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 VOL. 8, NO. 5, MAY 2013 ISSN 1819-6608
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EFFECT OF GREEN INHIBITOR ON THE CORROSION BEHAVIOUR

OF REINFORCED CARBON STEEL IN CONCRETE
Eyu D. G.1, Esah H.1, Chukwuekezie C.1, Idris J.1 and Mohammad I.2
1
Faculty of Mechanical Engineering, Universiti Teknologi Malaysia
2
Faculty of Civil Engineering, Universiti Teknologi Malaysia
E-Mail: [email protected]

ABSTRACT
The effect of inhibitors on the corrosion behaviour of carbon steel reinforced in concrete exposed to 3.5% NaCl
solution has been studied by electrochemical and weight loss tests. The corrosion potential and concrete resistivity were
determined during the immersion time of the concrete specimens. The results show that calcium nitrite and vernonia
amygdalina extract reduced corrosion rate compared to sodium nitrite. However, vernonia amygdalina inhibition was more
effective in the immersed concrete in simulated seawater. The weight loss results demonstrated that 2% sodium nitrite was
more effective with efficiency of 96% in comparison with 2% calcium nitrite and 6% vernonia amygdalina with efficiency
of 92% and 75%, respectively. From the results, it is evident that the extract from vernonia amygdalina (bitter leaf) acts as
an excellent corrosion inhibitor for rebar steel, efficiency increases with increase in dosage, and the inhibition mechanism
was by physical adsorption which is responsible for shielding the specimen from corrosive environment.

Keywords: carbon steel, corrosion, inhibitor, vernonia amygdalina, chloride, concrete.

1. INTRODUCTION of sodium nitrite on carbon steel is similar to that of

The degradation of reinforcing steel due to calcium nitrite.
corrosion is predominant in concrete structures. Generally, Moreover, the effect of plant extracts as corrosion
most structures are contaminated with chloride as a result inhibitor in mild steel in acidic medium have been studied.
of deicing during the winter and also in chloride laden It has been reported that vernonia amygdalina (bitter leaf)
environment such as marine for offshore and coastal and Azadirachita (Nee leaf) extracts performed optimally
structures [1]. Corrosion damage causes the weakening in acidic solution and that inhibition efficiency increases
and quickens the aging of high way structures [2]. with increase in dosage. The inhibition mechanism of
Environmental modification by means of inhibitors is one vernonia amygdalina is related to their physical adsorption
of the most effective measures for corrosion control in properties due to the presence of tannin, alkaloid and
rebar embedded in concrete. Cost of inorganic inhibitor is saponnins [8, 9, 10]. The use of organic compound to
low, however some of them are very toxic (harmful to reduce the corrosion of carbon steel has great importance
both human and environment) such as chromate, mercride, due to their applications in prevent corrosion in different
arsenate etc. aggressive environments [11]. However, no study of
Corrosion inhibitors are chemical substances vernonia amygdalina inhibition potency in reinforcing
which can prevent or reduce corrosion rate when present steel bar in concrete exposed to chloride laden
in adequate proportion. The use of inhibitors seems to be environment has been reported. Based on the background
more promising due to their simplicity in application, and of knowledge of vernonia amygdalina (bitter leaf), sodium
relatively less expensive. Generally, inhibitors are nitrite and the traditional calcium nitrite inhibitors, the
classified according to which electrode reaction they present study was designed to identify and evaluate the
influence. They can be identified as anodic, cathodic or behaviour of sodium nitrite, vernonia amygdalina and
mixed inhibitors [3]. So far many investigations have been calcium nitrite inhibitors on corrosion performance of
carried out on the effect of inorganic inhibitors on the carbon steel reinforced in concrete exposed to simulated
corrosion of carbon steel in concrete. Calcium nitrite was seawater.
able to reduce or inhibit initiated localized corrosion of
rebar steel chloride contaminated concrete as reported in 2. EXPERIMENTAL METHOD
previous study [4]. Calcium nitrite can inhibit the initiated,
localized corrosion of reinforcing steel in solutions 2.1. Materials
simulating chloride contaminated concrete, if it is present The following materials were used for the study:
in sufficient concentration in early stages of the corrosion substrates metal; carbon steel reinforcing bars, mild steel
process. Nitrites (calcium or sodium salt) are anodic plates for weight loss test, likewise the inhibitors used
inhibitors, they compete with chloride ions for the ferrous were calcium nitrite, sodium nitrites and vernonia
ions at the anode to form a film of ferric oxide (Fe2O3) [5]. amygdalina inhibitors. Similarly, cement, fine and coarse
Sodium nitrite inhibitor was found to be effective in aggregates, tap water and 3.5% NaCl solution were used
reducing corrosion rate in reinforced steel concrete at as test solutions.
4%wt dosage [6]. However, efficiency decreases as
chloride content increases [7]. The inhibitive mechanism

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2.2. Method Figure-1(b). Schematic diagram of mild steel coupon.

2.4. Material characterization
2.2.1. Preparation of vernonia amygdalina extract The low carbon steel chemical composition was
The leaves were obtained from the plant in the analyzed by Glow Discharge Spectrometer (GDS) model
neighborhood and thoroughly washed with water to Leco 850A after proper grinding with silicon carbide
remove unwanted materials and then weighed. The paper of 220 grit size. The chemical composition wt% is
weighed amount (200g) was put in a bottle container, as follows: C 0.032, Mn 0.193, P 0.012, S 0.014, Si 0.018,
methanol was added and the container was tightly covered Fe 99.6. The mild steel plate used for the weight loss
to prevent evaporation. The mixture was left for 48 hours measurement was equally analyzed with the same GDS.
to allow proper removal and concentration of the extracts. Similarly, Nikon microphot -FX optical microscope was
Afterward, the mixture was filtered to obtain a liquid used to examine the microstructure of the carbon steel
residue containing methanol. The methanol was removed before the corrosion test.
by heating the resulting solution over a water bath at76oC
for 20 minutes in rotary evaporator model Buchi R-200. 2.5. Concrete sample preparation
Figure-2 shows cylindrical reinforced concrete
2.3. Specimen dimension making process. Concrete mix is very crucial in concrete
In this study, specimen geometry that was used is making procedure. Batching, mixing and casting of entire
cylindrical concrete block with dimension 75mm diameter set were done one day, so that all the specimens with same
and 150mm height in accordance to ASTM C685M-11. individual inhibitors will have the same age. Prior to the
One plain carbon steel bar (grade 40) of diameter 10mm day of casting, all the aggregates were weighed to the
and length 170 mm was embedded at the centre of the nearest kilogram (0.01). Calcium nitrite and the plant
each concretes (lollipop). extracts inhibitor were measured volumetrically before the
Both ends of the bars were covered with epoxy mixing in different containers. However, sodium nitrite
and tape with electroplater tape so that the exposure area was weighed in the weighing balance. Hand mixing was
of each specimen will not corrode; the schematic diagram used in accordance to ASTM C685 (0.07m³). The cubic
of the sample dimension is shown in Figure-1(a). In volume of the concrete was calculated as follows;
addition, carbon steel plate of dimension 50x25x1.5mm Volume = πr2h +0.3πr2h. The concrete mix design is
was used for weight loss measurement for bare specimens shown in Table-1.
without concrete as shown in Figure-1(b). Where r is the radius of the cylinder in
millimetres and h, the height of the cylinder.
Volume of the concrete for the cylinder was
calculated to be: 8.62x10-4m3.
Seven concrete samples were used, each of the
samples aggregates were mixed with water containing the
inhibitors. Six samples were with inhibitors and one
without; the inhibitors used were in proportion of 6L/m3
and 12L/m3 for each of the two samples containing
calcium nitrite and vernonia amygdalina. However, the
remaining two samples consist of 2%wt and 4%wt sodium
nitrite inhibitors respectively.
Figure-1(a). Low carbon steel bar embedded in
cylindrical concrete block. Table-1. Concrete batch mix design (Kg/m³),
w/c = 0.50.
Constituents Weight (Kg/m3 )
Cement 360
Coarse aggregates 1008
Fine aggregates 552
Water 180

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(a) Concrete sample in the mould. (b) Curing process of concretes.

Figure-2. Cylindrical concrete sample making process.

2.6. Corrosion test 2.6.3. Determination of corrosion rate (mmpy) and

Corrosion test was conducted for the sample inhibition efficiency (%) for weight loss test
without concrete (bare samples) and sample with concrete The weight loss was calculated by finding the
as explained in sections 2.6.1 to 2.6.6. variation between initial and final weight of each coupons
after each immersion period from the relationship [3].
2.6.1. Visual inspection
Visual inspection is a Non Destructive Evaluation W = W i –W f (1)
method of corrosion monitoring. It is the simplest and the
oldest inspection technique. This method is economical Wi = initial weight, Wf = final weight
and fast. This simply involves most often the use of the
human eyes to observe the surface morphology. Although CPR = mmpy = 8600W/ ρAt (2)
this techniques has some limitations because it can only
provide qualitative results but not quantitative and W is the weight loss (mg) after exposure time t
sometimes pitting corrosion can only be detected with (h), ρ is density of metal (g/cm³) and A is the area of the
aided human eyes but it is always the first approach in specimen (cm²) and t, time of exposure in hours.
corrosion inspection. In this study, the specimens were The standard expression for measurement of
inspected prior and after the immersion time to examine corrosion rate in millimetre per year (mmpy) in equation
surface appearances. (2) above was used to determine the corrosion rate as
given [3].
2.6.2. Weight loss measurement The inhibition efficiency (IE %) was evaluated as
Weight loss measurement was carried out with given in the equation (3) using the relationship [3].
bare carbon steel prior to reinforced concrete immersion in
order to assess the suitability of the inhibitors in 3.5% IE % = (1- (3)
NaCl solution.
The size of the coupon used for the immersion Where W and Wo are the corrosion rates with and without
test was 50x25x1.5mm. Twenty specimens were used, the inhibitor, respectively.
four set of five coupons were abraided with silicon carbide
from 220 to 1200 grits, and were washed with doubly 2.6.4. Half-cell potential measurement
deionized water, degreased with acetone then air dried at Electrochemical method for corrosion rate
room temperature. The specimens were weighed in Ohaus measurement is the simplest monitoring techniques for
electronic digital weighing balance model PA 214 and reinforcing bar embedded in concrete. In this study,
each weight was recorded subsequent to immersion. Five copper-copper sulphate half-cell was used to measure the
coupons suspended by inextensible thread were immersed half-cell potentials of the steel rebar according to ASTMC
in a non-conductive container of 3.5% NaCl solution of 876-87 G3. Corrosion potential readings were taking by
2725ml (20ml/cm2). Four ponding containers were used, placing the copper-copper sulphate electrode (CSE) firmly
each contained vernonia amygdalina extracts (organic on the surface of the concrete at portions of the cylinder
inhibitors) 6%v/v, calcium nitrite 2%v/v, sodium nitrite block specimens (mapping) at close range interval, the
2%v/v inhibitors and the controlled experiment was measurement were carried out after the samples have been
without inhibitor. After each immersion period, specimens removed from immersion solutions for 2 hours to allow
were removed from the ponding solution; cleaned, diffusion of air through concrete pores.
thoroughly washed with distilled water, acetone, dried and
then weighed in order to evaluate the weight loss, rate of 2.6.5. Concrete resistivity measurement
corrosion, inhibition efficiency and degree of surface Electrical resistivity of concrete could be an
covering. The weight loss of each coupon was determined effective parameter to assess the risk of corrosion in
at 7 days, 14 days, 28 days, 42 days and 56 days. The reinforcing steel embedded in concrete especially for
study was conducted at temperature range within 280C- chloride induced corrosion. AC and DC are the two widely
35.70C. used techniques used for determining concrete resistivity.

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In the study, the Wenner four probes method was used as magnifications respectively. From these results, it can be
shown in Figure-3. This was done by placing the four visibly observed that the specimen consists of pearlite
probes in contact with the concrete directly above the (dark grey areas) and ferrite (light grey regions). The
reinforcing steel bar. Different readings were taken at ferrite matrix consists of larger percentage ferrite and
different locations at the surface of the concrete. The mean small amount of pearlite by composition. It can therefore
values of the readings were recorded as the final readings be deduced from this result that the microstructure is a
of the resistivity in the study. typical of low carbon steel.

Figure-4. Optical micrograph of low carbon steel.

Figure-3. Concrete electrical resistivity measurement.
3.3. Weight loss measurement after immersion
2.6.6. Determination of corrosion rate (mmpy) for duration
reinforcing steel bar in concrete From the chart in Figure-5, it can be seen that the
The corrosion rates in each of the specimens were weight loss for samples without inhibitor increased
evaluated from corrosion current density Icorr. Using the linearly from approximately 0.020 to 0.029g with an
formulae as stated below: average loss of 0.111 g/wk. On the other hand, samples
treated with 2%v/v sodium nitrite, 2% v/v calcium nitrite
Icorr. = p (4) and 6% v/v vernonia amygdalina demonstrate a reduction
in weight loss in comparison with the sample without
inhibitor.
Stern Geary relationship (Stern 1975).

Where

Icorr = Corrosion current density, µA/cm2.

B = Stern -Geary constant, 26mV (Andrade, 1978).
Rp = Polarization resistance, Ohm.cm2.
Corrosion rates in mm/yr was calculated as; 0.0116 ×Icorr.
as given by (Devi and Kannan, 2011).

3. RESULTS AND DISCUSSIONS

3.1. Vernonia amygdalina phytochemical composition

The leaves extract was characterized by IR Figure-5. Weight loss as a function of immersion duration
spectroscopic techniques and quantitative analyses. From for carbon steel immersed in
the screening, the result shows that the plant extract 3.5%NaCl solution.
contains alkaloids, saponin and tannin as shown in Table-
2. 3.4. Corrosion rate measurement after immersion
duration
Table-2. Phytochemical screening. From Figure-6, it is evident that the corrosion
rates of the unprotected carbon steel increased
Phytochemicals tested Remark dramatically from 0.04mm/yr to 0.09mm/yr and then
Alkaloids Positive reduced slight to 0.088mm/yr at the end of the eight week.
On the other hand, sodium nitrite inhibitor proved to be
Saponins Positive effective at 2%v/v in 3.5% NaCl solution. In similar trend,
Tannins Positive corrosion rates for samples with calcium nitrite inhibitor
increased from 0.001mm/yr in day 7 to 0.033mm/yr in the
second week and declined significantly to 0.007mm/yr at
3.2. Microstructural analysis of low carbon steel
the end of the test. The presences of tannins, alkaloids and
specimen
saponnins in vernonia amygdalina acts as a barrier on the
Nikon Optical microscopy was used to examine
metal surface, thus preventing the diffusion of ions from
the microstructure of the specimens. Figure-4 shows the
or to the surface of the corrodent thereby blocking the
results of the microstructure under 200 and 500

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anodic or cathodic site which consequently reduces stable and insoluble hydrated ferric oxides in the region of
corrosion rates as reported by [10]. stability of the oxide [12].

Figure-6. Corrosion rate (mm/yr) versus immersion Figure-7. Inhibition efficiency versus immersion duration.
duration for mild steel immersed in 3.5%
NaCl solution for 56 days. 3.6. Corrosion evaluation of reinforced carbon steel in
concrete immersed in solution
3.5. Inhibition efficiency Corrosion behaviour of reinforced bar was
Figure-7 shows the inhibition efficiency of the evaluated as explained in sections 3.6.1 to 3.6.4.
various inhibitors used for the weight loss test within the
56 days of immersion of immersion time. From the chart, 3.6.1. Visual inspection
it can be inferred that sodium nitrite inhibitor exhibits the Visual inspection is a Non Destructive Evaluation
highest inhibition efficiency of 96% at the end of the test. method for corrosion monitoring. It is the simplest and the
The inhibition increases from 68.8% in day 7 to 96% at oldest inspection technique. Although this technique has
the end of the study. This shows that the oxide films some limitations however, it is always the first approach in
formed on the carbon surface were thick and stable enough corrosion inspection. At the end of the end of the
to diminish corrosion rate due to the passivation influence experiment, pitting corrosion was observed only on the
of the nitrite inhibitor. The ferrous ions are converted into sample without inhibitor. Figure-8 shows the morphology
of the carbon steel after the immersion time.

Pitting
(a) Sample without inhibitor (b) 12L/m3 calcium nitrite (c) 2%wt sodium nitrite (d) 12L/m3 VA.
Figure-8. Visual inspection of reinforcing bar in concrete immersed in 3.5% NaCl solution for 56 days.

3.6.2. Half-cell potential measurement

Figures 9 and 10, it can be ascertained that no
pitting corrosion initiation is envisage for all the samples
with corrosion inhibitors at the end of the experiment, in
an aerated concrete, potential range is normally from
+100mV to -200mV SCE [13]. However, for low level of
chloride content (0 to 0.3) % by mass of cement, corrosion
potential +250mV and below shows that the probability of
corrosion initiation is negligible However, there is the
likelihood of corrosion initiation and propagation above
this corrosion potential in chloride environment [14]. In
addition, the visual inspection confirmed minute regions Figure-9. Corrosion potential as a function of time for
of pitting in the unprotected samples. immersion samples in 3.5% NaCl solution.

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3.6.4. Corrosion rate

From Figure-13, within the limited period of the
study, the corrosion rate was plotted against immersion
time for reinforcing bar in concrete samples immersed in
3.5% NaCl solution. Sample without inhibitor shows
insignificant protection, this is as a result of diffusion of
chloride ions due to differences in concentration gradient
between the immersion solution and the concrete pores
solution. The corrosion rate decreased significantlly for
Figure-10. Corrosion potential as a function of time for vernonia amygdalina [19] and calcium nitrite [20] for
immersion samples in 3.5% NaCl solution. 12L/m3 inhibitors dosage. However, increased in sodium
nitrite inhibitors dosage to 4%wt reduces the inhibition
3.6.3. Concrete resistivity performance by 8% this attribute agrees with the findings
Figures 11 and 12 show the plots of concrete of Devi and Kannan [18]. Overall, the inhibition
electrical resistivity as a function of immersion duration performance is in order of; vernonia amygdalina
for specimens immersed in 3.5% NaCl solution for 10 calcium nitrite sodium nitrite without inhibitor.
weeks. It can be observed that the curves follow the same
upward trends. However, sodium nitrite inhibitor assumed
a lower resistance position. This is in accordance with the
findings of previous study [15]. The lower resistivity is
due to higher ions as a result of the presence of Na+ and
NO2- in the aqueous phase filling the pores capillary.
According to Morris et al., [16], reinforcing steels are in
active corrosion risk when ρc is below 10kΩcm and attain
passivity at resistivity greater than 30kΩcm. Previously
study [17] reveals that resistivity above 20kΩcm indicates
negligible corrosion risk while between 10kΩcm to Figure-13. Corrosion rates (mm/yr) versus immersion
20kΩcm suggests low corrosion risk. However, 4%wt time for carbon steelin concrete immersed in 3.5%
sodium nitrite exhibits a lower resistivity of about15kΩcm NaCl solution.
among the three inhibitors as a result of aforementioned
reason. In addition it is also obvious to reiterate that 4. CONCLUSIONS
sodium nitrite inhibitor gives optimum inhibition effect in
concrete with inhibition composition between 2-3%wt by a) Vernonia amygdalina (plant extract) inhibitor shows
cement [18]. excellent Ecorr of +95mV and calcium nitrite +85mV
for 12L/m3 within the 70 days of immersion. This
shows that eco-friendly inhibitor can be harnessed for
corrosion inhibition in reinforcing concrete for marine
and chloride laden environment. However, 2%wt
sodium nitrite falls within +126mV at the end of the
study.
b) The degree of reduction in corrosion rates in
reinforcing carbon steel was higher in vernonia
amygdalina inhibitor compare to calcium nitrite and
sodium nitrite within the immersion period.
Figure-11. Concrete electrical resistivity versus c) Weight loss test revealed that sodium nitrite inhibitor
immersion time in 3.5% NaCl solution. shows higher inhibition efficiency of 96% followed by
calcium nitrite with 91% for 2%v/v inhibitor.
However, vernonia amygdalina has inhibition
efficiency of 75% with 6%v/v. The nitrites can
therefore be used as inhibitors in coolants.

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