhibitor

system.

TABLE:IV-2

Corrosion rates of carbon steel in ground water containing 0 ppm of sodium benzoate and
the inhibition efficiencies (IE) obtained by the inhibitor system.
: SB + Zn2+

Inhibitor

Immersion Period : 5 days

Zn2+

SB

CR

IE

ppm

ppm

mpy

43.82

10

63

-43

40

84

-91

50

33

25

60

62

-41

75

33

25

S.No

TABLE:IV-3

Corrosion rates of carbon steel in ground water containing 10 ppm of Zn2+ and the
inhibition efficiencies (IE) obtained by the inhibitor system.
Inhibitor

: SB + Zn2+

Immersion Period

: 5 days

Zn2+

SB

CR

IE

ppm

ppm

mpy

43.8

10

50

71

-61

10

100

86

10

150

86

-96

10

200

69

-57

10

250

71

-61

S.No

TABLE: IV-4

Corrosion rates of carbon steel containing 40 ppm of Zn 2+and the inhibition efficiencies
(IE) obtained by the inhibitor system.
Inhibitor

: SB +Zn2+

Immersion Period

: 5 days

Zn2+

SB

CR

IE

ppm

ppm

mpy

43.8

40

50

34

23

40

100

19

57

40

150

23

47

40

200

17

-61

40

250

15

-66

S.No

TABLE:IV-5

Corrosion rates of carbon steel containing 50 ppm of Zn2+and the inhibition efficiencies
(IE) obtained by the inhibitor system.
Inhibito

Zn2+

SB

CR

IE

ppm

ppm

mpy

43.8

50

50

33

25

50

100

33

25

50

150

29

34

50

200

27

39

50

250

13

71

S.No

Zn2+
Immersion

: SB +

Period : 5 days

TABLE: IV-6

Corrosion rates of carbon steel containing 60 ppm of Zn2+ and the inhibition efficiencies
(IE) obtained by the inhibitor system.
Inhibitor

: SB + Zn2+

Immersion Period : 5 days

Zn2+

SB

CR

IE

ppm

ppm

mpy

43.8

60

50

41

60

100

23

48

60

150

37

16

60

200

25

43

60

250

91

S.No

TABLE: IV-7
Corrosion rates of carbon steel containing 75 ppm of Zn2+and the inhibition efficiencies
(IE) obtained by the inhibitor system.
Inhibitor

: SB + Zn2+

Immersion Period : 5 days

Zn2+

SB

CR

IE

ppm

ppm

mpy

43.82

75

50

-5

89

75

100

118

75

150

15

-134

75

200

93

311

75

250

-24

46

S.No

TABLE: IV- 8
Corrosion rates (CR) of carbon steel in aqueous medium and the Inhibition efficiencies
(IE) obtained by weight loss method.
: SB + Zn2+ in aqueous medium

Inhibitor

SB

Corrosion Rates ( CR ) mpy

ppm
0

10

40

50

60

75

43.82

63

84

33

62

33

50

33

71

34

33

41

-5

100

33

19

33

23

150

66

86

23

29

37

-103

200

15

69

17

27

25

93

250

71

71

15

13

-24

TABLE :IV-9
The Inhibition efficiencies (IE) obtained by weight loss method

Zn 2+

SB
ppm

inhibition efficiency (IE) %

0

10

40

50

60

75

-43

-91

25

-41

25

50

25

-61

23

25

89

100

25

86

57

25

48

118

150

-50

-96

47

34

16

-134

200

66

-57

-61

39

43

311

250

-61

-61

-66

71

91

46

TABLE IV-10

Inhibition efficiencies and synergism parameters for various concentrations of sodium benzoate
Zn2+ systems, when carbon steel is immersed in ground water.

Zn2+ ppm

Sodium
benzoate
ppm
0

10

ppm

ppm

SI

40

SI

50

SI

pp

ppm

60

SI

ppm

75

SI

ppm

-43

-91

25

41

25

50

25

-62

0.7

23

1.9

25

0.75

1.1

87

4.9

100

25

96

57

1.3

25

0.75

48

1.3

118

-0.5

150

-50

-22

47

1.2

34

1.7

16

0.9

134

-0.12

200

66

-57

0.01

-61

0.1

39

0.4

43

0.5

311

-0.37

250

-62

-61

1.6

-66

1.6

71

3.4

91

10

46

-6.3

TABLE: IV- 11

Influence of pH on inhibition efficiency of sodium benzoate - Zn2+ system.

Zn2+

SB

CR

IE

ppm

ppm

mpy

250

60

64

-47

250

60

42

250

60

91

250

60

13

71

250

60

32

30

pH

TABLE: IV- 12

Immersion

Zn2+

SB

CR

I.E

S.No

period

ppm

ppm

mpy

250

60

91

period on the

250

60

34

22

inhibition efficiencies of

10

250

60

33

25

15

250

60

32

27

20

250

60

30

31

Influence of

system

immersion

SBZn2+

TABLE: IV-13

Distribution of F value between the inhibition efficiencies of various concentrations of sodium

benzoate (0 ppm Zn2+) and the inhibition efficiencies of resorcinol in the presence of 10, 40, 50,
60,75 ppm Zn2+.

Zn2+
(ppm)

Source
of

Within
Between

40

Within
Between

50

squares

variance
Between

10

Sum of

Within

0.68
39297
2.21
26001
3557
13280

Within

14

16206

0.68
4912

2.21

significance

0.00014

0.00068
p<0.05

3250

3557

1660

4016
8

p<0.05

1.98

2026
18020

2.1

p<0.05

113568

Level of

of F

18020
Within

Square

Between
75

p<0.05

4016

60

Mean

freedom

Between
TABLE: IV-

Degrees
of

14196

1.27
p<0.05

Corrosion parameters of carbon steel immersed in ground water in the absence and
presence of inhibitors obtained by potentiodynamic polarization method.
Inhibitor : SB, Zn2+.

system

Ecorr
V vs

bc
mv

ba

Icorr
mv

A/cm2

SCE

Ground water

-732.66

354.7

260.9

40.42

-626.83

324.3

218.5

23.64

Groundwater
+ 250ppmSB+
60ppm of Zn2+

TABLE: IV- 15

AC-Impedance parameters of carbon steel immersed in the presence and

absence of inhibitors obtained from AC Impedance spectra.

Rt

Cdl

system

Ohm cm2

F/cm2

Ground water

619.5

0.171

766.7

0.0270

Groundwater +
250ppm SB + 60 ppm
of

Zn2+

DISCUSSION

ANALYSIS OF RESULTS OF WEIGHT LOSS METHOD

Corrosion rates of carbon steel containing ground water in the absence and
presence of sodium benzoate and Zn 2+ obtained by weight loss method are given
in Tables IV -1 to IV 7. The inhibition efficiencies are also given in

these tables.

It is observed that when carbon steel is immersed in ground water, the

corrosion rate is 43.82 mpy. Upon addition of various concentrations
benzoate, the

corrosion

of sodium

rate decreases up to 50ppm and at 60 ppm corrosion rate

increases. There is a protection of the metal from corrosion by the addition of

250 ppm

of sodium benzoate to 60 ppm of Zn 2+ ions which

has 91 % inhibition

efficiency.
Influence of Zn2+ on the inhibition efficiency of sodiumbenzoate
The influence of a divalent metal ion, Zn 2+ , on the inhibition efficiencies
of sodium benzoate in controlling the corrosion of carbon steel, is given Tables
IV-3 to IV-7.

The

inhibition efficiencies

of various concentrations

of Zn 2+ ,

namely 10, 40, 50, 60 and 75 ppm are -43,-91,25,-41, and 25 % respectively. It is
observed from these tables

that

the

synergistic

effect

exist between Zn 2+ and

sodium benzoate. For example 60 ppm of Zn 2+ has -41% inhibition efficiency and
250 ppm

of sodium benzoate

alone

combination has 91% inhibition efficiency.

Analysis of Synergism parameters

has

-61% inhibition efficiency, but their

Synergism

parameters (SI), were calculated using the relation.

1-I1+2

SI =

_______
1-I1+2\\

Where,
I1+2

I1
I2

(I1+I2) - (I1 I2)

=

I1+2 =

Inhibition efficiencies of inhibitor 1

Inhibition efficiencies of inhibitor 2

combined inhibition efficiencies of inhibition 1 and 2.

Synergism parameters are indication of synergistic effect existing between two inhibitors.
The values of synergism parameters are greater than one, indicating synergistic effect existing
between Zn2+and various concentrations of sodium benzoate. This is true for 10 ppm, 40ppm,
50ppm and 60ppm of Zn2+. For 75ppm, the values of SI are less than one.

This suggests that

there is no synergistic effect between sodium benzoate and Zn2+ at this concentration.

Analysis of Variance (ANOVA)

To investigate whether, the influence of Zn2+ on the inhibition efficiencies

of sodium benzoate is statistically significant, the analysis of Variance ( F - test )
was carried out. These results are given

in Tables IV 13.

In Table IV-13, the influence of 10 ppm of Zn2 + on the inhibition efficiencies of

50, 100, 150, 200, 150 ppm of sodium benzoate is investigated. The obtained F-value
1.410-4 is not statistically significant, since it is less than the critical F-value 5.32
for

1, 8 degrees

concluded

that

of

freedom

at 0.05 level

of insignificance.

the

influence

of 10 ppm Zn 2+ on the

Therefore, it is

inhibition efficiencies of

various concentrations of sodium benzoate is statistically insignificant.

In Table IV-13, the
efficiencies

of

influence

of 40 ppm

than the critical

Zn 2+

on the inhibition

50, 100, 150,200 and 250 ppm of sodium benzoate is investigated.

F-value 6.810-4 is not statistically

The obtained

of

significant, since it is less

F- value 5.32 for 1,8 degrees of freedom at 0.05 level of

significance. Therefore , it is concluded that the influence of 40 ppm Zn 2+ on the

inhibition

efficiencies

of various

concentrations

of sodium benzoate

is

statistically insignificant.
In Table IV-13, the influence

of 50 ppm

of

Zn 2+

on the inhibition

efficiencies of 50, 100, 150, 200 ppm and 250 of sodium benzoate is investigated.
The obtained F-value 0.15 is not statistically significant, since it is less than the
critical F-value 5.32 for 1,8 degrees
Therefore, it is

of freedom at 0.05 level of significance.

concluded that the influence

of 50 ppm

Zn 2+

on

the inhibition

efficiencies

of various

concentrations

of sodium benzoate is

statistically

insignificant.
In Table IV-13 , the influence of 60 ppm of Zn 2+ on the inhibition efficiencies of
50, 100, 150, 200 ,250 ppm of sodium benzoate is investigated . The obtained F-value
1.26 is not statistically significant, since it is less than the critical F-value 5.32 for
1, 8 degrees of freedom at 0.05 level of significance. Therefore, it is concluded
that the

influence

of 60 ppm

Zn2+

concentrations of sodium benzoate is

on

the

inhibition efficiencies

of various

statistically insignificant.

In Table IV-13, the influence

of 75 ppm of Zn 2+ on the inhibition

efficiencies of 50, 100, 150, 200, 250 ppm of sodium benzoate is investigated. The
obtained F-value 1.18 is not statistically significant, since it is less than the critical
F-value 5.32 for 1, 8 degrees of freedom at 0.05 level of significance. Therefore, it
is concluded that the influence of 75 ppm Zn 2+ on the inhibition efficiencies of
various concentrations of sodium benzoate is statistically insignificant.
Analysis of potentiodynamic polarization Curves
The potentiodynamic polarization curves of carbon

steel immersed in ground

water, in the absence of inhibitors are shown in Fig.IV-1(a) and 1(b). The corrosion
parameters such as corrosion potential (Ecorr),corrosion current ( Icorr ) and Tafel slopes
(ba, bc) and are given Table IV-14.
When carbon steel is immersed in ground water, the corrosion potential is
-732.66 mV vs. SCE. When the inhibitors are added (250ppm of sodium benzoate and
60ppm of Zn2+ ), the corrosion potential shifts to the anodic side (-626.82 mV Vs

SCE). Further the corrosion current decreases from 40.42 A/cm 2 to 23.64. This result
suggests that a protective film (Fe2+-sodium benzoate complex) is formed on the metal
surface. This protects the metal from corrosion.
Analysis of AC-Impedance spectra
The AC-impedance spectra of carbon steel immersed in ground water in the
presence and absence of inhibitors are shown in Fig-IV-2(a) and 2(b ). The AC
impedance parameters such as charge transfer resistance ( R t ) and double layer
capacitance ( Cdl ) are given in table IV-15. in the presence of inhibitors ( 250 ppm
of sodium benzoate and 60 ppm of Zn2+ ) Rt value increases and Cdl value decreases.
This indicates that a protective film is formed on the metal surface.
Analysis of FTIR spectra
The FTIR spectrum of pure sodium benzoate is shown in FigIV-4(a).
The C=O

stretching frequency appears at 1730cm -1.

The C=C stretching

frequency appears at 1596cm-1. The C-H stretching frequency appears at 3062cm -1. The
C-O stretching frequency appears at 1240 cm -1 The FTIR spectrum of the film formed
on the metal surface after immersion in the solution containing ground water,
250ppm of sodium benzoate and 60 ppm of Zn 2+ is shown in Fig IV- 4 (b). It is
observed that the C=O stretching frequency appeared has shifted from 17501948cm-1.The C=C streching frequency appeared has shifted from 1550-1595 cm-1.
The C-H stretching frequency has shifted from 3062-2811 cm-1. The C-O
stretching frequency has disappeared. These observations indicate that Aminophenol

has coordinated with Fe2+ through oxygen atoms of phenolic group present in
Aminophenol and through the electrons of benzene ring resulting in the
formation of Fe2+ -C6H5COONa complex formed on the anodic sites of the metal
surface. The peak at 1350cm-1 is due to Zn( OH )2 formed on the cathodic sites of
the metal surface.
Mechanism of corrosion inhibition
Weight loss study reveals that the formulation consisting of 250 ppm of
sodium benzoate and 60 ppm of Zn2+ has 91 % inhibition efficiency in controlling
the corrosion of carbon steel immersed in ground water. Synergism parameters
suggest that a synergistic effect exists between sodium benzoate

and Zn 2+. Polarization

study reveals that this system functions as anodic inhibitor. AC impedance spectra
reveal that a protective film is formed on the metal surface. FTIR spectra reveal
that the protective film consists of Fe2+ - C6H5COONa complex and Zn(OH)2.
In order to explain the above fact in a holistic way the following
mechanism of corrosion inhibition is proposed.

When the formulation consisting of 250 ppm of sodium benzoate and

60 ppm of Zn2+ is prepared, there is formation of Zn 2+- C6H5COONa
complex in solution.

When carbon steel is immersed in this solution there is diffusion of

Zn2+- C6H5COONa complex towards the metal surface.

On the metal surface, it is converted in to Fe 2+- C6H5COO Na

Complex. Zn2+ is released and Zn (OH) 2 is formed.

Zn2+- C6H5COONa + Fe2+ Fe2+- C6H5COO Na + Zn2+

Zn2+ + 2OH-

Zn (OH) 2.

Thus the protective film consists of Fe 2+ - C6H5COONa.complex formed

on

anodic sites of the metal surface and

cathodic sites of the metal surface.

Zn(OH) 2 deposited on

CONCLUSION
The inhibition efficiencies of sodium benzoate - Zn 2+ system in controlling
corrosion of carbon steel ground water has been evaluated by weight loss method.
The present study leads to the following conclstions.
Weight loss study reveals that the formulation consisting of 250 ppm of
and 60 ppm of Zn2+ has 91% inhibition efficiencies in

sodium benzoate

controlling corrosion of carbon steel immersed in ground water.

Synergism parameter suggests that a synergistic effect exist between sodium
benzoate and Zn2+.
Polarization study reveals that sodium benzoate - Zn2+ system functions as as
anodic inhibitor.
AC impedance spectra (Bode plots) reveals that a protective layer is formed
on the metal surface.
FTIR

spectra

reveals

that

the

C6H5COONa complex and Zn(OH)2.

protective

film

consists

of

Fe 2+-

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